CN115430594A - Dynamically reconfigurable plasma two-dimensional ordered nano array and three-dimensional chiral nano array and preparation method thereof - Google Patents

Dynamically reconfigurable plasma two-dimensional ordered nano array and three-dimensional chiral nano array and preparation method thereof Download PDF

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CN115430594A
CN115430594A CN202211138047.5A CN202211138047A CN115430594A CN 115430594 A CN115430594 A CN 115430594A CN 202211138047 A CN202211138047 A CN 202211138047A CN 115430594 A CN115430594 A CN 115430594A
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CN115430594B (en
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聂志鸿
王亚子
李红艳
叶顺盛
杨帆
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Yiwu Research Institute Of Fudan University
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    • B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
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Abstract

The invention relates to a dynamic reconfigurable plasma two-dimensional ordered nano array and a three-dimensional chiral nano array and a preparation method thereof, wherein the method comprises the following steps: modifying the magnetic-plasma nano hybrid rod; sequentially carrying out silane modification and nanosphere photoetching technology treatment on the matrix; placing the patterned substrate in a nano hybrid rod solution with negative charges, applying a magnetic field in the horizontal direction, and performing adsorption orientation to obtain a two-dimensional ordered nano array; modifying the nanometer hybrid rod of the two-dimensional ordered nanometer array, and then carrying out polymer film spin coating on the array; and (3) placing the treated two-dimensional ordered nano array in a nano hybridization rod solution with negative charges, adjusting the horizontal direction of a magnetic field, and adsorbing and orienting to obtain the three-dimensional chiral nano array. The invention can obtain the nano array structure with dynamic reconfigurable chiral optical properties by self-assembling the magnetic field induced nano particles, has simple preparation and low price, and is suitable for large-area production.

Description

Dynamically reconfigurable plasma two-dimensional ordered nano array and three-dimensional chiral nano array and preparation method thereof
Technical Field
The invention relates to the field of nanoparticle self-assembly, in particular to a dynamically reconfigurable plasma two-dimensional ordered nano array and a three-dimensional chiral nano array and preparation methods thereof.
Background
The super surface is a two-dimensional super material formed by artificial structural units with sub-wavelength thickness, has the advantages of low optical loss, easiness in preparation and integration and the like, can flexibly regulate and control the amplitude, phase and polarization state of electromagnetic waves, and has wide application prospects in the fields of lenses, biosensing, imaging and the like. The development of super-surfaces is dependent on innovations in processing technology. The common super-surface preparation technologies mainly comprise: electron beam lithography, focused ion beam lithography, interference lithography, nanoimprint, self-assembly techniques, and the like.
Although the use of "top-down" lithography techniques is well established, there are still some problems that need to be solved: (1) Materials are limited, usually requiring photolithography over hard materials such as silicon wafers, metal films; (2) the technology is complex, and large-scale preparation is difficult; and (3) the controllability is poor, and the material is difficult to dynamically regulate and control. In contrast, "bottom-up" colloidal self-assembly techniques are more flexible, in that they spontaneously assemble previously synthesized colloidal particles into ordered complex structures. The size, the morphology, the crystallinity and the like of the colloid particles can be reasonably controlled through physical and chemical reactions, so that high-quality artificial structural units can be obtained, and the preparation of the high-performance super-surface material is facilitated.
