CN110423305B - Preparation of Fe3O4Method for @ PVP @ PNIPAM magnetic photonic crystal nano-chain particles - Google Patents
Preparation of Fe3O4Method for @ PVP @ PNIPAM magnetic photonic crystal nano-chain particles Download PDFInfo
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Abstract
The invention relates to a method for regulating Fe3O4The simple and controllable method for the distance between the @ PVP @ PNIPAM photonic crystal nano-chain particles regulates and controls Fe by adjusting the concentration of polyacrylic acid aqueous solution or/and the quantity ratio of methylene bisacrylamide to N-isopropylacrylamide in a reaction system3O4The particle spacing of the @ PVP @ PNIPAM magnetic photonic crystal nano-chain is changed, the concentration of the polyacrylic acid aqueous solution is changed within the range of 0.33-1.09 g/L, and the quantity ratio of the methylene bisacrylamide to the N-isopropylacrylamide is changed within the range of 0.01-0.1. Due to the adoption of the technical scheme, compared with the prior art, the invention has the following advantages and positive effects: 1) the method is simple, efficient, low in cost, good in controllability and repeatability and easy to apply and popularize in industry. 2) The brightness and the chroma are wide in regulation and control range, and the regulation and control method is simple and efficient.
Description
Technical Field
The invention relates to the technical field of magnetic nano materials, in particular to Fe regulation and control3O4@ PVP @ PNIPAM lightA simple, controllable method of sub-crystalline nanochain particle spacing.
Background
Compared with the traditional inorganic pigment and organic dye, the structural color has the advantages of environmental protection, energy conservation, fastness, easy adjustment and the like, has important potential application in the fields of visual sensing, display, anti-counterfeiting, camouflage and the like, and the magnetic photonic crystal is an important structural color material and is concerned because of the advantages of simple preparation method, high response speed, reversible response and the like. According to the Bragg law, the structural color of the one-dimensional magnetic photonic crystal nanochain is mainly determined by the particle size and the particle distance, and is currently based on superparamagnetic ferroferric oxide (Fe)3O4) The preparation of one-dimensional magnetic photonic crystals of colloidal nanoparticles and the color control thereof have made important research progress. The document [ Angew. chem. int. Ed.,2011,50, 3747-3750 ] discloses a silicon dioxide (SiO)2) Coated with superparamagnetic Fe3O4The nano-chain of the colloidal nano-particles obtains Fe under the action of an external magnetic field3O4@SiO2The nanochain shows stable structural color, changes the direction of an external magnetic field, can realize color display and hiding, and uses Fe with different sizes3O4The colloid nano particles are assembly elements, and can be used for preparing nano chains with three colors of red, green and blue. The document [ Nanoscale,2017,9,3105-2) Coated with superparamagnetic Fe3O4The nanorod of the colloidal nanoparticle realizes the regulation and control of color brightness based on the regulation and control of lattice defects under different magnetic field strengths. The nanorods with different particle distances can be prepared by changing the external magnetic field strength in the preparation process. Patents [ CN 104629232 a ] and documents [ Nano lett, 2018, DOI: 10.1021/acs. nanolett.7b04218 ] disclose a responsive magnetic photonic crystal chain that enables dynamic, fast, reversible modulation of color based on volume changes of a responsive gel layer under external field stimulation. At present, the color control of the magnetic photonic crystal nano-chain is mainly realized by adjusting the size of an assembly element, the intensity of an external magnetic field and environmental stimulation, and the methods have complex process and need to equipment and environmentThe method has the advantages of solving the defects of high product quality and the like, and has important significance in developing a simple, efficient and controllable method for preparing photonic crystal nano-chains with different colors.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: provides a method for regulating Fe3O4The method for the distance between the @ PVP @ PNIPAM magnetic photonic crystal nano-chain particles does not need to change the particle size and the size of an external magnetic field, has the advantages of simplicity, high efficiency, low cost, good controllability and repeatability and the like, and can be used for treating Fe with different colors3O4The preparation of the @ PVP @ PNIPAM magnetic photonic crystal nano-chain has important significance.
