CN112625388A - Cu with bright structural color2O single crystal nano particle-polymer composite film and preparation method thereof - Google Patents
Cu with bright structural color2O single crystal nano particle-polymer composite film and preparation method thereof Download PDFInfo
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Abstract
The invention discloses Cu with bright structural color2An O single crystal nano particle-polymer composite film and a preparation method thereof belong to the field of new material preparation. The Cu2The process of coloring the polymer film with O single crystal nanoparticles can be roughly divided into three steps, first, Cu with uniform size is sprayed on the glass substrate2Preparation of Cu with structural color from O single crystal nano particles2O film, and then coating the polymer solution on Cu with glass substrate uniformly by using a coater2O film surface, peeling it from glass substrate after polymer solution is dried, single crystal Cu2The O nano particles are locked in the polymer film to obtain the Cu with bright color and certain transparency2O single crystal nano particle-polymer composite structure color film. The composite film has excellent mechanical performance, friction resistance and sun-proof performance. Green, environment-friendly and recyclable Cu2The O monocrystal nanoparticle-polymer composite film can realize large-area preparation, and is expected to be applied to the fields of packaging, display, decoration and the like.
Description
Technical Field
The invention relates to the field of structural color materials, in particular to Cu with bright structural color2An O single crystal nano particle-polymer composite film and a preparation method thereof belong to the field of new material research.
Background
Polymer films play a very important role in human production and life and cover many fields such as films for packaging, films for building materials or leather or some high-performance films with excellent mechanical and optical properties for industrial applications, stimuli-responsive polymer films for sensing applications, etc., and thus it is important to combine these polymer films with color aesthetics.
For example, coloring polymer films with dyes and pigments is disadvantageous for applications in packaging and the like. The physical color generated by the interaction of light and the micro-nano structure, namely the structural color, has the characteristics of no toxicity, environmental protection, excellent weather resistance and the like, and is considered as a powerful substitute for dyes and pigments. For example, the coloring of polymer films with structural colors is expected to achieve pollution-free green printing. However, the polymer film is colored by the structural color film taking the low-refractive-index microspheres as the construction units, and the coating is too thick and is easy to fall off (Scientific Reports,2015,5, 8340; Nanoscale,2018,10, 14755-; e.g. using Cu having a higher refractive index2The O film has better coloring effect on the polymer film.
Disclosure of Invention
The invention aims to provide a brand new Cu2Method for coloring polymer film with O single crystal nano particles, and method for directly coating polymer solution on Cu2On the O film, after the solution is dried, the polymer film directly combines Cu with the O film2O single crystal nano particles are coated in a polymer film to obtainTo Cu having a brilliant structural color2The O single crystal nano particle-polymer composite film has excellent mechanical performance, friction resistance and weather resistance. Fundamentally has solved the fastness problem of using structural color to give the polymer film colour. The method has simple and safe process and can simultaneously monodisperse Cu2The O single crystal nano particles are combined with polymer materials commonly used in production and life, and the method has strong practicability.
The invention relates to Cu with bright structural color2O single crystal nano particle-polymer composite film and preparation method thereof, wherein a single-layer disordered Cu is coated inside the polymer film2And (4) O single crystal. Cu2At least 2-3O single crystals are aggregated and randomly dispersed.
In order to solve the fastness problem that the structural color gives the polymer film color, the invention adopts a technical scheme that: monodisperse Cu2Spraying O single crystal nano particles on a substrate to obtain Cu2O film, coating polymer solution to Cu2On the O film, drying the film, and adding Cu to the polymer film2O single crystal nano particles are coated in the film to obtain Cu with bright structural color2O single crystal nano particle-polymer composite film. The realization process comprises the following process steps:
preparing monodisperse Cu2O single crystal nano particles and preparing the O single crystal nano particles into a dispersion liquid with a certain concentration.
② mixing Cu2Spraying the dispersion liquid of O single crystal nano particles on a substrate at a certain coverage density to prepare Cu2And (3) an O film.
Thirdly, preparing the polymer into solution and coating the solution on Cu with a certain thickness2Drying the O film for a certain time at a certain temperature, and removing the O film from the substrate to obtain Cu with bright structural color2O single crystal nano particle-polymer composite film.