In the use process of the self-assembly technology, a template is usually needed, the template has the function of providing specific binding sites for the colloidal particles, and the template can be flexibly designed according to the size, the shape, the surface property and the like of the colloidal particles. However, as with the photolithography technique, it is still difficult to prepare precise, dynamic, and complex micro-nano three-dimensional structures in a large area by the current self-assembly technique.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a dynamic reconfigurable plasma two-dimensional ordered nano array and a three-dimensional chiral nano array which have accurate, dynamic and complex micro-nano three-dimensional structures, simple process and low price and are suitable for large-area production, and a preparation method thereof.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of a dynamic reconfigurable plasma two-dimensional ordered nano array comprises the following steps:
modifying the magnetic-plasma nano hybrid rod to make the surface of the nano hybrid rod have negative charges to obtain a nano hybrid rod solution with negative charges;
sequentially carrying out silane modification and nanosphere photoetching technology treatment on the substrate to form periodic sites with positive charges on the surface of the substrate to obtain a patterned substrate;
and (3) placing the patterned substrate in a nano hybrid rod solution with negative charges, applying a magnetic field, and adsorbing and taking the substrate backwards to obtain the dynamically reconfigurable plasma two-dimensional ordered nano array.
Further, the magnetic-plasma nano hybrid rod comprises Fe 3 O 4 -Au nano hybrid rod, fe 3 O 4 -an Ag nano hybrid rod, a Co3O4-Au nano hybrid rod, a Co3O4-Ag nano hybrid rod, a NiO-Au nano hybrid rod or a NiO-Ag nano hybrid rod, having a diameter of 20-100nm and a length of 50-800nm; the modifier used in the modification process comprises citrate.
Further, the substrate comprises a silicon wafer or a quartz wafer; the silane used in the silane modification includes an aminosilane coupling agent; the nanospheres are polystyrene nanospheres, and the size of the nanospheres is 200-1000nm.
Further, the specific process of forming the patterned substrate comprises the following steps:
(1) Placing the substrate in a silane solution, reacting, and drying to complete silane modification;
(2-1) dispersing the nanospheres into a solvent to prepare a nanosphere solution;
(2-2) injecting the nanosphere solution to form a compact single-layer nanosphere film, and transferring the film onto a silane modified substrate;
and (2-3) heating, plasma etching and cleaning the substrate in sequence, and then finishing the nanosphere photoetching technology treatment to form the patterned substrate with periodic sites.
Further, the silane solution comprises an alcohol solution of silane, and the solvent comprises alcohol and/or water.
A dynamic reconfigurable plasma two-dimensional ordered nano array prepared by the method.
A preparation method of a dynamic reconfigurable plasma three-dimensional chiral nano array comprises the following steps:
modifying the two-dimensional ordered nano array to make the surface of the two-dimensional ordered nano array positively charged, and then carrying out polymer film spin coating on the two-dimensional ordered nano array to expose the upper surface of the nano hybridization rod;
and (3) placing the processed two-dimensional ordered nano array in a nano hybrid rod solution with negative charges, adjusting the direction of a magnetic field, and adsorbing and orienting to obtain the dynamically reconfigurable plasma three-dimensional chiral nano array.
Further, the spin coating of the polymer film comprises the following specific steps: and spin-coating the polymer solution on the surface of the array, and heating in vacuum to separate the polymer from the nano-hybrid rod, thereby completing the spin coating of the polymer film.
Furthermore, the strength of the magnetic field is 600-6000Gs, and the time of adsorption orientation is 2-12h.
A dynamic reconfigurable plasma three-dimensional chiral nano-array prepared by the method.
Compared with the prior art, the invention has the following advantages:
(1) The invention can prepare accurate, dynamic and complex micro-nano three-dimensional structure in large area;
(2) The invention can obtain the nano array structure with dynamic reconfigurable chiral optical properties by self-assembling the magnetic field induced nano particles, has simple preparation and low price and is suitable for large-area production.
Drawings
FIG. 1 is a flow chart of the preparation of two-dimensional ordered nanoarrays in the examples.
FIG. 2 is a flow chart of the preparation of the three-dimensional chiral nano-array in the example.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the protection scope of the present invention is not limited to the following embodiments.
