CN111688189B - Method for preparing structural color three-dimensional array pattern based on sessile liquid drops - Google Patents

Method for preparing structural color three-dimensional array pattern based on sessile liquid drops Download PDF

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CN111688189B
CN111688189B CN202010558310.0A CN202010558310A CN111688189B CN 111688189 B CN111688189 B CN 111688189B CN 202010558310 A CN202010558310 A CN 202010558310A CN 111688189 B CN111688189 B CN 111688189B
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colloidal particles
structural color
dimensional array
array pattern
preparing
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CN111688189A (en
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余子夷
钦义鹏
张静
姜超
汤保
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Nanjing Yuyuan New Energy Carbon Neutralization Technology Co ltd
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Nanjing Tech University
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    • B29C64/00—Additive manufacturing, i.e. manufacturing of three-dimensional [3D] objects by additive deposition, additive agglomeration or additive layering, e.g. by 3D printing, stereolithography or selective laser sintering
    • B29C64/10—Processes of additive manufacturing
    • B29C64/106—Processes of additive manufacturing using only liquids or viscous materials, e.g. depositing a continuous bead of viscous material
    • B29C64/124—Processes of additive manufacturing using only liquids or viscous materials, e.g. depositing a continuous bead of viscous material using layers of liquid which are selectively solidified
    • B29C64/129—Processes of additive manufacturing using only liquids or viscous materials, e.g. depositing a continuous bead of viscous material using layers of liquid which are selectively solidified characterised by the energy source therefor, e.g. by global irradiation combined with a mask
    • B29C64/135—Processes of additive manufacturing using only liquids or viscous materials, e.g. depositing a continuous bead of viscous material using layers of liquid which are selectively solidified characterised by the energy source therefor, e.g. by global irradiation combined with a mask the energy source being concentrated, e.g. scanning lasers or focused light sources
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Abstract

The invention discloses a method for preparing a three-dimensional array pattern of structural colors based on sessile droplets, which mainly combines a multi-axis mechanical arm positioning and an automatic continuous ink supply system and adopts a method of colloidal particle assembly and gel curing to deposit the three-dimensional array pattern of structural colors with controllable appearance and adjustable layer number on a hydrophilic-hydrophobic patterned substrate. The method can realize the formation of the sessile liquid drops, ensure the uniform distribution of the printing ink on the substrate, and simultaneously, the liquid drops can be deposited for many times in the vertical direction, thereby realizing the construction of a multilayer structure. The method for preparing the structural color three-dimensional array pattern has the advantages of simple process, random design of microarray pixel point shape, strong pattern adjustability, uniform color, good repeatability and the like, and simultaneously, the multi-color pattern display can be realized by using a plurality of colloidal inks in parallel, and the construction of an optical coding array with a multilayer structure can also be realized.

Description

Method for preparing structural color three-dimensional array pattern based on sessile liquid drops
Technical Field
The invention relates to a method for patterning a structural color material, in particular to a method for preparing a structural color three-dimensional array pattern based on sessile liquid drops.
Background
The color is different from chemical colors such as dyes and pigments, physical colors, also called structural colors, is generated after the ordered micro-nano structure of the material scatters, diffracts or interferes light with different wavelengths, has the advantages of high brightness, high saturation, fastness to fading and the like, and has wide application prospects in the fields of sensing, displaying, anti-counterfeiting labels and the like. The preparation method of the opal structure or one-dimensional structure photonic crystal is an economical preparation method of the structural color material.
In recent years, patterning strategies for various structural color materials have been developed, and the application of the patterning strategies to various components is greatly promoted. For example, a structural color pattern of various topographical features can be constructed by introducing structural color material into a preformed template groove. However, the method has complicated steps, long preparation period and expensive template structure to make the pattern, so that the method cannot meet the requirements of arbitrary customization, mass production and the like. The photolithography technique is an effective way to realize high-precision structural color patterns, but the method also has the problems of expensive price of required instruments, long pattern preparation period and the like. Based on the Chinese patent CN104044380A, a method for preparing continuous photonic crystal patterns by ink-jet printing is disclosed, continuous photonic crystal lines are prepared by controlling the adjacent interval time of continuous ink-jet ink drops, and the simple and convenient and easily-scaled preparation of the continuous photonic crystal patterns is realized. Although the ink jet printing process is fast and efficient, it is highly ink demanding, requires high surface tension and low viscosity, and also places certain demands on the print substrate to overcome the coffee ring effect. The 3D printing technology is a method for efficiently constructing a three-dimensional structural color material developed in recent years, for example, chinese patent CN106042377A discloses a method for adding a structural color coating on a product based on 3D printing, but the structural color printing ink material applied to this scheme is few at present, and the pattern saturation is poor, which limits its large-scale application.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide a method for preparing a structural color three-dimensional array pattern based on sessile liquid drops, which solves the problems of poor pattern designability, poor stability of liquid drop pixel points, complex process, incapability of colorful display and uncontrollable deposition liquid form and structure in the existing method.
