CN109232884A - A kind of interface preparation method of two dimension organic framework materials - Google Patents
A kind of interface preparation method of two dimension organic framework materials Download PDFInfo
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Abstract
The present invention provides a kind of interface preparation method of two-dimentional organic framework materials.The two-dimentional stannous chloride nanocrystal for playing template and catalytic action is evenly spread on smooth silicon wafer, select the 1 of various concentration, 3, the aromatic amino compounds acetonitrile solution such as 5- triaminobenzene, coated on the silicon chip surface for being loaded with stannous chloride, the sequentially drop coating aromatic amino compound acetonitrile solution from high concentration to low concentration, in stannous chloride surface growing large-area two dimension organic framework materials.The method disclosed in the present is using the nanometer polymer that first pre-polymerization generates as crystal seed, it then proceedes to be slowly added to monomer, the two-dimentional monocrystalline organic framework materials of more large scale are finally obtained in two-dimentional stannous chloride template surface, reaction condition is mild, and preparation method is simple.
Description
Technical field
The present invention relates to two-dimentional organic framework materials preparation fields, more particularly to one kind, and big face is prepared on catalysts template
The interface preparation method of product two dimension organic framework materials.
Background technique
Two-dimentional organic framework materials are a kind of porous organic crystal material by being covalently keyed, porosity, crystallization
Property and two-dimensional directional pi-electron conjugated system assign its excellent photoelectricity, mechanics, molecule transmitting etc. performances.Covalent organic frame
Material has the attribute that can be designed, can cut, and passes through the two-dimentional organic framework material of Topology Structure Design and monomer selection preparation
Have the characteristics that density is low, structurally ordered, large specific surface area, low cost, and rear synthetic modification, the filling of hole object can be passed through
Or the modes such as load, Material cladding realize the functionalization to two-dimentional organic framework material, in gas absorption, heterogeneous catalysis, energy
The research fields such as amount storage have important application value and vast market prospect, and it is emerging to cause the strong research of scientific circles
Interest.
But the synthetic method of two-dimentional organic framework materials is typically all to tend to be received based on monomer polymerization
The aggregate of metrical scale crystal, rather than the two-dimensional structure of large area.For all crystal seed growth methods, how all presence are put down
The problem of weighing apparatus nucleation and growth, the two-dimentional organic framework materials as organic single-crystal are no exception.If in growth phase monomer
Excessive velocities are added, is more than nucleation critical concentration, new nucleus will be generated, final crystallite dimension is caused to become small and uneven.Separately
Outside, up to the present the preparation of two-dimentional organic framework material is only limitted to the chemical reaction for being easy to carry out, and is related to reactive species very
It is limited, limit the exploitation of new construction and new material.With the development of two-dimentional organic polymer material, for synthetic polymer
Type and function also proposed more requirements, and there is an urgent need to develop novel two-dimentional organic polymers to meet various practical need
It asks.
Summary of the invention
A kind of preparation method of two-dimentional organic framework materials is proposed, it is especially a kind of that big face is prepared on catalysts template
The interface preparation method of product two dimension organic framework materials.
The present invention adopts the following technical scheme:
A kind of interface preparation method of two dimension organic framework materials, includes the following steps:
(1) by the ethanol solution of copper chloride and ferric trichloride be coated on copper foil surface, at a certain range of temperature and when
In make rapid reaction, directly prepared in copper foil substrate play template and catalytic action two-dimentional stannous chloride it is nanocrystalline
Body material is evenly spread to after being cleaned with ethyl alcohol on smooth silicon wafer；
(2) selecting 1,3,5- triaminobenzenes etc. to have the aromatic amino compound of similar symmetrical structure is monomer molecule,
It is dissolved in acetonitrile and is configured to the solution of various concentration, matched solution is coated on and is loaded with two-dimentional stannous chloride nano crystal material silicon
Piece surface maintains half an hour rear venting at room temperature in closed container, suitable from high concentration to low concentration after acetonitrile volatilization completely
Secondary drop coating aromatic amino compound acetonitrile solution, is repeated several times, in two-dimentional stannous chloride nanocrystal surface growing large-area
Two-dimentional organic framework materials.
The range of ferric trichloride additive amount is the 0.01%-10% of copper chloride solution molar concentration in step (1).
Make rapid reaction in step (1) at a certain range of temperature and in the time, preferred temperature is 0~80
DEG C, the preferred time is 0.1~600s.