A preparation method of a dynamic reconfigurable plasma two-dimensional ordered nano array and a three-dimensional chiral nano array comprises the following steps:
(1) Modifying the magnetic-plasma nano hybrid rod to make the surface thereof have negative charges; the magnetic-plasma nano hybrid rod is Fe 3 O 4 -Au nano hybrid rod, fe 3 O 4 -one of an Ag nano hybrid rod, a Co3O4-Au nano hybrid rod, a Co3O4-Ag nano hybrid rod, a NiO-Au nano hybrid rod, and a NiO-Ag nano hybrid rod; the diameter of the nano hybrid rod is 20-100nm, and the length of the nano hybrid rod is 50-800nm; the modifier of the nano hybrid rod is a citrate compound.
(2) Sequentially carrying out silane modification and nanosphere photoetching technology treatment on the substrate to form periodic sites with positive charges on the surface of the substrate; the substrate is one of a silicon wafer or a quartz wafer; the silane is an aminosilane coupling agent; the nanospheres are polystyrene nanospheres, and the size of the nanospheres is 200-1000nm.
(3) And (3) placing the patterned substrate in a nano hybrid rod solution with negative charges, applying a magnetic field in the horizontal direction, and adsorbing and orienting to obtain the two-dimensional ordered nano array. The intensity of the magnetic field is 600-6000Gs; the time of adsorption orientation is 2-12h.
(4) Modifying the nano hybrid rod of the two-dimensional ordered nano array to make the surface of the nano hybrid rod positively charged, and then carrying out polymer film spin coating on the array to expose the upper surface of the nano hybrid rod; the modifier of the nano hybrid rod is poly-4-vinylpyridine; the polymer film is polymethyl methacrylate and has a thickness of 10-60nm.
(5) And (3) placing the treated two-dimensional ordered nano array in a nano hybrid rod solution with negative charges, adjusting the horizontal direction of a magnetic field, and adsorbing and orienting to obtain the three-dimensional chiral nano array. The intensity of the magnetic field is 600-6000Gs; the time of adsorption orientation is 2-12h.
Example 1
Preparing a two-dimensional ordered nano array: fe with the diameter of 20nm and the length of 50nm 3 O 4 And (4) placing the Au nano hybrid rod in a sodium citrate solution, and stirring for 12h. Putting the silicon wafer into an ethanol solution containing 3-aminopropyltrimethoxysilane (the volume fraction is 0.2 percent), reacting for 30min, washing the silicon wafer with ethanol, and drying the silicon wafer in a 120 ℃ oven for 1.5h. Dispersing Polystyrene (PS) nanospheres with the size of 200nm into a mixed solution of ethanol and deionized water (volume ratio is 1. And (3) drying the silicon wafer in a drying oven at 110 ℃ for 5min, treating for 60s by using a plasma cleaning machine, then putting the silicon wafer into ethanol, and ultrasonically removing the PS nanospheres on the silicon wafer to form a periodic site structure. Immersing a silicon wafer having periodic sites in Fe 3 O 4 And (3) placing the Au nano hybrid rod solution between two magnets, setting the magnetic field intensity to be 6000Gs, standing for 12h, taking out the silicon wafer, and washing the silicon wafer with deionized water to obtain the two-dimensional ordered nano array.
Preparing a three-dimensional chiral nano array: immersing the two-dimensional ordered nano array in an ethanol solution containing 1% poly 4-vinylpyridine (P4 VP), standing for 12h, washing a silicon wafer with absolute ethanol, drying, spin-coating a toluene solution containing polymethyl methacrylate (PMMA) on the surface of the array, then placing the array in a vacuum drier, placing a weighing bottle containing 5mL of tetrahydrofuran/toluene (volume ratio 1) mixed solvent at the bottom of the drier in advance, pumping the vacuum degree in the container to 30mbr by using a vacuum pump, then placing the container in an oven at 35 ℃ for 30min, and enabling the PMMA film and Fe to be mixed in an oven, wherein the vacuum degree is controlled by a control unit, and the temperature of the oven is controlled by the control unit 3 O 4 And the Au nano hybrid rods are subjected to phase separation, and the thickness of the PMMA film is controlled to be about 10 nm. Finally, the treated array was immersed in Fe 3 O 4 And (3) placing the Au nano hybrid rod solution between two magnets, setting the magnetic field intensity to be 6000Gs, standing for 12h, taking out the silicon wafer, and washing the silicon wafer with deionized water to obtain the three-dimensional chiral nano array.