The invention adopts the following technical scheme for solving the technical problems: regulation of Fe3O4The method for measuring the distance between the @ PVP @ PNIPAM magnetic photonic crystal nano-chain particles comprises the following steps:
s1, dispersing N-isopropylacrylamide, methylene bisacrylamide and 2-hydroxy-2-methyl propiophenone in the ferroferric oxide colloidal nanoparticle solution, and ultrasonically mixing uniformly to form a pre-polymerization solution;
s2 adding polyacrylic acid aqueous solution into the pre-polymerization solution, mixing uniformly by ultrasonic, applying external magnetic field, carrying out ultraviolet light initiated polymerization, centrifugally separating the product after the reaction is finished, washing the product with ethanol, and finally obtaining Fe3O4The @ PVP @ PNIPAM magnetic photonic crystal nano-chain is dispersed in water or ethanol;
wherein Fe is regulated and controlled by adjusting the concentration of polyacrylic acid aqueous solution or/and the quantity ratio of methylene bisacrylamide and N-isopropylacrylamide in the reaction system3O4The particle spacing of the @ PVP @ PNIPAM magnetic photonic crystal nano-chain is changed, the concentration of the polyacrylic acid aqueous solution is changed within the range of 0.33-1.09 g/L, and the quantity ratio of the methylene bisacrylamide to the N-isopropylacrylamide is changed within the range of 0.01-0.1.
According to the above scheme, Fe3O4The @ PVP @ PNIPAM magnetic photonic crystal nano-chain is dispersed in water, and the brightness and the chromaticity of the nano-chain can be adjusted by changing an external magnetic field and temperature respectively.
The polyacrylic acid contains a large amount of carboxyl, and can form hydrogen bonds with polyvinylpyrrolidone and N-isopropyl acrylamide of a ferroferric oxide colloid nanoparticle shell layer, the concentration of the polyacrylic acid in a reaction system influences the concentration of N-isopropyl acrylamide monomers around particles, the higher the concentration of the polyacrylic acid is, the higher the concentration of the monomers around the particles is, the polymerization of the monomers around the particles is facilitated, a compact polymer shell layer is formed, and the particles in the obtained nano chain are tightly connected, and the chain spacing is smaller. When the concentration of polyacrylic acid is lower, the concentration of monomers around the particles is low, the formed polymer shell is thin, the steric hindrance repulsion force between ferroferric oxide colloid nano particles in the obtained nano chain is larger, and the chain spacing is larger. When the content of the cross-linking agent methylene-bis-propyl acrylamide in the reaction system is high, after photo-initiated polymerization, the obtained poly-N-isopropyl acrylamide polymer among nano-chain particles has a compact network structure and smaller particle spacing. When the content of the cross-linking agent methylene-bis-propyl acrylamide in the reaction system is low, after photo-initiated polymerization, the obtained poly-N-isopropyl acrylamide polymer among nano-chain particles has a loose network structure and larger particle spacing.
Fe prepared by the method provided by the invention3O4The luminance and chromaticity regulation and control principle of the @ PVP @ PNIPAM magnetic photonic crystal nano-chain is as follows:
the prepared nano-chain is in a natural bending state when no external magnetic field exists, the chain gradually rotates and extends along with the increase of the external magnetic field, the periodicity along the magnetic field direction becomes good, the intensity of the diffraction peak of the chain increases along with the increase of the magnetic field intensity, the position of the diffraction peak does not change, and the brightness of the chain is visually shown to be adjustable under the same chromaticity. In addition, the poly-N-isopropylacrylamide as the shell layer has temperature sensitivity, and when the environmental temperature changes, the distance between nano-chain particles changes, and the chromaticity of the nano-chain particles also changes correspondingly.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following advantages and positive effects:
1) the method has the advantages of simple method, high efficiency, low cost, good controllability and repeatability, and easy industrial application and popularization.
2) The resulting Fe3O4The @ PVP @ PNIPAM magnetic photonic crystal nanochain aqueous dispersion has wide brightness and chromaticity regulation and control range, and the regulation and control method is simple and efficient, and has important potential application in the fields of display, visual sensing, anti-counterfeiting, camouflage and the like.
