CN108387963B - Porous layered structure chromogenic material and preparation method thereof - Google Patents
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Abstract
The invention relates to a porous layered structure chromogenic material and a preparation method thereof, belonging to the field of new materials, in particular to the field of chromogenic new materials. A porous layered structure chromogenic material is formed by a material with high thermal stability and a material with low thermal stability through a layer-by-layer self-assembly mode to form an alternate stacked layered structure, and then sintering at 200-800 ℃ to obtain the porous layered structure chromogenic material, wherein the material with high thermal stability is an inorganic oxide, clay, zeolite or laponite with a melting point higher than 800 ℃; the material with low thermal stability is a high-molecular polymer with the glass transition temperature of below 200 ℃, or a mixture of the polymer and the material with high thermal stability, and the mass ratio of the polymer to the material with high thermal stability is 1: 9-9: 1. The porous layered structure chromogenic material has the characteristic of rich material selection of the high-refractive-index material layer, can construct multiple colors by using materials prepared under one condition, and has bright color and simple and convenient preparation method.
Description
Technical Field
The invention relates to a porous layered structure chromogenic material and a preparation method thereof, belonging to the field of new materials, in particular to the field of chromogenic new materials.
Background
The multilayer film type chromogenic material is a bionic chromogenic material, namely a periodic structure material formed by alternately stacking high-refractive index materials and low-refractive index materials, and has wide application prospect in the fields of naked eye identification sensing, anti-counterfeiting, photovoltaic materials, display and the like. Inorganic materials with the refractive index of more than 2, such as titanium oxide, zirconium oxide and the like, are mostly adopted as high-refractive-index materials, and the types of selectable materials are few; the low refractive index is inorganic material or high molecular polymer material, such as silicon dioxide, and the refractive index of the material is about 1.4 mostly. Only if the two types of materials form a high-low refractive index difference, structural color can be generated, and the larger the refractive index difference is, the more beautiful the structural color is easily generated. The refractive index of air is about 1, so if air is introduced into the material to form a pore structure, the refractive index of the material is reduced, and the larger the porosity is, the more the refractive index is reduced.
Disclosure of Invention
The invention aims to provide a porous layered structure chromogenic material. According to the invention, air is introduced into the material layer with low thermal stability by a method of material thermal decomposition or thermal deformation to form pores, so that the refractive index of the material layer is greatly reduced, and the difference of the refractive indexes of the two base materials is increased, thereby obtaining the porous material with bright structural color characteristics. By the method, the optional categories of the high-refractive-index layer materials can be effectively expanded, and the structural color materials with good application performance can be obtained.
A porous layered structure chromogenic material is prepared by forming an alternate stacked layered structure by a material with high thermal stability and a material with low thermal stability in a layer-by-layer self-assembly mode, sintering at 200-800 ℃,
wherein the material with high thermal stability is inorganic oxide, clay, zeolite or laponite with the melting point higher than 800 ℃; the material with low thermal stability is a high-molecular polymer with the glass transition temperature of below 200 ℃, or a mixture of the polymer and the material with high thermal stability, and the mass ratio of the polymer to the material with high thermal stability is 1: 9-9: 1.
The porous multilayer material is formed by alternately stacking material layers with high thermal stability and low thermal stability from bottom to top on a substrate along the direction vertical to the plane of the substrate.
The thickness of each layer of the material layer with high thermal stability is 50-400 nm, and further the thickness of the layer is preferably 70-200 nm. .
The thickness of each layer of the material layer with low thermal stability is 50-400 nm, and further the thickness of the layer is preferably 80-300 nm.
The inorganic oxide with the melting point higher than 800 ℃ is one of silicon oxide, titanium oxide, zirconium oxide, zinc oxide, magnesium oxide, aluminum oxide or tin oxide.
Preferably, the material with high thermal stability is silicon oxide, clay, titanium oxide, tin oxide, zirconium oxide.
The material with low thermal stability is selected from high molecular polymers with the glass transition temperature below 200 ℃, and comprises polystyrene, polyacrylate, polyacrylonitrile, polyvinyl alcohol, polycarbonate, polyacrylic acid and polymethyl methacrylate. Further, it is preferable that the material having low thermal stability is polystyrene, polymethyl methacrylate, polyacrylic acid, or polyvinyl alcohol.
