CN107974131B - Carbon dot ink and preparation method and application thereof - Google Patents
Carbon dot ink and preparation method and application thereof Download PDFInfo
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- CN107974131B CN107974131B CN201711136053.6A CN201711136053A CN107974131B CN 107974131 B CN107974131 B CN 107974131B CN 201711136053 A CN201711136053 A CN 201711136053A CN 107974131 B CN107974131 B CN 107974131B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/50—Sympathetic, colour changing or similar inks
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/16—Writing inks
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- G—PHYSICS
- G06—COMPUTING; CALCULATING OR COUNTING
- G06F—ELECTRIC DIGITAL DATA PROCESSING
- G06F21/00—Security arrangements for protecting computers, components thereof, programs or data against unauthorised activity
- G06F21/60—Protecting data
- G06F21/602—Providing cryptographic facilities or services
Abstract
The invention discloses carbon dot ink and a preparation method and application thereof, wherein cationic polymer electrolyte and anionic polymer electrolyte are used as raw materials to obtain carbon dots, and then the carbon dot ink is prepared in a self-assembly mode.
Description
Technical Field
The invention relates to the field of carbon nano materials, in particular to carbon dot ink and a preparation method and application thereof.
Background
Information security issues in the economic, military, political and daily lives are increasingly being valued by people. In recent years, researchers have developed a series of related technologies such as plasma security tags, magnetic response and luminescence imaging to protect these important and valuable data from corruption and counterfeiting. Among them, fluorescence imaging has many significant advantages including simple preparation, easy operation, high yield, etc., and is widely used for data security.
Fluorescence imaging can become a powerful technique for data recording, security and anti-counterfeiting, and mainly originates from the emergence of various fluorescent materials. It is reported that some fluorescent materials such as fluorescent crystals, transition metal complexes, dyes, etc. can be applied to optical data recording, device protection, sensor matrix, etc. by external mechanical, thermal, and vapor stimulation techniques. The potential biotoxicity, low light resistance, high cost and low stability of most materials have hindered their practical use.
As an emerging nanomaterial, fluorescent carbon dots have recently received increasing attention in bioimaging, photocatalysis, sensing, optoelectronic devices and other applications due to their unique advantages of environmental protection, enhanced chemical inertness, low toxicity, excellent biocompatibility, excellent chemo-optical stability, and excellent optoelectronic properties. Much research is currently focused on the preparation of carbon dots. Among them, the hydrothermal reaction of a carbon precursor is more and more widely used due to its advantages of greenness, economy, and simplicity of operation. Most of carbon points synthesized by hydrothermal method have hydrophilic group, so it can be dissolved in water well, and this property is very beneficial to application such as biological imaging, medical diagnosis and ink imaging. However, such carbon dots are generally not practical in environments where humidity and temperature change with time due to severe instability of the material to water or organic solvents due to weak van der waals and affinity forces between the surface groups of the carbon dots and the substrate.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of carbon dot ink, which has the advantages of low cost, simple and efficient preparation process, environment-friendly prepared carbon dot ink, high stability and capability of being applied to the fields of data information encryption, printing display and the like.
The technical scheme adopted by the invention is as follows:
the invention provides a preparation method of carbon dot ink, which comprises the following steps:
adding a solvent into a cationic polymer electrolyte, and transferring the cationic polymer electrolyte into a reaction kettle to react to obtain a first solution;
taking a dialysis bag to dialyze the solution I, collecting the solution outside the permeation bag, and drying to obtain carbon dots I;
adding a solvent into the anionic polymer electrolyte, and transferring the anionic polymer electrolyte into a reaction kettle to react to obtain a solution II;
dialyzing the solution II by using a dialysis bag, collecting the solution outside the permeation bag, and drying to obtain carbon dots II;
and (3) adding a solvent into the carbon dot I to prepare a solution III, adding a solvent into the carbon dot II to prepare a solvent IV, and mixing the solution III and the solution IV to prepare the carbon dot ink, wherein the charge number of the ions of the solution III is the same as that of the ions of the solution IV.
Preferably, the cationic polymer electrolyte is at least one of polyacrylamide hydrochloride, polyethyleneimine and polydiallyldimethylammonium chloride.
Preferably, the anionic polymer electrolyte is at least one of sodium polystyrene sulfonate and polyacrylic acid.
Preferably, the solvent is deionized water.
Preferably, the dialysis bag has a molecular weight cut-off of 3500 or less.
Preferably, the temperature of the reaction in the reaction kettle is 150-250 ℃.
Preferably, the reaction time in the reaction kettle is more than or equal to 5 hours.