The technical scheme is as follows: the invention discloses a method for preparing a structural color three-dimensional array pattern based on sessile droplets, which comprises the following steps:
(1) preparing a printing substrate having a hydrophobic-hydrophilic arrayed micropattern;
(2) the ink containing the monodisperse colloid particles and the polymer precursor is conveyed to a printing nozzle through a continuous ink supply device, and the printing nozzle is controlled by a multi-shaft mechanical arm to construct a fixed drop dot matrix containing the monodisperse colloid particles and the polymer monomer at a local preset position of a substrate;
(3) the fixed drop lattice is solidified by chemical cross-linking, and the colloid particles in the drop are arranged orderly by adopting volatilization self-assembly or external field induced self-assembly to form a structural color pattern.
Wherein the step (1) is specifically as follows: and introducing hydrophilic patterns by using a mask method to perform plasma treatment or ozone treatment on the hydrophobic substrate, or introducing hydrophilic patterns by performing laser burning oxidation on local positions of the hydrophobic substrate.
In the step (2), the mass of the monodisperse colloid particles accounts for 0.01-80% of the mass of the solvent, the mass of the polymer monomer accounts for 1-100% of the mass of the solvent, and the solvent is at least one of water, glycol, dimethylformamide and dimethyl sulfoxide.
The particle size of the monodisperse colloidal particles in the step (2) is 80nm-300nm, and the monodisperse colloidal particles include any one of organic monodisperse colloidal particles, inorganic monodisperse colloidal particles or composite colloidal particles.
The organic monodisperse colloidal particles are polystyrene colloidal particles or polymethyl methacrylate colloidal particles, the inorganic monodisperse colloidal particles are silica, titanium dioxide and ferroferric oxide colloidal particles, and the composite colloidal particles are silica-coated ferroferric oxide and polymethyl methacrylate-coated polystyrene.
The polymer monomer in the step (2) is at least one of acrylamide, dimethylacrylamide, isopropylacrylamide, hydroxyethyl methyl acrylate, phenylboronic acid modified hyperbranched polyethylene glycol diacrylate, polyvinyl alcohol, dextran, sulfydryl or double-bond functionalized gelatin, sulfydryl or double-bond functionalized sodium alginate, sulfydryl or double-bond functionalized hyaluronic acid, hyperbranched polyethylene glycol diacrylate and polyethylene glycol acrylate.
The step (2) is specifically as follows: and constructing a liquid drop dot matrix at a preset position of a printing substrate by a 3D printing multi-axis mechanical arm in a one-dimensional, two-dimensional or three-dimensional positioning writing method.
The polymer crosslinking and curing method in the step (3) is a Michael addition reaction, a photo-initiated free radical polymerization reaction or a thermal-initiated free radical polymerization reaction.
Has the advantages that: the invention can effectively realize the uniform distribution of the colloidal dispersion liquid on the substrate and the formation of the fixed liquid drop by utilizing the hydrophobic-hydrophilic function, and can realize the construction of any liquid drop array pattern by combining the continuous ink supply system and the mechanical arm device; meanwhile, the gel material solidified in situ is introduced into the liquid drops, so that flexible support is provided for the colloid assembly unit, particle sedimentation is effectively inhibited, and the stability and adjustability of the structural color pattern are ensured; the whole process has simple steps and low equipment cost, provides a new technical scheme for realizing the preparation of the colorful pattern with large-area structural color, and has important application value in the fields of optical devices, sensors, biological coding and the like.
Drawings
FIG. 1 is a schematic diagram of a process for fabricating a hydrophobic-hydrophilic array patterned substrate;
FIG. 2 is a graph showing the results of droplet adhesion capability tests of micro-droplets in plasma treated and untreated areas;
FIG. 3 is the molecular formula of the starting material in example 6;
FIG. 4 shows different shapes of structural color material units;
FIG. 5 is a reflectance spectrum of a structural color material;
FIG. 6 is a schematic structural diagram of a microfluidic continuous ink supply device and an automatic positioning device of a mechanical arm;
FIG. 7 is a bi-color structure color pattern prepared based on a fixed dot matrix;
FIG. 8 is a preparation of a patterned array of multilayer structures.