Drawings
FIG. 1 is a scanning electron micrograph of the product obtained in example 1;
FIG. 2 is a light microscopic bright field image of the product obtained in example 1;
FIG. 3 is an infrared spectrum of the product obtained in example 1;
FIG. 4 is a thermogravimetric plot of the product obtained in example 1;
FIG. 5 is a magnetic hysteresis loop diagram of the product obtained in example 1;
FIG. 6 is a spectrum of the product obtained in example 1 at different temperatures and magnetic field strengths;
FIG. 7 is a dark field diagram of the microscope showing the product of example 1 at 4 ℃ under different magnetic field strengths;
FIG. 8 is a dark field diagram of a microscope showing the product of example 1 at 32 degrees Celsius under different magnetic field strengths;
FIG. 9 is a dark field diagram of a microscope showing the product of example 1 at 38 degrees Celsius under different magnetic field strengths;
FIG. 10 is a scanning electron micrograph of a product obtained in example 2;
FIG. 11 is a light microscopic bright field image of the product obtained in example 2;
FIG. 12 is a spectrum of the products obtained in example 2 and example 3 at different magnetic field strengths;
FIG. 13 is an optical microscope dark field plot of the product obtained in example 2;
FIG. 14 is a scanning electron micrograph of a product obtained in example 3;
FIG. 15 is a light microscopic bright field image of the product obtained in example 3;
FIG. 16 is an optical microscope dark field plot of the product obtained in example 3;
FIG. 17 is a scanning electron micrograph of a product obtained in example 4;
FIG. 18 is a light microscopic bright field image of the product obtained in example 4;
FIG. 19 is a spectrum of the products obtained in examples 4 to 6 at different magnetic field strengths;
FIG. 20 is an optical microscope dark field plot of the product obtained in example 4;
FIG. 21 is a scanning electron micrograph of a product obtained in example 5;
FIG. 22 is a light microscopic bright field image of the product obtained in example 5;
FIG. 23 is an optical microscope dark field plot of the product obtained in example 5;
FIG. 24 is a scanning electron micrograph of a product obtained in example 6;
FIG. 25 is a light microscopic bright field image of the product obtained in example 6;
FIG. 26 is an optical microscope dark field plot of the product obtained in example 6;
FIG. 27 is a scanning electron micrograph of a product obtained in example 7.
Detailed Description
In order to better understand the present invention, the following examples are further provided to illustrate the present invention, but the present invention is not limited to the following examples.
Example 1:
(1) the method in the literature (adv.Mater.2014,26, 1058-1064) is adopted to prepare the superparamagnetic ferroferric oxide colloidal nanoparticles, and the specific steps are as follows:
adding 0.13 mmol of polyvinylpyrrolidone (PVP) and 0.06 mmol of tannic acid into a beaker containing 30 ml of ethylene glycol, heating and stirring at 80 ℃ for 15 minutes until the PVP is completely dissolved, cooling the solution to room temperature, adding 2.6 mmol of ferric chloride hexahydrate, stirring for 30 minutes, adding 34 mmol of anhydrous sodium acetate, stirring for 40 minutes, transferring the obtained solution to a 50 ml of polytetrafluoroethylene reaction kettle lining, placing the lining into a stainless steel kettle, reacting at 200 ℃ for 10 hours, cooling, performing magnetic separation and washing by using ethanol and water, and finally dispersing the product into 20 ml of anhydrous ethanol for later use.
(2) Preparing a pre-polymerization solution:
taking 0.3 ml of ethanol solution of the ferroferric oxide colloidal nanoparticles in the solution (1), carrying out centrifugal separation, removing supernatant, adding 1 ml of ethylene glycol, carrying out ultrasonic treatment to uniformly disperse the particles, respectively weighing 0.3 g of N-isopropylacrylamide, 0.0204 g of methylene bisacrylamide (the mass ratio of the methylene bisacrylamide to the N-isopropylacrylamide is 0.05) and 0.05 g of 2-hydroxy-2-methyl propiophenone, adding the mixture into the solution, and carrying out ultrasonic mixing to uniformly form a pre-polymerization solution.