Preferably, the dialysis time is 48h or more.
The invention also provides carbon dot ink prepared by the preparation method of the carbon dot ink.
The carbon dot ink is applied to the fields of data information encryption and printing display.
The invention has the beneficial effects that:
the carbon dot ink obtained by the preparation method has the optical properties of the traditional fluorescent ink, and the data written on paper has higher stability, and can be applied to the fields of data information encryption, printing display and the like.
Drawings
FIG. 1 is a schematic diagram of the preparation of a carbon dot ink in example 1;
FIG. 2 is a TEM topography of the carbon dot ink of example 1;
FIG. 3 is a graph of the fluorescence spectra of the carbon dot ink of example 1 at different excitation wavelengths;
FIG. 4 is a stability test of the carbon dot ink of the present invention.
Detailed Description
The concept and technical effects of the present invention will be clearly and completely described below in conjunction with the embodiments and the accompanying drawings to fully understand the objects, features and effects of the present invention. It is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and those skilled in the art can obtain other embodiments without inventive effort based on the embodiments of the present invention, and all embodiments are within the protection scope of the present invention.
Example 1
Weighing 10g of polyacrylamide hydrochloride (PAH) to dissolve in 10mL of deionized water, transferring the solution after ultrasonic dissolution to a 30mL reaction kettle with a polytetrafluoroethylene lining, and reacting for 5 hours in an oven at 200 ℃. Dialyzing the solution obtained by the above reaction for three days by using a dialysis bag with molecular weight cutoff of 3500 to remove the solution as a reaction raw material and an intermediate product, collecting the solution outside the dialysis bag, and freeze-drying to obtain powdery carbon dots I.
10g of sodium polystyrene sulfonate (PSS) is weighed and dissolved in 10mL of deionized water, the solution is transferred to a reaction kettle with a 30mL polytetrafluoroethylene lining after ultrasonic dissolution, and the reaction is carried out for 5 hours in an oven at 200 ℃. Dialyzing the solution obtained by the reaction for three days by using a dialysis bag with the molecular weight cutoff of 3500 to remove the solution as a reaction raw material and an intermediate product, collecting the solution outside the dialysis bag, and freeze-drying to obtain a powdery carbon dot II.
Dissolving the first carbon dot in deionized water to obtain a first solution, dissolving the second carbon dot in deionized water to obtain a second solution, calculating the number of cationic charges in the first solution according to the mass of the first solution and the molecular weight of the polyelectrolyte repeating units in the first solution, calculating the number of anionic charges in the second solution according to the mass of the second solution and the molecular weight of the polyelectrolyte repeating units in the second solution, and controlling the adding amount of the first carbon dot and the second carbon dot according to equivalent weight calculation so that the number of ionic charges in the first solution is equal to that in the second solution, and mixing the first solution and the second solution to obtain the carbon dot ink.
Example 2
Weighing 10g of polyacrylamide hydrochloride (PAH) to dissolve in 10mL of deionized water, transferring the solution after ultrasonic dissolution to a 30mL reaction kettle with a polytetrafluoroethylene lining, and reacting in an oven at 150 ℃ for 8 hours. Dialyzing the solution obtained by the reaction for four days by using a dialysis bag with the molecular weight cutoff of 2000 to remove the solution as a reaction raw material and an intermediate product, collecting the solution outside the dialysis bag, and freeze-drying to obtain powdery carbon dots I.
10g of sodium polystyrene sulfonate (PSS) is weighed and dissolved in 10mL of deionized water, the solution is transferred to a reaction kettle with a 30mL polytetrafluoroethylene lining after ultrasonic dissolution, and the reaction is carried out in an oven at 150 ℃ for 8 hours. Dialyzing the solution obtained by the reaction for three days by using a dialysis bag with the molecular weight cutoff of 2000 to remove the solution as a reaction raw material and an intermediate product, collecting the solution outside the dialysis bag, and freeze-drying to obtain a powdery carbon dot II.
And (3) dissolving the first carbon dot in deionized water to obtain a first solution, dissolving the second carbon dot in deionized water to obtain a second solution, controlling the adding amount of the first carbon dot and the second carbon dot to ensure that the number of charges carried by the ions in the first solution is the same as that of the ions in the second solution, and mixing the first solution and the second solution to obtain the carbon dot ink.
Example 3
10g of Polyethyleneimine (PEI) was weighed, dissolved in 10mL of deionized water, ultrasonically dissolved, transferred to a 30mL polytetrafluoroethylene-lined reaction kettle, and reacted in an oven at 250 ℃ for 10 hours. Dialyzing the solution obtained by the reaction for three days by using a dialysis bag with the molecular weight cutoff of 1000 to remove the solution as a reaction raw material and an intermediate product, collecting the solution outside the dialysis bag, and freeze-drying to obtain powdery carbon dots I.