Detailed Description
The invention is further illustrated below with reference to examples and figures.
Example 1
(1) Preparation of structural color ink
Taking 50 mu L of aqueous solution containing 0.1% of silicon dioxide coated ferroferric oxide colloid particles, dissolving 50 mu L of 5% hyperbranched polyethylene glycol diacrylate in the solution, adjusting the pH value to 9, and filling the solution into a first syringe; and (3) taking 100 mu L of 1% thiolated hyaluronic acid, adjusting the pH value of the mixed solution to be 7.5, filling the mixed solution into a second syringe, placing the two syringes on an ink supply device 1 of the microfluidic device, injecting the aqueous solutions of the two syringes into a 3D printing nozzle through the ink supply device, and mixing to obtain the structural color ink.
(2) Preparation of hydrophobic-hydrophilic patterned printing substrates
As shown in fig. 1, a mask method is used to attach laser-punched paper to a black silica gel plate, only micropores are reserved, the paper is placed into an oxygen plasma device for processing, the processed position presents hydrophilicity, the part covered by the paper is hydrophobic, the paper is removed to obtain a hydrophobic-hydrophilic patterned printing substrate, the pattern shape on the printing substrate is changed to obtain droplet arrays with different shapes, fig. 2 shows that the phenomenon of droplet adhesion on the surface can occur when droplets are dripped on the position processed by the oxygen plasma, while the unprocessed position keeps a hemispherical shape, which shows that the processed hydrophilic surface is easy to be fixed with droplets to form the droplet arrays.
(3) Preparation of structural color material patterning
Extruding the structural color ink through microfluidic equipment, connecting an injector with a printing nozzle, controlling the printing nozzle to write the structural color ink in the step (1) at a preset position of a printing substrate in real time by using a multi-axis mechanical arm 2, controlling the 3D printing nozzle to act to accurately control the spatial orientation of the structural color ink, connecting different structural color inks in parallel on an ink supply device to realize colorful printing in spatial positions, and preparing a multilayer structural pattern with structural colors under the condition of a magnetic field.
Example 2
(1) Preparation of structural color ink
Dissolving 10% acrylamide and 1% N, N methylene bisacrylamide in 100 μ L of aqueous solution containing 80% silica colloidal particles, and filling into a first syringe after completely dissolving; and (3) dissolving 5% of photoinitiator 2959 in 100 mu L of water, filling the solution into a second injector after the solution is completely dissolved, injecting the water solution of the two injectors into the 3D printing nozzle through an ink supply device, and mixing to obtain the structural color ink.
(2) Preparation of hydrophobic-hydrophilic patterned printing substrates
And directly printing pattern micropores on a black silica gel plate by adopting a laser etching method, putting a sample into an oxygen plasma device for processing, and tearing off a film on the surface to obtain the hydrophobic-hydrophilic patterned printing substrate.
(3) Preparation of structural color material patterning
Extruding the structural color ink into a printing nozzle by using an ink supply device of the microfluidic control equipment, controlling the printing nozzle by using a multi-shaft mechanical arm to write the structural color ink in the step (1) at a preset position of a printing substrate in real time, and curing by using ultraviolet rays to obtain a multilayer structural pattern with structural colors.
Example 3:
(1) preparation of structural color ink
Dissolving 5% phenylboronic acid modified hyperbranched polyethylene glycol diacrylate, 10% acrylamide and 1% polyvinyl alcohol in 100 μ L of an aqueous solution containing 0.01% polymethyl methacrylate colloidal particles in the mixed solution, adjusting the pH of the mixed solution to 8, and filling the mixed solution into a first syringe; and (3) dissolving 5% of photoinitiator in 100 mu L of water, filling the mixture into a second injector after the photoinitiator is completely dissolved, injecting the water solutions of the two injectors into a 3D printing nozzle through an ink supply device, and mixing to obtain the structural color ink.
(2) Preparation of hydrophobic-hydrophilic patterned printing substrates
And attaching the laser-punched paper to a silica gel plate by using a mask method, only keeping micropores, putting the silica gel plate into oxygen plasma for treatment, wherein the treated position presents hydrophilicity, the untreated position is hydrophobicity, and removing the paper to obtain the hydrophobic-hydrophilic patterned printing substrate.
(3) Preparation of structural color material patterning
Extruding the structural color ink into a printing nozzle by using an ink supply device of the microfluidic control equipment, controlling the printing nozzle by using a multi-shaft mechanical arm to write the structural color ink in the step (1) at a preset position of a printing substrate in real time, and curing by using ultraviolet rays to obtain a multilayer structural pattern with structural colors.