Further, in the above-mentioned embodiment, the monodisperse Cu described in step (i)2The O single crystal nano particle is Cu2O single crystal ball, Cu2O single crystal 14-face body, Cu226-face body of O single crystal and Cu2One of 6-sided bodies of O single crystal "round corner".
Further, in the above technical means, the particle diameter of the monodisperse nanoparticle in the step (i) is 90nm to 500 nm.
Further, in the above-mentioned embodiment, the monodisperse Cu described in the step (r)2The concentration of the O monocrystal nanoparticle dispersion liquid is 0.1 wt% -20 wt%.
Further, in the above technical scheme, the solvent of the dispersion liquid in the step (i) is one or more of methanol, ethanol, dimethyl sulfoxide, acetone, butanol, ethylene glycol, water, n-hexane and cyclohexane.
Furthermore, in the above technical solution, the Cu described in step II2The coverage density of the O single crystal nano particles is 7.6mg/cm2～25.3mg/cm2。
Further, in the above technical solution, the substrate in the second step is one of glass, a steel plate, an aluminum plate, an iron plate, and a silicon plate.
Further, in the above technical solution, the polymer in step (c) is one of polyvinyl alcohol (PVA for short, average molecular weight is 10000-200000), starch (average molecular weight is 1000-14000), carboxymethyl cellulose (average molecular weight is 6400-17000), polyester film (PET for short), and cellulose (50000-2500000).
Further, in the above technical solution, the coating thickness of the polymer solution in the third step is 1 μm to 1 cm.
Further, in the above technical scheme, the concentration of the polymer solution in the third step is 1 wt% -60 wt%.
Further, in the above technical scheme, the drying temperature in the third step is 20-80 ℃.
Furthermore, in the above technical scheme, the drying time in the third step is 0.5 to 72 hours.
Advantageous effects of the invention
Cu for use in the invention2Cu prepared from O single crystal nano particles2O film, coating polymer solution to Cu2On an O film, drying to obtain the product with beautiful appearanceStructural colored Cu2An O single crystal nano particle-polymer composite film and a preparation method thereof. Fundamentally has solved the fastness problem of using structural color to give the polymer film colour, and the method is simple and safe, green, and the practicality is strong moreover.
Drawings
The invention is further illustrated with reference to the following figures and examples.
FIG. 1 shows monodisperse Cu having a particle size of 270nm in example 12Cu prepared from O monocrystal ball2Scanning electron micrographs of the O film;
FIG. 2 shows monodisperse Cu having a particle size of 270nm in example 12Cu prepared from O monocrystal ball2A scanning electron microscope for a digital photo and a reflection spectrogram of the O single crystal sphere/PVA composite film and a plane and a section of the composite structure color film;
FIG. 3 shows Cu in example 12Rubbing the digital photos and the corresponding reflection spectrums of the O single crystal ball/PVA composite film for 100 times by using a rubbing instrument; the results show that the intensity of the reflection spectrum after 100 times of rubbing is reduced by only about 4% compared with the intensity of the reflection spectrum before rubbing, indicating that the prepared Cu2The O single crystal ball/PVA composite film has good friction resistance.
FIG. 4 shows Cu in example 12The reflection spectrum of the O single crystal ball/PVA composite structure color film after being respectively bent for 300 times and 600 times and the stretch-proof graph of the composite structure color film; the bending results show that Cu2After the O/PVA composite film is bent for 600 times, the reflection spectrum and Cu before bending2The intensity ratio of the reflection spectrum of the O single crystal ball/PVA composite film is basically unchanged, and the prepared Cu is proved2The film with the O single crystal ball/PVA composite structural color has good flexibility and good bending stability. The stretching results showed that the tensile strength at break of the PVA film was about 12.8MPa, and the strain at break was 250%. Due to Cu2Addition of O single crystal ball leads to Cu2The breaking tensile strength of the O single crystal ball/PVA composite film is increased by 7.8MPa compared with that of the PVA film, so that the breaking tensile of the composite film can reach 20.6MPa, the breaking strain is also increased to 300 percent, and the single crystal Cu is proved to be2Addition of O rigid particles imparts Cu2And the O single crystal ball/PVA composite film has better ductility.
FIG. 5 is a Cu with a brilliant structural color2A preparation flow schematic diagram of the O single crystal nano particle-polymer composite film.