(3)Fe3O4Preparing a @ PVP @ PNIPAM magnetic photonic crystal nano chain:
putting 200 microliters of the pre-polymerized solution into a 5 milliliter small beaker, adding 2 milliliters of polyacrylic acid aqueous solution with the concentration of 0.54 grams per liter (g/L), uniformly mixing by ultrasonic waves, placing the small beaker right above a magnet, adjusting the magnetic field intensity to 725 gauss, after inducing for 30 seconds, opening an ultraviolet lamp, polymerizing for 120 seconds under the conditions of ultraviolet irradiation and magnetic field induction, after the reaction is finished, centrifugally separating, washing for 3 times by using ethanol, and finally dispersing the product into water.
Scanning electron micrographs, bright field micrographs, infrared spectrograms, thermogravimetric graphs, magnetic hysteresis curves, spectrograms under different temperatures and magnetic fields and microscopic dark field graphs of the obtained product are shown in figures 1-9, the scanning electron micrographs and the bright field micrographs show that the product is a one-dimensional nanochain with good dispersibility, the average chain length is 15.5 microns, the infrared spectrograms can deduce that the product contains poly-nitrogen isopropyl acrylamide, ferroferric oxide and hydrogen bonds, the thermogravimetric analysis graph calculates that the content of organic matters in the product is 34.37%, the magnetic hysteresis loop shows that the saturation magnetization of the product is 33.09emu/g, the spectrograms show that the diffraction peak positions of the obtained nanochain at 4 degrees, 32 degrees and 38 degrees are 592 nanometers, 536 nanometers and 488 nanometers respectively, and the diffraction peak intensity is increased along with the increase of the magnetic field intensity. From a microscope dark field image, the obtained nano-chains are golden yellow, green and blue at 4 degrees, 32 degrees and 38 degrees respectively, and the color brightness is increased along with the increase of the intensity of the external magnetic field.
Example 2:
the procedure of example 1 was followed except that 0.0041 g of methylenebisacrylamide (i.e., the amount of methylenebisacrylamide to N-isopropylacrylamide species ratio) was present in the prepolymerization solution, and the final product was dispersed in ethanol. The scanning electron micrograph, bright field micrograph, spectrogram and dark field micrograph of the obtained product are shown in FIGS. 10-13. The scanning electron microscope and the bright field microscope picture show that the obtained product is a nano chain with good dispersibility, the spectrogram shows that the diffraction peak position of the obtained nano chain is 647 nanometers, and the diffraction peak intensity is increased along with the increase of the magnetic field intensity. The chain spacing of the resulting nanochain was 88 nm as calculated from the bragg equation. The resulting photonic crystal chain was red as seen from the microscope.
Example 3:
the procedure of example 1 was followed, except that 0.041 g of methylenebisacrylamide (i.e., the ratio of the amounts of methylenebisacrylamide to the amount of N-isopropylacrylamide material was 0.1) was present in the prepolymerization solution, and the final product was dispersed in ethanol. The obtained product has a spectrogram, a scanning electron micrograph, a bright field micrograph and a dark field micrograph shown in FIGS. 12 and 14 to 16. The obtained product is a nano chain with good dispersibility according to a topographic map, the diffraction peak position of the obtained nano chain is 560 nanometers according to a spectrogram, and the diffraction peak intensity is increased along with the increase of the magnetic field intensity. The chain spacing of the resulting nanochain was calculated to be 56 nanometers according to the bragg equation. The resulting photonic crystal chains are green as seen by dark field microscopy.
Example 4:
the procedure of example 1 was followed except that the amount of methylene bisacrylamide in the prepolymerization solution was 0.0082 g (i.e., the ratio of the amount of methylene bisacrylamide to the amount of N-isopropylacrylamide was 0.02), and the final product was dispersed in ethanol. The topography, spectra and micrographs of the resulting product are shown in FIGS. 17-20. The obtained product is a nano chain with good dispersibility according to a topographic map, the diffraction peak position of the obtained nano chain is 607 nm according to a spectrogram, and the diffraction peak intensity is increased along with the increase of the magnetic field intensity. The chain spacing of the resulting nanochain was calculated to be 73 nm according to the bragg equation. The dark field microscopic picture shows that the obtained photonic crystal chain is yellow green.