Or the material with low thermal stability is a mixture consisting of the high-molecular polymer and the material with high thermal stability, and the mass ratio of the high-molecular polymer to the material with high thermal stability is 1: 9-9: 1.
Further, the mass ratio of the high-molecular polymer to the thermally stable material is preferably 1:1 to 2:1
Further, it is preferable that the material having low thermal stability is a mixture of silicon oxide and polystyrene. Further, it is preferable that the mass ratio of the silicon oxide to the polystyrene is 1:1 or 2: 1.
The porous layer-structured chromogenic material is self-assembled on a substrate layer by layer. Further, the substrate is preferably quartz, silicon, glass, iron, steel, copper substrate.
Another object of the present invention is to provide a method for preparing the above material.
A preparation method of a porous layered structure chromogenic material comprises the following process steps:
preparing material dispersion liquid or sol with high thermal stability;
preparing dispersion, sol or solution of the material with low thermal stability;
thirdly, the materials obtained in the first step and the materials obtained in the second step are assembled on the substrate alternately by adopting a layer-by-layer self-assembly method, and drying and curing treatment are carried out after each layer of materials is assembled;
and fourthly, placing the multilayer structure formed by alternately assembling the two materials obtained in the third step into a sintering furnace, heating, and treating for 1-120 min at 200-800 ℃ to obtain the porous layered structure chromogenic material.
The layer-by-layer self-assembly preparation method is a spin coating method, a dipping method or a spraying method.
In the above technical scheme, in the second step, when the material with low thermal stability is formed by mixing two materials, a dispersion, a sol or a solution of a mixture of the two materials is prepared first.
Further, the thickness of the material layer with high thermal stability is 50-400 nm; and the thickness of the material layer with low thermal stability is 50-400 nm.
In the above technical solution, in the step (i), the mass percentage concentration of the material dispersion or sol with high thermal stability is 1% to 40%, and more preferably 2% to 15%.
In the above technical solution, in the step (i), the preparation method of the material dispersion or sol with high thermal stability is a liquid phase chemical synthesis method and a vapor deposition method.
In the above technical scheme, in the second step, the mass percentage concentration of the dispersion, sol or solution of the material with low thermal stability is 1-70%, and more preferably 3-50%.
In the above technical solution, in the second step, the preparation method of the dispersion, sol or solution of the material with low thermal stability is a liquid phase chemical synthesis method or a vapor deposition method.
In the technical scheme, in the third step, after the preparation of each layer of material in the construction method is finished, the sample is dried for 1-30 minutes at 30-100 ℃; further preferably, the drying is carried out at 40 to 70 ℃ for 1 to 25 minutes.
In the technical scheme, in the fourth step, the multilayer structure in the method is heated, the treatment temperature is 200-800 ℃, and the treatment time is 1-120 minutes; further preferably 200 to 500 ℃ for 5 to 60 minutes.
The invention has the beneficial effects that: the porous layered structure chromogenic material has the characteristic of rich material selection of the high-refractive-index material layer, can construct multiple colors by using materials prepared under one condition, and has bright color and simple and convenient preparation method. The porous layered structure color material constructed by the method has wide application prospects in the aspects of sensing, anti-counterfeiting, displaying and the like.
Drawings
FIG. 1 is a digital photograph of a purple-structured color-producing film obtained in example 13;
FIG. 2 is a cross-sectional scanning electron micrograph of the color-developing film of example 13.
Detailed Description
The following non-limiting examples are presented to enable those of ordinary skill in the art to more fully understand the present invention and are not intended to limit the invention in any way.
The test methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
Example 1
10.0g of ethanol, 0.1g of 2mol/L HCl and 0.9g of deionized water are mixed uniformly in a reaction bottle, then 2.08g of ethyl orthosilicate is added, and the obtained mixed solution is stirred for 3 hours at room temperature to obtain silica sol.
Adding 20.0g of styrene into a three-neck flask, heating to 80 ℃ for prepolymerization, raising the temperature to 110 ℃ for reaction for 3 hours, then raising the temperature to 140 ℃ for further polymerization for 1 hour, and then cooling the reaction liquid to room temperature to obtain the polystyrene.