Detailed Description
The following description of the preferred embodiments of the present invention with reference to the accompanying drawings makes the present invention better understood by those skilled in the art, and thus clearly defines the scope of the present invention.
Example 1
Cu2Preparation of O single crystal ball/PVA composite film
First, monodisperse Cu is prepared2The preparation method of the O monocrystal microsphere comprises the following steps:
PVP (Mw 55000) and trisodium citrate dihydrate (Na) are weighed according to the molar ratio of 7.7:1:13Cit·2H2O) and copper acetate monohydrate, placing it in a beaker, adding a mixed solution of water and ethylene glycol, and stirring gently. Transferring the mixed solution into a three-necked bottle, adding 0.5M NaOH solution at a dropping rate of 2mL/min to form a dark blue clear solution, stirring vigorously, then adding 0.12M ascorbic acid at a dropping rate of 0.4mL/s, stirring, rapidly adding 0.12M ascorbic acid under stirring, reacting for 1h, centrifuging and washing with a mixed solution of ethanol and water for three times, and drying for later use.
Weighing a certain amount of monodisperse Cu2And adding absolute ethyl alcohol into the O single crystal ball powder to prepare 1 wt% dispersion liquid.
A certain amount of polyvinyl alcohol powder with the molecular weight of 77000 is weighed and added with water to prepare 10 wt% of PVA solution.
Mixing Cu2Ethanol dispersion of O single crystal spheres at 11.5mg/cm2Is sprayed on a glass substrate to obtain Cu2And (3) an O film. The spraying mode is that a simple air pump spraying pen is adopted, and other complex devices and technologies are not needed.
A certain amount of PVA solution was uniformly applied to Cu at a thickness of 1mm by a coater2Drying the O film for 6h at 50 ℃ and then tearing off the O film from the substrate to obtain Cu with bright structural color2O single crystal nano particle-polymer composite filmThe flow is shown in FIG. 5.
Example 2
The difference from example 1 is that Cu is not used2O single crystal spheres, but using monodisperse Cu2The O single crystal is a 6-sided body with round corners.
Cu2Preparing the O single crystal round corner 6-surface body/PVA composite film.
Preparation of monodisperse Cu2The O 'fillet' 6-surface body is prepared by the following specific steps:
based on the method for preparing the monocrystal sphere, the equal proportion of reactants and ligands is kept unchanged, and only EG and H are added2The mass ratio of O was increased to 5:10 to obtain monodisperse Cu2The O single crystal is a 6-sided body with round corners.
Weighing a certain amount of monodisperse Cu2O single crystal 6-surface powder with round corners is added with absolute ethyl alcohol to prepare 2 wt% dispersion liquid.
A certain amount of polyvinyl alcohol powder with the molecular weight of 77000 is weighed and added with water to prepare a solution with the weight percent of 6.
Mixing Cu2The ethanol dispersion of O single crystal 6-sided body with round corners is 7.9mg/cm2Is sprayed on a glass substrate to obtain Cu2And (3) an O film.
A certain amount of PVA solution was uniformly applied to Cu at a thickness of 1mm by a coater2Drying the O-structure color film for 6h at 50 ℃ and then removing the O-structure color film from the substrate to obtain Cu with bright color2O single crystal 6-face PVA composite film with rounded corners.
Example 3
Cu2Preparation of O single crystal ball/cellulose composite membrane
The difference from example 1 is that polyvinyl alcohol is not used
Cu in example 1 was used2Preparation of Cu from O monocrystal ball dispersion2And the O film is prepared into a solution with the mass fraction of 10% by taking cellulose as a polymer component and adding water. Taking a certain amount of cellulose solution, coating the solution on Cu with a thickness of 5mm by using a coating machine2And coating the structural color film of the O-structural color film. Drying at 80 deg.C for 16 hr, and peeling off the substrate to obtain pigmentBrightly colored Cu2O single crystal ball/cellulose composite membrane.