The aromatic amino compound in step (2) with similar symmetrical structure includes 2,4,6- triethylbenzenes -1,3,5-
Trimethylamine, 2,4,6- trimethylbenzenes -1,3,5- triamine, 1,3,5- triamidos -2,4,6- trinitrobenzen etc..
Aromatic amino compound acetonitrile solution concentration is 1mmol/mL, 0.5mmol/mL, 0.4mmol/ in step (2)
ML, 0.3mmol/mL, 0.2mmol/mL, 0.1mmol/mL, 0.05mmol/mL, 0.01mmol/mL etc..
Sequentially the number of drop coating is 2~20 times in step (2), and solution concentration is randomly choosed according to sequence from high to low,
The selection of solution concentration can repeat.
The present invention has the advantage that
(1) it using the nanometer polymer of first pre-polymerization generation as crystal seed, then proceedes to be slowly added to monomer, finally obtain more
The two-dimentional monocrystalline organic framework materials of large scale.
(2) reacting for tactful on's progress is assisted to contribute to form large-area two-dimensional and have from catalyst and template or substrate
Machine frame frame material.
(3) reaction condition is mild, have prepare it is simple, at low cost, be easy to the characteristics of industrialized mass production.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph that the method for the present invention prepares stannous chloride nano-sheet crystals material.
Fig. 2 is the method for the present invention schematic diagram.
Specific embodiment
Of the invention for ease of understanding, it is as follows that the present invention enumerates embodiment.Those skilled in the art are it will be clearly understood that the implementation
Example is used only for helping to understand the present invention, should not be regarded as a specific limitation of the invention.
Embodiment 1
(1) copper foil of 25um thickness is selected, the one side of copper foil or two sides are the planes by polishing treatment, use deionization
It is dried for standby for 60 DEG C after water cleaning copper foil surface.
(2) 134.45mg Copper dichloride dihydrate powder is added in 10ml deionized water, is stirred 2 minutes, configuration~
The copper chloride solution of 0.1mol/L.Copper chloride solution is added in 1.63mg anhydrous ferric trichloride powder.
(3) by 10mL~copper chloride solution of 0.1mol/L is added drop-wise to the burnishing surface of copper foil, by bar coating method
Liquid is uniformly dispersed in copper foil surface, forms the film of uniformly continuous.
(4) copper foil for carrying copper chloride solution is placed in the baking oven that temperature is 60 DEG C and is dried 5min.
(5) it is collected after scraping the cuprous chloride crystal of copper foil surface with blade, it is brilliant with washes of absolute alcohol stannous chloride
Body powder is coated on silicon wafer after ethyl alcohol stirring is added.
(6) the 1 of 0.123g, 3,5- triaminobenzene is dissolved in 1.0mL acetonitrile, is divided into several pieces, then in every part points
Not Jia Ru respective volume acetonitrile solution, configure 1mmol/mL, 0.5mmol/mL, 0.4mmol/mL, 0.3mmol/mL,
The solution of 0.2mmol/mL, 0.1mmol/mL, 0.05mmol/mL, 0.01mmol/mL.
(7) the 1 of 1mmol/mL, 3,5- triaminobenzene acetonitrile solution is coated on and is loaded with two-dimentional stannous chloride nanocrystal material
Expect silicon chip surface, temperature setting is room temperature, and half an hour is maintained in closed container.
(8) closed container ventilation is opened, after acetonitrile volatilization completely, the 1 of drop coating 0.5mmol/mL, 3,5- triaminobenzene second
Nitrile solution, temperature setting are room temperature, and half an hour is maintained in closed container.
(9) closed container ventilation is opened, after acetonitrile volatilization completely, the 1 of drop coating 0.4mmol/mL, 3,5- triaminobenzene second
Nitrile solution, temperature setting are room temperature, and half an hour is maintained in closed container.
(10) closed container ventilation is opened, after acetonitrile volatilization completely, the 1 of drop coating 0.3mmol/mL, 3,5- triaminobenzenes
Acetonitrile solution, temperature setting are room temperature, and half an hour is maintained in closed container.
(11) closed container ventilation is opened, after acetonitrile volatilization completely, the 1 of drop coating 0.2mmol/mL, 3,5- triaminobenzenes
Acetonitrile solution, temperature setting are room temperature, and half an hour is maintained in closed container.
(12) closed container ventilation is opened, after acetonitrile volatilization completely, the 1 of drop coating 0.1mmol/mL, 3,5- triaminobenzenes
Acetonitrile solution, temperature setting are room temperature, and half an hour is maintained in closed container.