Example 4:
(1) preparation of structural color ink
Dissolving 5% phenylboronic acid modified hyperbranched polyethylene glycol diacrylate, 10% acrylamide and 1% polyvinyl alcohol in 100 μ L of aqueous solution containing 10% polystyrene colloid particles in the mixed solution, adjusting the pH value of the mixed solution to 8, and filling the mixed solution into a first syringe; and (3) dissolving 5% of photoinitiator in 100 mu L of water, filling the mixture into a second injector after the photoinitiator is completely dissolved, injecting the water solutions of the two injectors into a 3D printing nozzle through an ink supply device, and mixing to obtain the structural color ink.
(2) Preparation of hydrophobic-hydrophilic patterned printing substrates
Attaching the laser-punched paper on a silica gel plate by using a mask method, only keeping micropores, putting the silica gel plate into an oxygen plasma device for processing, enabling the processed position to present hydrophilicity, and enabling the unprocessed position to be hydrophobic, and removing the paper to obtain the hydrophobic-hydrophilic patterned printing substrate.
(3) Preparation of structural color material patterning
Extruding the structural color ink into a printing nozzle by using an ink supply device of the microfluidic control equipment, controlling the printing nozzle by using a multi-shaft mechanical arm to write the structural color ink in the step (1) at a preset position of a printing substrate in real time, and curing by using ultraviolet rays to obtain a multilayer structural pattern with structural colors.
Example 5:
(1) preparation of structural color ink
Dissolving 1% isopropyl acrylamide and 0.1% N, N methylene bisacrylamide in 100 μ L of aqueous solution containing 1% ferroferric oxide colloidal particles, and filling the mixture into a first syringe after the mixture is completely dissolved; 5% of potassium persulfate is dissolved in 100 mu L of water, the potassium persulfate is filled into a second injector after being completely dissolved, the water solutions of the two injectors are injected into a 3D printing nozzle through an ink supply device, and the structural color ink is prepared after mixing.
(2) Preparation of hydrophobic-hydrophilic patterned printing substrates
And attaching the laser-punched paper to the silica gel plate by using a mask method, only keeping micropores, and putting the silica gel plate into an oxygen plasma device for treatment, wherein the treated position presents hydrophilicity, and the untreated position presents hydrophobicity. And removing the paper to obtain the hydrophobic-hydrophilic patterned printing substrate.
(3) Preparation of structural color material patterning
Extruding the structural color ink into a printing nozzle by using an ink supply device of the microfluidic control equipment, controlling the printing nozzle by using a multi-shaft mechanical arm to write the structural color ink in the step (1) at a preset position of a printing substrate in real time to obtain an uncured pattern, and placing the uncured pattern into a 60 ℃ drying oven under the condition of a magnetic field for curing and crosslinking to obtain the multilayer structural pattern with structural color.
Example 6:
(1) preparation of structural color ink
Taking 50 mu L of mixed solution of ethylene glycol and water containing 0.1 percent of silicon dioxide coated ferroferric oxide colloidal particles, wherein the mass concentration of the ethylene glycol is 5 percent, and the balance is water. Dissolving 50 μ L of 5% hyperbranched polyethylene glycol diacrylate in the above solution, adjusting the pH to 9, and filling into a first syringe; taking 100 mu L of 2% sulfhydrylated hyaluronic acid, adjusting the pH value of the mixed solution to 7.5, filling the mixed solution into a second syringe, injecting the water solutions of the two syringes into a 3D printing nozzle through an ink supply device, and mixing to obtain the structural color ink, wherein the graph in figure 3 shows that photonic crystals of silicon dioxide coated ferroferric oxide and molecular formulas of sulfhydrylated hyaluronic acid and hyperbranched polyethylene glycol diacrylate are combined with polymer monomers, and the two polymer monomers can form gel through Michael addition reaction of sulfhydryl and double bonds at normal temperature under the alkaline condition.
(2) Preparation of hydrophobic-hydrophilic patterned printing substrates
Attaching the laser-punched paper on a silica gel plate by using a mask method, only keeping micropores, putting the silica gel plate into an oxygen plasma device for processing, wherein the processed position presents hydrophilicity, the unprocessed position is hydrophobicity, and removing the paper to obtain the hydrophobic-hydrophilic patterned printing substrate.