Example 2
Preparing a two-dimensional ordered nano array: fe with the diameter of 60nm and the length of 360nm 3 O 4 And (3) putting the-Ag nano hybrid rod into a sodium citrate solution, and stirring for 12 hours. Putting the silicon wafer into an ethanol solution containing 3-aminopropyltrimethoxysilane (the volume fraction is 0.2 percent), reacting for 30min, washing the silicon wafer with ethanol, and drying the silicon wafer in a 120 ℃ oven for 1.5h. Dispersing PS nanospheres with the size of 700nm into a mixed solution of ethanol and deionized water (volume ratio is 1. And (3) drying the silicon wafer in a drying oven at 110 ℃ for 5min, treating for 60s by using a plasma cleaning machine, then putting the silicon wafer into ethanol, and ultrasonically removing the PS nanospheres on the silicon wafer to form a periodic site structure. Immersing a silicon wafer having periodic sites in Fe 3 O 4 And (3) putting the Ag nano hybrid rod solution between two magnets, setting the magnetic field intensity to 2800Gs, standing for 6h, taking out the silicon wafer, and washing the silicon wafer with deionized water to obtain the two-dimensional ordered nano array.
Preparing a three-dimensional chiral nano array: immersing the two-dimensional ordered nano array in an ethanol solution containing 1% P4VP, standing for 12h, washing the silicon wafer with absolute ethanol, drying, spin-coating a toluene solution containing PMMA on the surface of the array, putting the array in a vacuum drier, placing a weighing bottle containing 5mL of tetrahydrofuran/toluene (volume ratio 1) 3 O 4 The Ag nano hybrid rod is subjected to phase separation, and the thickness of the PMMA film is controlled to be about 46 nm. Finally, the treated array was immersed in Fe 3 O 4 And (3) putting the Ag nano hybrid rod solution between two magnets, setting the magnetic field intensity to 2800Gs, standing for 6h, taking out the silicon wafer, and washing the silicon wafer with deionized water to obtain the three-dimensional chiral nano array.
Example 3
Preparing a two-dimensional ordered nano array: fe with the diameter of 100nm and the length of 800nm 3 O 4 -Ag and Fe 3 O 4 And (4) respectively placing the Au nano hybrid rods in a sodium citrate solution, and stirring for 12h. Putting the silicon chip into an ethanol solution containing 3-aminopropyltriethoxysilane (volume fraction of 0.2%), reacting for 30min, washing with ethanol, and oven drying at 120 deg.C for 1.5h. Dispersing PS nanospheres with the size of 1000nm into a mixed solution of ethanol and deionized water (volume ratio is 1. And (3) drying the silicon wafer in a drying oven at 110 ℃ for 5min, treating for 60s by using a plasma cleaning machine, then putting the silicon wafer into ethanol, and ultrasonically removing the PS nanospheres on the silicon wafer to form a periodic site structure. Immersing a silicon wafer having periodic sites in Fe 3 O 4 And (3) placing the Ag nano hybrid rod solution between two magnets, setting the magnetic field intensity to be 600Gs, standing for 2h, taking out the silicon wafer, and washing the silicon wafer with deionized water to obtain the two-dimensional ordered nano array.
Preparation of three-dimensional chiral nano-array: immersing the two-dimensional ordered nano array in an ethanol solution containing 1% P4VP, standing for 12h, washing the silicon wafer with absolute ethanol, drying, spin-coating a toluene solution containing PMMA on the surface of the array, putting the array in a vacuum drier, placing a weighing bottle containing 5mL of tetrahydrofuran/toluene (volume ratio 1) 3 O 4 The Ag nano hybrid rod is subjected to phase separation, and the thickness of the PMMA film is controlled to be about 60nm. Finally, the treated array was immersed in Fe 3 O 4 And (3) placing the Au nano hybrid rod solution between two magnets, setting the magnetic field intensity to be 600Gs, standing for 2h, taking out the silicon wafer, and washing the silicon wafer with deionized water to obtain the three-dimensional chiral nano array.