Taking 3% mass fraction of silica sol and 5% mass fraction of polystyrene toluene solution to spin on a silicon wafer alternately at the rotating speed of 3000rpm, drying the sample at 70 ℃ for 3min after each layer of material is prepared, and preparing the layered structure chromogenic material.
And heating the prepared color-developing material with the layered structure at 320 ℃ for 10min to obtain the color-developing material with the porous layered structure.
Examples 2 to 6
The procedure of example 1 was followed, except that quartz, glass, iron, steel, copper, etc. were used instead of the silicon wafer as the substrate material to construct the porous layered structure coloring material.
Example 7
Adding 20.0g of styrene into a three-neck flask, heating to 80 ℃ for prepolymerization, raising the temperature to 110 ℃ for reaction for 3 hours, then raising the temperature to 140 ℃ for further polymerization for 1 hour, and then cooling the reaction liquid to room temperature to obtain the polystyrene.
Taking 3% of clay dispersion liquid with the granularity of 50nm and 5% of polystyrene toluene solution in mass percentage, alternately spin-coating on a silicon wafer at the rotating speed of 3000rpm, drying a sample at 70 ℃ for 3min after the preparation of each layer of material is finished, and preparing the layered structure chromogenic material.
And heating the prepared color-developing material with the layered structure at 320 ℃ for 10min to obtain the color-developing material with the porous layered structure.
Examples 8 to 12
The procedure of example 7 was followed, except that quartz, glass, iron, steel, copper, etc. were used instead of the silicon wafer as the substrate material to construct the porous layered structure coloring material.
Example 13
4mL of tetrabutyl titanate and 2mL of isopropanol were mixed uniformly in a 50mL conical flask to obtain a mixed solution. 0.21mL of deionized water, 17 mu L of concentrated hydrochloric acid and 4mL of isopropanol are mixed in a weighing bottle, stirred at room temperature for 10min, the mixed solution is slowly dripped into the mixed solution of tetrabutyl titanate and isopropanol, and stirred at room temperature for 5h after dripping is finished, thus obtaining the titanium oxide sol.
Adding 20.0g of styrene into a three-neck flask, heating to 80 ℃ for prepolymerization, raising the temperature to 110 ℃ for reaction for 3 hours, then raising the temperature to 140 ℃ for further polymerization for 1 hour, and then cooling the reaction liquid to room temperature to obtain the polystyrene.
And (3) taking titanium oxide sol with the mass fraction of 3% and toluene solution of polystyrene with the mass fraction of 5% to spin on a silicon wafer alternately at the rotating speed of 3000rpm, drying the sample for 2min at 70 ℃ after the preparation of each layer of material is finished, and preparing the layered structure chromogenic material.
And heating the prepared color-developing material with the layered structure at 320 ℃ for 10min to obtain the color-developing material with the porous layered structure.
Examples 14 to 18
The procedure of example 13 was repeated except that quartz, glass, iron, steel, copper, or the like was used instead of the silicon wafer as the substrate material to construct a porous layered structure color-developing material.
Example 19
10.0g of ethanol, 0.1g of 2mol/L HCl and 0.9g of deionized water are mixed uniformly in a reaction bottle, then 2.08g of ethyl orthosilicate is added, and the obtained mixed solution is stirred for 3 hours at room temperature to obtain silica sol.
40.0g of water, 10.0g of styrene and 1.0g of dodecyl trimethyl ammonium chloride are placed in a three-neck flask and stirred, heated to 75 ℃, 0.034g of ammonium persulfate is added into a reaction bottle, and after reaction for 1 hour, polystyrene sol is obtained.
Taking silica sol with the mass fraction of 3 percent and mixed sol of polystyrene and silica with the mass fraction of 4 percent (the mass ratio of the polystyrene to the silica is 1:1) to alternately spin-coat on a silicon wafer at the rotating speed of 3000rpm, drying a sample at 70 ℃ for 3min after the preparation of each layer of material is finished, and preparing the layered structure chromogenic material.
And heating the prepared color-developing material with the layered structure at 400 ℃ for 20min to obtain the color-developing material with the porous layered structure.
Examples 20 to 24
The procedure of example 19 was repeated except that quartz, glass, iron, steel, copper, or the like was used instead of the silicon wafer as the substrate material to construct a porous layered structure color-developing material.