(13) closed container ventilation is opened, after acetonitrile volatilization completely, the 1 of drop coating 0.05mmol/mL, 3,5- triaminobenzenes
Acetonitrile solution, temperature setting are room temperature, and half an hour is maintained in closed container.
(14) closed container ventilation is opened, after acetonitrile volatilization completely, the 1 of drop coating 0.01mmol/mL, 3,5- triaminobenzenes
Acetonitrile solution, temperature setting are room temperature, and half an hour is maintained in closed container.
Fig. 1 includes the SEM figure that the present embodiment prepares stannous chloride nano-sheet crystals material.
Fig. 2 includes the present embodiment process schematic.
Embodiment 2
(1) copper foil of 25um thickness is selected, the one side of copper foil or two sides are the planes by polishing treatment, use deionization
It is dried for standby for 60 DEG C after water cleaning copper foil surface.
(2) 134.45mg Copper dichloride dihydrate powder is added in 10ml deionized water, is stirred 2 minutes, configuration~
The copper chloride solution of 0.1mol/L.Copper chloride solution is added in 1.63mg anhydrous ferric trichloride powder.
(3) by 10mL~copper chloride solution of 0.1mol/L is added drop-wise to the burnishing surface of copper foil, by bar coating method
Liquid is uniformly dispersed in copper foil surface, forms the film of uniformly continuous.
(4) copper foil for carrying copper chloride solution is placed in the baking oven that temperature is 60 DEG C and is dried 5min.
(5) it is collected after scraping the cuprous chloride crystal of copper foil surface with blade, it is brilliant with washes of absolute alcohol stannous chloride
Body powder is coated on silicon wafer after ethyl alcohol stirring is added.
(6) by the 2 of 0.249g, 4,6- triethylbenzenes -1,3,5- trimethylamine is dissolved in 1.0mL acetonitrile, is divided into several pieces,
Again to the acetonitrile solution for being separately added into respective volume in every part, 1mmol/mL, 0.5mmol/mL, 0.4mmol/mL are configured,
The solution of 0.3mmol/mL, 0.2mmol/mL, 0.1mmol/mL, 0.05mmol/mL, 0.01mmol/mL.
(7) the 1 of 1mmol/mL, 3,5- triaminobenzene acetonitrile solution is coated on and is loaded with two-dimentional stannous chloride nanocrystal material
Expect silicon chip surface, temperature setting is room temperature, and half an hour is maintained in closed container.
(8) closed container ventilation is opened, after acetonitrile volatilization completely, the 1 of drop coating 0.5mmol/mL, 3,5- triaminobenzene second
Nitrile solution, temperature setting are room temperature, and half an hour is maintained in closed container.
(9) closed container ventilation is opened, after acetonitrile volatilization completely, the 1 of drop coating 0.4mmol/mL, 3,5- triaminobenzene second
Nitrile solution, temperature setting are room temperature, and half an hour is maintained in closed container.
(10) closed container ventilation is opened, after acetonitrile volatilization completely, the 1 of drop coating 0.3mmol/mL, 3,5- triaminobenzenes
Acetonitrile solution, temperature setting are room temperature, and half an hour is maintained in closed container.
(11) closed container ventilation is opened, after acetonitrile volatilization completely, the 1 of drop coating 0.2mmol/mL, 3,5- triaminobenzenes
Acetonitrile solution, temperature setting are room temperature, and half an hour is maintained in closed container.
(12) closed container ventilation is opened, after acetonitrile volatilization completely, the 1 of drop coating 0.1mmol/mL, 3,5- triaminobenzenes
Acetonitrile solution, temperature setting are room temperature, and half an hour is maintained in closed container.
(13) closed container ventilation is opened, after acetonitrile volatilization completely, the 1 of drop coating 0.05mmol/mL, 3,5- triaminobenzenes
Acetonitrile solution, temperature setting are room temperature, and half an hour is maintained in closed container.
(14) closed container ventilation is opened, after acetonitrile volatilization completely, the 1 of drop coating 0.01mmol/mL, 3,5- triaminobenzenes
Acetonitrile solution, temperature setting are room temperature, and half an hour is maintained in closed container.
Embodiment 3
(1) copper foil of 25um thickness is selected, the one side of copper foil or two sides are the planes by polishing treatment, use deionization
It is dried for standby for 60 DEG C after water cleaning copper foil surface.