Example 4
Preparing a two-dimensional ordered nano array: and putting the NiO-Ag nano hybrid rod with the diameter of 60nm and the length of 360nm into a sodium citrate solution, and stirring for 12h. Putting the silicon chip into an ethanol solution containing 3-aminopropyltriethoxysilane (volume fraction of 0.2%), reacting for 30min, washing with ethanol, and oven drying at 120 deg.C for 1.5h. Dispersing PS nanospheres with the size of 700nm into a mixed solution of ethanol and deionized water (volume ratio is 1. And (3) drying the silicon wafer in a drying oven at 110 ℃ for 5min, treating for 60s by using a plasma cleaning machine, then putting the silicon wafer into ethanol, and ultrasonically removing the PS nanospheres on the silicon wafer to form a periodic site structure. And (3) immersing the silicon wafer with periodic sites into a NiO-Ag nano hybrid rod solution, placing the silicon wafer between two magnets, setting the magnetic field intensity to 2800Gs, standing for 6h, taking out the silicon wafer, and washing the silicon wafer with deionized water to obtain the two-dimensional ordered nano array.
Preparing a three-dimensional chiral nano array: immersing the two-dimensional ordered nano array in an ethanol solution containing 1 percent of P4VP, standing for 12 hours, washing a silicon wafer by absolute ethanol, drying, spin-coating a toluene solution containing PMMA on the surface of the array, putting the array into a vacuum drier, placing a weighing bottle containing 5mL of tetrahydrofuran/toluene (volume ratio 1. And finally, immersing the processed array into a NiO-Ag nano hybrid rod solution, placing the NiO-Ag nano hybrid rod solution between two magnets, setting the magnetic field intensity to 2800Gs, standing for 6 hours, taking out the silicon wafer, and washing the silicon wafer with deionized water to obtain the three-dimensional chiral nano array.
Example 5
Preparing a two-dimensional ordered nano array: niO-Au and Co3O4-Ag nano hybrid rods with the diameter of 60nm and the length of 360nm are respectively placed in a sodium citrate solution and stirred for 12 hours. Putting the quartz plate into an ethanol solution containing 3-aminopropyltrimethoxysilane (the volume fraction is 0.2 percent), reacting for 30min, washing the quartz plate with ethanol, and drying the quartz plate in a 120 ℃ drying oven for 1.5h. The method comprises the steps of dispersing PS nanospheres with the size of 700nm into a mixed solution of ethanol and deionized water (volume ratio is 1. And (3) drying the quartz plate in a drying oven at 110 ℃ for 5min, treating for 60s by using a plasma cleaning machine, then putting into ethanol, and ultrasonically removing the PS nanospheres on the quartz plate to form a periodic site structure. And (3) immersing a quartz plate with periodic sites into the NiO-Au nano hybrid rod solution, placing the quartz plate between two magnets, setting the magnetic field intensity to 2800Gs, standing for 6h, taking out the quartz plate, and washing the quartz plate by deionized water to obtain the two-dimensional ordered nano array.
Preparing a three-dimensional chiral nano array: immersing the two-dimensional ordered nano array in an ethanol solution containing 1 percent of P4VP, standing for 12h, washing a quartz plate with absolute ethanol, drying, spin-coating a toluene solution containing PMMA on the surface of the array, putting the array into a vacuum drier, placing a weighing bottle containing 5mL of tetrahydrofuran/toluene (volume ratio 1. And finally, immersing the processed array into a Co3O4-Ag nano hybrid rod solution, placing the mixture between two magnets, setting the magnetic field intensity to 2800Gs, standing for 6 hours, taking out a quartz plate, and washing the quartz plate with deionized water to obtain the three-dimensional chiral nano array.