Example 25
40.0g of water, 10.0g of styrene and 1.0g of dodecyl trimethyl ammonium chloride are placed in a three-neck flask and stirred, heated to 75 ℃, 0.034g of ammonium persulfate is added into a reaction bottle, and after reaction for 1 hour, polystyrene sol is obtained.
Taking 3% of clay dispersion liquid with the granularity of 50nm and 4% of polystyrene and clay mixed sol (the mass ratio of the polystyrene to the clay is 1:1) in mass percentage, alternately spin-coating on a silicon wafer at the rotating speed of 3000rpm, drying a sample at 70 ℃ for 3min after the preparation of each layer of material is finished, and preparing the layered structure chromogenic material.
And heating the prepared color-developing material with the layered structure at 400 ℃ for 20min to obtain the color-developing material with the porous layered structure.
Examples 26 to 30
The procedure of example 25 was repeated except that quartz, glass, iron, steel, and copper were used instead of the silicon wafer as the substrate material to construct a porous layered structure coloring material.
Example 31
4mL of tetrabutyl titanate and 2mL of isopropanol were mixed uniformly in a 50mL conical flask to obtain a mixed solution. 0.21mL of deionized water, 17 mu L of concentrated hydrochloric acid and 4mL of isopropanol are mixed in a weighing bottle, stirred at room temperature for 10min, the mixed solution is slowly dripped into the mixed solution of tetrabutyl titanate and isopropanol, and stirred at room temperature for 5h after dripping is finished, thus obtaining the titanium oxide sol.
40.0g of water, 10.0g of styrene and 1.0g of dodecyl trimethyl ammonium chloride are placed in a three-neck flask and stirred, heated to 75 ℃, 0.034g of ammonium persulfate is added into a reaction bottle, and after reaction for 1 hour, polystyrene sol is obtained.
Taking titanium oxide with the mass fraction of 3 percent and polystyrene and silicon oxide mixed sol with the mass fraction of 4 percent (the mass ratio of the polystyrene to the silicon oxide is 1:1) to alternately spin-coat on a silicon wafer at the rotating speed of 3000rpm, drying a sample at 70 ℃ for 3min after the preparation of each layer of material is finished, and preparing the layered structure chromogenic material.
And heating the prepared color-developing material with the layered structure at 400 ℃ for 20min to obtain the color-developing material with the porous layered structure.
Examples 32 to 36
The procedure of example 31 was repeated except that quartz, glass, iron, steel, and copper were used instead of the silicon wafer as the substrate material to construct a porous layered structure coloring material.
Example 37
4mL of tetrabutyl titanate and 2mL of isopropanol were mixed uniformly in a 50mL conical flask to obtain a mixed solution. 0.21mL of deionized water, 17 mu L of concentrated hydrochloric acid and 4mL of isopropanol are mixed in a weighing bottle, stirred at room temperature for 10min, the mixed solution is slowly dripped into the mixed solution of tetrabutyl titanate and isopropanol, and stirred at room temperature for 5h after dripping is finished, thus obtaining the titanium oxide sol.
40.0g of water, 10.0g of styrene and 1.0g of dodecyl trimethyl ammonium chloride are placed in a three-neck flask and stirred, heated to 75 ℃, 0.034g of ammonium persulfate is added into a reaction bottle, and after reaction for 1 hour, polystyrene sol is obtained.
Taking titanium oxide with the mass fraction of 3 percent and mixed sol of polystyrene and clay with the mass fraction of 4 percent (the mass ratio of the polystyrene to the clay is 1:1) to alternately spin-coat on a silicon wafer at the rotating speed of 3000rpm, drying a sample at 70 ℃ for 3min after the preparation of each layer of material is finished, and preparing the layered structure chromogenic material.
And heating the prepared color-developing material with the layered structure at 400 ℃ for 20min to obtain the color-developing material with the porous layered structure.
Examples 38 to 42
The procedure of example 37 was repeated except that quartz, glass, iron, steel, and copper were used instead of the silicon wafer as the substrate material to construct a porous layered structure coloring material.
Example 43
4mL of tetrabutyl titanate and 2mL of isopropanol were mixed uniformly in a 50mL conical flask to obtain a mixed solution. 0.21mL of deionized water, 17 mu L of concentrated hydrochloric acid and 4mL of isopropanol are mixed in a weighing bottle, stirred at room temperature for 10min, the mixed solution is slowly dripped into the mixed solution of tetrabutyl titanate and isopropanol, and stirred at room temperature for 5h after dripping is finished, thus obtaining the titanium oxide sol.