(2) 134.45mg Copper dichloride dihydrate powder is added in 10ml deionized water, is stirred 2 minutes, configuration~
The copper chloride solution of 0.1mol/L.Copper chloride solution is added in 1.63mg anhydrous ferric trichloride powder.
(3) by 10mL~copper chloride solution of 0.1mol/L is added drop-wise to the burnishing surface of copper foil, by bar coating method
Liquid is uniformly dispersed in copper foil surface, forms the film of uniformly continuous.
(4) copper foil for carrying copper chloride solution is placed in the baking oven that temperature is 60 DEG C and is dried 5min.
(5) it is collected after scraping the cuprous chloride crystal of copper foil surface with blade, it is brilliant with washes of absolute alcohol stannous chloride
Body powder is coated on silicon wafer after ethyl alcohol stirring is added.
(6) by the 2 of 0.165g, 4,6- trimethylbenzenes -1,3,5- triamine is dissolved in 1.0mL acetonitrile, is divided into several pieces, then
To the acetonitrile solution for being separately added into respective volume in every part, 1mmol/mL, 0.5mmol/mL, 0.4mmol/mL are configured,
The solution of 0.3mmol/mL, 0.2mmol/mL, 0.1mmol/mL, 0.05mmol/mL, 0.01mmol/mL.
(7) the 1 of 1mmol/mL, 3,5- triaminobenzene acetonitrile solution is coated on and is loaded with two-dimentional stannous chloride nanocrystal material
Expect silicon chip surface, temperature setting is room temperature, and half an hour is maintained in closed container.
(8) closed container ventilation is opened, after acetonitrile volatilization completely, the 1 of drop coating 0.5mmol/mL, 3,5- triaminobenzene second
Nitrile solution, temperature setting are room temperature, and half an hour is maintained in closed container.
(9) closed container ventilation is opened, after acetonitrile volatilization completely, the 1 of drop coating 0.2mmol/mL, 3,5- triaminobenzene second
Nitrile solution, temperature setting are room temperature, and half an hour is maintained in closed container.
(10) closed container ventilation is opened, after acetonitrile volatilization completely, the 1 of drop coating 0.1mmol/mL, 3,5- triaminobenzenes
Acetonitrile solution, temperature setting are room temperature, and half an hour is maintained in closed container.
(11) closed container ventilation is opened, after acetonitrile volatilization completely, the 1 of drop coating 0.05mmol/mL, 3,5- triaminobenzenes
Acetonitrile solution, temperature setting are room temperature, and half an hour is maintained in closed container.
(12) closed container ventilation is opened, after acetonitrile volatilization completely, the 1 of drop coating 0.01mmol/mL, 3,5- triaminobenzenes
Acetonitrile solution, temperature setting are room temperature, and half an hour is maintained in closed container.
Embodiment 4
(1) copper foil of 25um thickness is selected, the one side of copper foil or two sides are the planes by polishing treatment, use deionization
It is dried for standby for 60 DEG C after water cleaning copper foil surface.
(2) 134.45mg Copper dichloride dihydrate powder is added in 10ml deionized water, is stirred 2 minutes, configuration~
The copper chloride solution of 0.1mol/L.Copper chloride solution is added in 1.63mg anhydrous ferric trichloride powder.
(3) by 10mL~copper chloride solution of 0.1mol/L is added drop-wise to the burnishing surface of copper foil, by bar coating method
Liquid is uniformly dispersed in copper foil surface, forms the film of uniformly continuous.
(4) copper foil for carrying copper chloride solution is placed in the baking oven that temperature is 60 DEG C and is dried 5min.
(5) it is collected after scraping the cuprous chloride crystal of copper foil surface with blade, it is brilliant with washes of absolute alcohol stannous chloride
Body powder is coated on silicon wafer after ethyl alcohol stirring is added.
(6) by the 1 of 0.258g, 3,5- triamido -2,4,6- trinitrobenzen is dissolved in 1.0mL acetonitrile, is divided into several pieces,
Again to the acetonitrile solution for being separately added into respective volume in every part, 1mmol/mL, 0.5mmol/mL, 0.4mmol/mL are configured,
The solution of 0.3mmol/mL, 0.2mmol/mL, 0.1mmol/mL, 0.05mmol/mL, 0.01mmol/mL.