10g of polyacrylic acid (PAA) was weighed, dissolved in 10mL of deionized water, ultrasonically dissolved, transferred to a 30mL polytetrafluoroethylene-lined reaction vessel, and reacted in an oven at 250 ℃ for 10 hours. Dialyzing the solution obtained by the reaction for 48h by using a dialysis bag with the molecular weight cutoff of 1000 to remove the solution as a reaction raw material and an intermediate product, collecting the solution outside the dialysis bag, and freeze-drying to obtain powdery carbon dots II.
And (3) dissolving the first carbon dot in deionized water to obtain a first solution, dissolving the second carbon dot in deionized water to obtain a second solution, controlling the adding amount of the first carbon dot and the second carbon dot to ensure that the number of charges carried by the ions in the first solution is the same as that of the ions in the second solution, and mixing the first solution and the second solution to obtain the carbon dot ink.
Example 4
10g of poly (diallyldimethylammonium chloride) (PDDA) was weighed, dissolved in 10mL of deionized water, ultrasonically dissolved, transferred to a 30mL polytetrafluoroethylene-lined reaction vessel, and reacted in an oven at 180 ℃ for 5 hours. Dialyzing the solution obtained by the reaction for 60h by using a dialysis bag with the molecular weight cutoff of 3500 to remove the solution as a reaction raw material and an intermediate product, collecting the solution outside the dialysis bag, and freeze-drying to obtain powdery carbon dots I.
10g of sodium polystyrene sulfonate (PSS) is weighed and dissolved in 10mL of deionized water, the solution is transferred to a reaction kettle with a 30mL polytetrafluoroethylene lining after ultrasonic dissolution, and the reaction is carried out for 5 hours in an oven at 180 ℃. Dialyzing the solution obtained by the reaction for three days by using a dialysis bag with the molecular weight cutoff of 3500 to remove the solution as a reaction raw material and an intermediate product, collecting the solution outside the dialysis bag, and freeze-drying to obtain a powdery carbon dot II.
And (3) dissolving the first carbon dot in deionized water to obtain a first solution, dissolving the second carbon dot in deionized water to obtain a second solution, controlling the adding amount of the first carbon dot and the second carbon dot to ensure that the number of charges carried by the ions in the first solution is the same as the number of charges carried by the ions in the second solution, and mixing the first solution and the second solution to obtain the carbon dot ink, wherein the self-assembly process is shown in figure 1. The TEM topography of the carbon dot ink is shown in FIG. 2, and it can be seen from the graph that the carbon dot size distribution is uniform, and the diameter of the carbon dot is 15-50 nm.
The fluorescence spectrograms of the carbon dot ink under the excitation wavelengths of 310nm, 320nm, 330nm, 340nm, 350nm, 360nm, 370nm and 380nm are taken, as shown in FIG. 3, and the optimal excitation wavelength is 310 nm.
Example 5: stability test
Using the solution one (C-PAH), the solution two (C-PSS) and the carbon dot inks (SA-CDs) in example 1, data were written on paper, respectively, the paper was air-dried, and the paper was put in water (H) under ultraviolet rays, respectively2O), n-hexane, chloroform (CHCl)3) And dimethyl sulfoxide (DMSO), the phenomenon was observed after 5 minutes, as shown in fig. 4. As can be seen from the figure, the data written by using the C-PAH and C-PSS solution as the fluorescent carbon dots are stable in organic solvent and extremely unstable in aqueous solution, while the data written by using the carbon dot ink SA-CDs prepared by the invention show excellent stability in both aqueous solution and organic solvent, which shows that the carbon dot ink prepared based on self-assembly not only has the fluorescence performance of the traditional fluorescent ink, but also has high stability, and can be applied to the fields of data information encryption, printing display and the like.
Example 6
A mixture of 10g of polyallylamine hydrochloride (PAH) and Polyethyleneimine (PEI) was weighed out and dissolved in 10mL of deionized water, and after ultrasonic dissolution, the mixture was transferred to a 30mL polytetrafluoroethylene-lined reaction kettle and reacted in an oven at 250 ℃ for 10 hours. Dialyzing the solution obtained by the reaction for three days by using a dialysis bag with the molecular weight cutoff of 1000 to remove the solution as a reaction raw material and an intermediate product, collecting the solution outside the dialysis bag, and freeze-drying to obtain powdery carbon dots I.