40.0g of water, 10.0g of styrene and 1.0g of dodecyl trimethyl ammonium chloride are placed in a three-neck flask and stirred, heated to 75 ℃, 0.034g of ammonium persulfate is added into a reaction bottle, and after reaction for 1 hour, polystyrene sol is obtained.
Taking titanium oxide with the mass fraction of 3 percent and polystyrene and titanium oxide mixed sol with the mass fraction of 4 percent (the mass ratio of the polystyrene to the titanium oxide is 1:1) to alternately spin-coat on a silicon wafer at the rotating speed of 3000rpm, drying a sample at 70 ℃ for 3min after the preparation of each layer of material is finished, and preparing the layered structure chromogenic material.
And heating the prepared color-developing material with the layered structure at 400 ℃ for 20min to obtain the color-developing material with the porous layered structure.
Examples 44 to 48
The procedure of example 43 was repeated except that quartz, glass, iron, steel, and copper were used instead of the silicon wafer as the substrate material to construct a porous layered structure coloring material.
Example 49
10.0g of ethanol, 0.1g of 2mol/L HCl and 0.9g of deionized water are mixed uniformly in a reaction bottle, then 2.08g of ethyl orthosilicate is added, and the obtained mixed solution is stirred for 3 hours at room temperature to obtain silica sol.
Taking 3% of silica sol and 8% of polyvinyl alcohol 17-92 aqueous solution by mass fraction, alternately spin-coating on a silicon wafer at the rotating speed of 3000rpm, drying a sample at 70 ℃ for 3min after the preparation of each layer of material is finished, and preparing the layered structure chromogenic material.
And heating the prepared color-developing material with the layered structure at 350 ℃ for 10min to obtain the color-developing material with the porous layered structure.
Examples 50 to 54
The procedure of example 43 was repeated except that quartz, glass, iron, steel, and copper were used instead of the silicon wafer as the substrate material to construct a porous layered structure coloring material.
Claims (7)
1. A porous layered structure chromogenic material characterized in that: the color-generating material is prepared by forming an alternate stacked layered structure by a material with high thermal stability and a material with low thermal stability in a layer-by-layer self-assembly mode and sintering at 200-800 ℃,
wherein the material with high thermal stability is inorganic oxide, clay, zeolite or laponite with the melting point higher than 800 ℃;
the material with low thermal stability is a high molecular polymer with the glass transition temperature below 200 ℃.
2. The material of claim 1, wherein: the inorganic oxide with the melting point higher than 800 ℃ is silicon oxide, titanium oxide, zirconium oxide, zinc oxide, magnesium oxide, aluminum oxide or tin oxide.
3. The material of claim 1, wherein: the high molecular polymer is polystyrene, polyacrylate, polyacrylonitrile, polyvinyl alcohol, polycarbonate, polyacrylic acid or polymethyl methacrylate.
4. A preparation method of a porous layered structure chromogenic material is characterized by comprising the following steps: the method comprises the following process steps:
preparing material dispersion liquid or sol with high thermal stability;
preparing dispersion, sol or solution of the material with low thermal stability;
thirdly, the materials obtained in the first step and the materials obtained in the second step are assembled on the substrate alternately by adopting a layer-by-layer self-assembly method, and drying and curing treatment are carried out after each layer of materials is assembled;
and fourthly, placing the multilayer structure formed by alternately assembling the two materials obtained in the third step into a sintering furnace, heating, and treating for 1-120 min at 200-800 ℃ to obtain the porous layered structure chromogenic material.
5. The method for preparing a porous layered structure color-producing material according to claim 4, characterized in that: and the thickness of the material layer with high thermal stability is 50-400 nm.
6. The method for preparing a porous layered structure color-producing material according to claim 4, characterized in that: and the thickness of the material layer with low thermal stability is 50-400 nm.
7. The method for preparing a porous layered structure color-producing material according to claim 4, characterized in that: and thirdly, drying and curing each layer of the material in an oven at the temperature of 30-100 ℃ for 1-30 min after the material is assembled.
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