Example 5:
the procedure is as in example 4, but the polyacrylic acid concentration used is 0.33 g per liter. The obtained product has a spectrogram, a scanning electron micrograph, a bright field micrograph and a dark field micrograph shown in FIGS. 19, 21-23. The scanning electron microscope image and the bright field microscope image show that the obtained product is a nano chain with good dispersibility, the spectrogram shows that the diffraction peak position of the obtained nano chain is 656 nm, and the diffraction peak intensity is increased along with the increase of the magnetic field intensity. The chain spacing of the resulting nanochain was calculated to be 91 nm according to the bragg equation. The dark field microscopic image shows that the obtained photonic crystal chain is red.
Example 6:
the procedure of example 4 was followed, but the polyacrylic acid concentration used was 1.09g per liter. The obtained product has a spectrogram, a scanning electron micrograph, a bright field micrograph and a dark field micrograph shown in FIGS. 19 and 24-26. The obtained product is a nano chain with good dispersibility and small chain distance as can be seen from the topographic map, the diffraction peak position of the obtained nano chain is 527 nm as can be seen from the spectrogram, and the diffraction peak intensity is increased along with the increase of the magnetic field intensity. The chain spacing of the resulting nanochain was calculated to be 44 nm according to the bragg equation. The dark field microscopic image shows that the obtained photonic crystal chain is blue-green.
Example 7:
the procedure of example 1 was followed, except that 0.0123 g of methylenebisacrylamide (i.e., the amount of methylenebisacrylamide to N-isopropylacrylamide was 0.03) was used in the prepolymerization solution, and the concentration of polyacrylic acid used was 0.73 g per liter. The scanning electron micrograph of the resulting product is shown in FIG. 27. The obtained product is the nano-chain with good dispersity, and the spacing between the nano-chain is small.
Claims (1)
1. Preparation of Fe3O4The method for preparing the @ PVP @ PNIPAM magnetic photonic crystal nano-chain particles comprises the following steps:
(1) the method in the literature (adv. mater.2014,26, 1058-:
adding 0.13 mmol of polyvinylpyrrolidone and 0.06 mmol of tannic acid into a beaker containing 30 ml of ethylene glycol, heating and stirring at 80 ℃ for 15 minutes until PVP is completely dissolved, cooling the solution to room temperature, adding 2.6 mmol of ferric chloride hexahydrate, stirring for 30 minutes, adding 34 mmol of anhydrous sodium acetate, stirring for 40 minutes, transferring the obtained solution to a lining of a 50 ml of polytetrafluoroethylene reaction kettle, placing the lining into a stainless steel kettle, reacting at 200 ℃ for 10 hours, cooling, performing magnetic separation and washing by using ethanol and water, and finally dispersing the product into 20 ml of anhydrous ethanol for later use;
(2) preparing a pre-polymerization solution:
taking 0.3 ml of ethanol solution of ferroferric oxide colloid nano particles in the step (1), carrying out centrifugal separation, removing supernatant, adding 1 ml of ethylene glycol into the ethanol solution, carrying out ultrasonic treatment to uniformly disperse the particles, respectively weighing 0.3 g of N-isopropylacrylamide and 0.0204 g of methylene bisacrylamide, wherein the mass ratio of the methylene bisacrylamide to the N-isopropylacrylamide is 0.05 and 0.05 g of 2-hydroxy-2-methyl propiophenone, adding the mixture into the solution, and carrying out ultrasonic mixing uniformly to form a pre-polymerization solution;
(3) preparing a Fe3O4@ PVP @ PNIPAM magnetic photonic crystal nano-chain:
putting 200 microliters of the pre-polymerized solution into a 5 milliliter small beaker, adding 2 milliliters of polyacrylic acid aqueous solution with the concentration of 0.54 grams per liter (g/L), uniformly mixing by ultrasonic waves, placing the small beaker right above a magnet, adjusting the magnetic field intensity to 725 gauss, after inducing for 30 seconds, opening an ultraviolet lamp, polymerizing for 120 seconds under the conditions of ultraviolet irradiation and magnetic field induction, after the reaction is finished, centrifugally separating, washing for 3 times by using ethanol, and finally dispersing the product into water.
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