The foregoing is directed to preferred embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention will still fall within the protection scope of the technical solution of the present invention.

Claims (10)

1. A preparation method of a dynamically reconfigurable plasma two-dimensional ordered nano array is characterized by comprising the following steps:
modifying the magnetic-plasma nano hybrid rod to make the surface of the nano hybrid rod have negative charges to obtain a nano hybrid rod solution with negative charges;
sequentially carrying out silane modification and nanosphere photoetching technology treatment on the substrate to form periodic sites with positive charges on the surface of the substrate to obtain a patterned substrate;
and (3) placing the patterned substrate in a nano hybrid rod solution with negative charges, applying a magnetic field, and adsorbing and taking the substrate backwards to obtain the dynamically reconfigurable plasma two-dimensional ordered nano array.
2. The method for preparing a dynamically reconfigurable plasma two-dimensional ordered nano array according to claim 1, wherein the magnetic-plasma nano hybrid rods comprise Fe 3 O 4 -Au nano hybrid rod, fe 3 O 4 -Ag nano hybrid rod, co 3 O 4 -Au nano hybrid rod, co 3 O 4 -Ag nano hybrid rods, niO-Au nano hybrid rods or NiO-Ag nano hybrid rods, the diameter is 20-100nm, and the length is 50-800nm; the modifier used in the modification process comprises citrate.
3. The method for preparing the dynamically reconfigurable plasma two-dimensional ordered nano array according to claim 1, wherein the substrate comprises a silicon wafer or a quartz wafer; the silane used in the silane modification includes an aminosilane coupling agent; the nanospheres are polystyrene nanospheres, and the size of the nanospheres is 200-1000nm.
4. The preparation method of the dynamically reconfigurable plasma two-dimensional ordered nano array according to claim 1, wherein the specific process of forming the patterned substrate comprises the following steps:
(1) Placing the substrate in a silane solution, reacting, and drying to complete silane modification;
(2-1) dispersing the nanospheres into a solvent to prepare a nanosphere solution;
(2-2) injecting the nanosphere solution to form a compact single-layer nanosphere film, and transferring the film onto a silane-modified substrate;
and (2-3) heating, plasma etching and cleaning the substrate in sequence, and then finishing the nanosphere photoetching technology treatment to form the patterned substrate with periodic sites.
5. The method according to claim 4, wherein the silane solution comprises an alcohol solution of silane, and the solvent comprises alcohol and/or water.
6. A dynamically reconfigurable plasma two-dimensional ordered nanoarray prepared by the method of any one of claims 1 to 5.
7. A preparation method of a dynamic reconfigurable plasma three-dimensional chiral nano array is characterized by comprising the following steps:
modifying the two-dimensional ordered nano array of claim 6 to make the surface of the two-dimensional ordered nano array positively charged, and then performing polymer film spin coating on the two-dimensional ordered nano array to expose the upper surface of the nano hybrid rod;
and (3) placing the processed two-dimensional ordered nano array in a nano hybrid rod solution with negative charges, adjusting the direction of a magnetic field, and adsorbing and orienting to obtain the dynamically reconfigurable plasma three-dimensional chiral nano array.
8. The method for preparing the dynamically reconfigurable plasma three-dimensional chiral nanoarray according to claim 7, wherein the spin coating of the polymer film comprises the following specific steps: and spin-coating the polymer solution on the surface of the array, and heating in vacuum to separate the polymer from the nano-hybrid rod, thereby completing the spin coating of the polymer film.
9. The method for preparing the three-dimensional chiral nano array of the dynamically reconfigurable plasma according to claim 7, wherein the strength of the magnetic field is 600-6000Gs, and the time of adsorption orientation is 2-12h.
10. A dynamically reconfigurable plasma three-dimensional chiral nanoarray prepared by the method of any one of claims 7 to 9.
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