(7) the 1 of 1mmol/mL, 3,5- triaminobenzene acetonitrile solution is coated on and is loaded with two-dimentional stannous chloride nanocrystal material
Expect silicon chip surface, temperature setting is room temperature, and half an hour is maintained in closed container.
(8) closed container ventilation is opened, after acetonitrile volatilization completely, the 1 of drop coating 0.5mmol/mL, 3,5- triaminobenzene second
Nitrile solution, temperature setting are room temperature, and half an hour is maintained in closed container.
(9) closed container ventilation is opened, after acetonitrile volatilization completely, the 1 of drop coating 0.2mmol/mL, 3,5- triaminobenzene second
Nitrile solution, temperature setting are room temperature, and half an hour is maintained in closed container.
(10) closed container ventilation is opened, after acetonitrile volatilization completely, the 1 of drop coating 0.1mmol/mL, 3,5- triaminobenzenes
Acetonitrile solution, temperature setting are room temperature, and half an hour is maintained in closed container.
(11) closed container ventilation is opened, after acetonitrile volatilization completely, the 1 of drop coating 0.05mmol/mL, 3,5- triaminobenzenes
Acetonitrile solution, temperature setting are room temperature, and half an hour is maintained in closed container.
(12) closed container ventilation is opened, after acetonitrile volatilization completely, the 1 of drop coating 0.01mmol/mL, 3,5- triaminobenzenes
Acetonitrile solution, temperature setting are room temperature, and half an hour is maintained in closed container.
The Applicant declares that the present invention is explained by the above embodiments detailed process equipment and process flow of the invention,
But the present invention is not limited to the above detailed process equipment and process flow, that is, it is above-mentioned detailed not mean that the present invention must rely on
Process equipment and process flow could be implemented.It should be clear to those skilled in the art, any improvement in the present invention,
Addition, selection of concrete mode of equivalence replacement and auxiliary element to each raw material of product of the present invention etc., all fall within of the invention
Within protection scope and the open scope.
Claims (6)
1. a kind of interface preparation method of two dimension organic framework materials, includes the following steps:
(1) ethanol solution of copper chloride and ferric trichloride is coated on copper foil surface, at a certain range of temperature and in the time
Make rapid reaction, the two-dimentional stannous chloride nanocrystal material for playing template and catalytic action is directly prepared in copper foil substrate
Material, evenly spreads to after being cleaned with ethyl alcohol on smooth silicon wafer；
(2) selecting 1,3,5- triaminobenzenes etc. to have the aromatic amino compound of similar symmetrical structure is monomer molecule, is dissolved in
Matched solution is coated on and is loaded with two-dimentional stannous chloride nano crystal material silicon wafer table by acetonitrile and the solution for being configured to various concentration
Face maintains half an hour rear venting sequentially to drip from high concentration to low concentration after acetonitrile volatilization completely in closed container at room temperature
Aromatic amino compound acetonitrile solution is applied, is repeated several times, in two-dimentional stannous chloride nanocrystal surface growing large-area two dimension
Organic framework materials.
2. preparation method according to claim 1, which is characterized in that ferric trichloride adds in ethanol solution in step (1)
The range of amount is the 0.01%-10% of copper chloride solution molar concentration.
3. preparation method according to claim 1, which is characterized in that described in step (1) at a certain range of temperature
Occur with rapid reaction in the time, preferred temperature is 0~80 DEG C, and the preferred time is 0.1~600s.
4. preparation method according to claim 1, which is characterized in that have similar symmetrical structure described in step (2)
Aromatic amino compound include 2,4,6- triethylbenzenes -1,3,5- trimethylamine, 2,4,6- trimethylbenzenes -1,3,5- triamine, 1,
3,5- triamidos -2,4,6- trinitrobenzen etc..
5. preparation method according to claim 1, which is characterized in that aromatic amino compound second described in step (2)
Nitrile solution concentration be 1mmol/mL, 0.5mmol/mL, 0.4mmol/mL, 0.3mmol/mL, 0.2mmol/mL, 0.1mmol/mL,
0.05mmol/mL, 0.01mmol/mL etc..
6. preparation method according to claim 1, which is characterized in that described in step (2) sequentially the number of drop coating be 2~
20 times, solution concentration is randomly choosed according to sequence from high to low, and the selection of solution concentration can repeat.
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Cited By (1)
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| CN109894082A (en) * | 2019-02-21 | 2019-06-18 | 浙江大学 | A kind of preparation method and application of the covalent organic frame composite material of nanometer of flower pattern |
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Application publication date: 20190118 |