Example 4
Cu2Preparation of O single crystal 26-surface body/PVA composite membrane
First, monodisperse Cu is prepared2The O single crystal 26-surface body is prepared by the following specific method:
polyvinylpyrrolidone (PVP) having a molecular weight of 55000 and copper acetate monohydrate were weighed to a molar ratio of 7.7:1, and dissolved completely with 100mL of water. Then pouring the mixed solution into a three-necked bottle, adding 0.5M NaOH solution at the dropping rate of 2mL/min, then violently stirring, then adding 0.12M ascorbic acid into the solution at the dropping rate of 0.4mL/s, then gently stirring, then adding 0.12M ascorbic acid 8mL into the reaction solution together, and obtaining monodisperse Cu after 1h2And (3) forming an O single crystal 26-surface body, centrifuging the product for 3 times by using a mixed solution of water and ethanol, and drying the product for later use.
A certain amount of polyvinyl alcohol powder with the molecular weight of 77000 is weighed and added with water to prepare a solution with the weight percent of 6.
Mixing Cu2Ethanol dispersion of O single crystal spheres at 16.9mg/cm2Is sprayed on a glass substrate to obtain Cu2And (3) an O film.
A certain amount of PVA solution was uniformly applied to Cu at a thickness of 1mm by a coater2Drying the O film for 6h at 50 ℃ and then removing the O film from the substrate to obtain Cu with bright color2O single crystal 26-face body/PVA composite film.
Examples 5 to 7
The polyethanol used in example 1 can be replaced by starches with molecular weights of 5000,10000 and 14000 respectively to prepare Cu2O single crystal ball/starch composite film.
Examples 8 to 10
Cu was prepared by substituting the polyvinyl alcohol of example 2 with carboxymethyl cellulose having molecular weights of 7000, 13000 and 15000, respectively2O single crystal 'round corner' 6-face body/carboxymethyl cellulose composite membrane.
Examples 11 to 12
Cu in example 32O sheetCu for crystal balls2O single crystal "rounded corner" 6-sided body and Cu226-face substitution of O single crystal can respectively obtain Cu2O single crystal 'round corner' 6-face body/cellulose composite film and Cu2O single crystal 26-face body/cellulose composite film.
Claims (8)
1. Cu with bright structural color2The O single crystal nano particle-polymer composite film is characterized in that:
the polymer film is internally wrapped with single-layer disordered Cu2And (4) O single crystal.
The polymer is one of polyvinyl alcohol with the average molecular weight of 10000-200000, starch with the average molecular weight of 1000-14000, carboxymethyl cellulose with the average molecular weight of 6400-17000, a polyester film with the average molecular weight of 10000-100000 and cellulose with the average molecular weight of 50000-2500000; cu2The O single crystal nano particle comprises one of a single crystal sphere, a single crystal 14-surface body, a single crystal 26-surface body and a single crystal 6-surface body with a round angle, and the particle size of the monodisperse nano particle is 90-500 nm.
2. Cu as claimed in claim 12The preparation method of the O single crystal nano particle-polymer composite film comprises the following process steps:
preparing monodisperse Cu2O single crystal nano particles are prepared into dispersion liquid with a certain concentration;
② preparing Cu from the first step2Spraying O monocrystal nano particles on a substrate at a certain coverage density to obtain Cu2An O film;
preparing polymer solution with certain concentration, and coating the polymer solution on the Cu obtained in the step (c) by a coating machine with certain thickness2Drying the O film for a period of time at a certain temperature, and removing the O film from the substrate to obtain Cu with bright structural color2O single crystal nano particle-polymer composite film.
3. The method according to claim 2, wherein the solvent in the dispersion is one or more selected from methanol, ethanol, dimethyl sulfoxide, acetone, butanol, ethylene glycol, water, n-hexane and cyclohexane.
4. The method according to claim 2, wherein the Cu is2The coverage density of the O single crystal nano particles is 7.6mg/cm2～25.3mg/cm2。
5. The method of claim 2, wherein the monodisperse Cu is2The concentration of the O monocrystal nanoparticle dispersion liquid is 0.1 wt% -20 wt%.
6. The method according to claim 2, wherein the drying temperature is 20 ℃ to 80 ℃.
7. The method according to claim 2, wherein the drying time is 0.5 to 72 hours.
8. The method according to claim 2, wherein the substrate is one of glass, steel plate, aluminum plate, iron plate, and silicon plate; the concentration of the polymer solution is 1 to 60 weight percent; the coating thickness of the polymer solution is 1 mu m-1 cm.
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| ZHIPENG MENG: "Bio-inspired transparent structural color film and its application in biomimetic camouflage", 《NANOSCALE》 * |
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