(3) Preparation of structural color material patterning
Extruding the ink supply device of the micro-fluidic equipment for the structural color ink into a printing nozzle, controlling the printing nozzle to write the structural color ink in the step (1) at a preset position of a printing substrate in real time through a multi-shaft mechanical arm, controlling the 3D printing nozzle to accurately control the spatial orientation of the structural color ink, connecting different structural colors of ink in parallel on the ink supply device to realize colorful printing in spatial positions, and finally preparing a multilayer structural pattern with the structural colors under the condition of a magnetic field.
FIG. 4 is a display unit of structural color gel material made into different shapes by way of localized writing using a robotic arm, with plasma treatment of different laser-drilled sheets. Fig. 5 is a spectrum diagram of the prepared structural color material, the magnetic field intensity is gradually increased from right to left, and it can be seen that different structural colors are displayed under different magnetic field intensities. The structural colors in the centrifuge tube in the figure are red, green and blue from right to left in sequence. Fig. 6 is a diagram of an experimental setup of a microfluidic continuous ink supply system and a multi-axis robotic arm automatic positioning system, where a structural color material is combined with a microfluidic, and a robotic arm is used to extrude droplets for patterned positioning writing on a print substrate. Fig. 7 shows a flower pattern with a structural color whose display is controlled by the presence or absence of an applied magnetic field. Fig. 8 shows that a structural color three-dimensional array pattern with multiple layers is formed after curing and crosslinking by dripping ink drops with different structural colors on a hydrophobic-hydrophilic micro-patterned printing substrate.

Claims (6)

1. A method for preparing a structural color three-dimensional array pattern based on sessile droplets is characterized by comprising the following steps:
(1) preparing a printing substrate with a hydrophobic-hydrophilic arrayed micro-pattern, wherein the printing substrate with the hydrophobic-hydrophilic arrayed micro-pattern is constructed by adopting one of the following two ways: introducing hydrophilic patterns by using a mask method to perform plasma treatment or ozone treatment on the hydrophobic substrate, or introducing hydrophilic patterns by performing laser burning oxidation on local positions of the hydrophobic substrate;
(2) the ink containing the monodisperse colloidal particles and the polymer precursor is conveyed to a printing nozzle through a continuous ink supply device, the printing nozzle is controlled by a multi-shaft mechanical arm to construct a sessile drop lattice containing the monodisperse colloidal particles and a polymer monomer at a local preset position of a substrate, and the polymer monomer is at least one of acrylamide, hydroxyethyl methyl acrylate, phenylboronic acid modified hyperbranched polyethylene glycol diacrylate, polyvinyl alcohol, dextran, sulfydryl or double-bond functionalized gelatin, sulfydryl or double-bond functionalized sodium alginate, sulfydryl or double-bond functionalized hyaluronic acid and hyperbranched polyethylene glycol diacrylate;
(3) the fixed drop lattice is solidified by chemical cross-linking, and the colloid particles in the drop are arranged orderly by adopting volatilization self-assembly or external field induced self-assembly to form a structural color pattern.
2. The method for preparing a structural color three-dimensional array pattern based on sessile droplets as claimed in claim 1, wherein the mass fraction of the monodisperse colloidal particles in step (2) is 0.01-80% of the mass of the solvent, the mass fraction of the polymer precursor is 1-100% of the mass fraction of the solvent, and the solvent is at least one of water, ethylene glycol, dimethylformamide and dimethylsulfoxide.
3. The method for producing a three-dimensional array pattern of structural colors based on sessile droplets as claimed in claim 1, wherein said monodisperse colloidal particles in step (2) have a particle size of 80nm to 300nm, and said monodisperse colloidal particles comprise any one of organic monodisperse colloidal particles, inorganic monodisperse colloidal particles or composite colloidal particles.
4. The method for preparing a structural color three-dimensional array pattern based on sessile droplets as claimed in claim 3, wherein the organic monodisperse colloidal particles are polystyrene colloidal particles or polymethyl methacrylate colloidal particles, the inorganic monodisperse colloidal particles are silica, titanium dioxide, ferroferric oxide colloidal particles, and the composite colloidal particles are silica-coated ferroferric oxide, polymethyl methacrylate-coated polystyrene.
5. The method for producing a structural color three-dimensional array pattern based on sessile droplets as claimed in claim 1, wherein said step (2) is specifically: and constructing a liquid drop dot matrix at a preset position of a printing substrate by a 3D printing multi-axis mechanical arm in a one-dimensional, two-dimensional or three-dimensional positioning writing method.
6. The method for preparing a structural color three-dimensional array pattern based on sessile droplets as claimed in claim 1, wherein the chemical crosslinking curing method in step (3) is a Michael addition reaction, a photo-initiated radical polymerization reaction or a thermal initiated radical polymerization reaction.
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