10g of polyacrylic acid (PAA) was weighed, dissolved in 10mL of deionized water, ultrasonically dissolved, transferred to a 30mL polytetrafluoroethylene-lined reaction vessel, and reacted in an oven at 250 ℃ for 10 hours. Dialyzing the solution obtained by the reaction for 48h by using a dialysis bag with the molecular weight cutoff of 1000 to remove the solution as a reaction raw material and an intermediate product, collecting the solution outside the dialysis bag, and freeze-drying to obtain powdery carbon dots II.
And (3) dissolving the first carbon dot in deionized water to obtain a first solution, dissolving the second carbon dot in deionized water to obtain a second solution, controlling the adding amount of the first carbon dot and the second carbon dot to ensure that the number of charges carried by the ions in the first solution is the same as that of the ions in the second solution, and mixing the first solution and the second solution to obtain the carbon dot ink.
Example 7
A mixture of 10g of Polyethyleneimine (PEI) was weighed out and dissolved in 10mL of deionized water, and after ultrasonic dissolution, the mixture was transferred to a 30mL polytetrafluoroethylene-lined reaction vessel and reacted in an oven at 250 ℃ for 10 hours. Dialyzing the solution obtained by the reaction for three days by using a dialysis bag with the molecular weight cutoff of 1000 to remove the solution as a reaction raw material and an intermediate product, collecting the solution outside the dialysis bag, and freeze-drying to obtain powdery carbon dots I.
A mixture of 10g of sodium polystyrene sulfonate (PSS) and polyacrylic acid (PAA) was weighed, dissolved in 10mL of deionized water, ultrasonically dissolved, transferred to a 30mL polytetrafluoroethylene-lined reaction vessel, and reacted in an oven at 250 ℃ for 10 hours. Dialyzing the solution obtained by the reaction for 48h by using a dialysis bag with the molecular weight cutoff of 1000 to remove the solution as a reaction raw material and an intermediate product, collecting the solution outside the dialysis bag, and freeze-drying to obtain powdery carbon dots II.
And (3) dissolving the first carbon dot in deionized water to obtain a first solution, dissolving the second carbon dot in deionized water to obtain a second solution, controlling the adding amount of the first carbon dot and the second carbon dot to ensure that the number of charges carried by the ions in the first solution is the same as that of the ions in the second solution, and mixing the first solution and the second solution to obtain the carbon dot ink.
Claims (8)
1. A preparation method of carbon dot ink is characterized by comprising the following steps:
adding a solvent into a cationic polymer electrolyte, and transferring the cationic polymer electrolyte into a reaction kettle to react to obtain a first solution;
taking a dialysis bag to dialyze the solution I, collecting the solution outside the permeation bag, and drying to obtain carbon dots I;
adding a solvent into the anionic polymer electrolyte, and transferring the anionic polymer electrolyte into a reaction kettle to react to obtain a solution II;
dialyzing the solution II by using a dialysis bag, collecting the solution outside the permeation bag, and drying to obtain carbon dots II;
and adding a solvent into the first carbon dot to prepare a third solution, adding a solvent into the second carbon dot to prepare a fourth solution, and mixing the third solution with the fourth solution to prepare the carbon dot ink, wherein the charge number of ions of the third solution is the same as that of ions of the fourth solution, the cationic polymer electrolyte is at least one of polyacrylamide hydrochloride, polyethyleneimine and polydiallyldimethylammonium chloride, and the anionic polymer electrolyte is at least one of sodium polystyrene sulfonate and polyacrylic acid.
2. The method of claim 1, wherein the solvent is deionized water.
3. The method of claim 1, wherein the dialysis bag has a molecular weight cut-off of 3500.
4. The method for preparing the carbon dot ink according to claim 1, wherein the reaction temperature in the reaction kettle is 150 to 250 ℃.
5. The method for preparing the carbon dot ink according to claim 1, wherein the reaction time in the reaction kettle is not less than 5 hours.
6. The method for preparing the carbon dot ink according to claim 1, wherein the dialysis time is not less than 48 hours.
7. A carbon dot ink produced by the method for producing a carbon dot ink according to any one of claims 1 to 6.
8. Use of the carbon dot ink according to claim 7 in the fields of data information encryption and print display.
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| CN109540857B (en) * | 2018-11-12 | 2021-05-04 | 安庆师范大学 | Preparation method of fluorescent test paper for rapidly detecting barium ions |
| CN110294963B (en) * | 2019-08-12 | 2022-02-08 | 厦门欧化实业有限公司 | Water-based UV treatment-free surface printing ink and processing method and processing equipment thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1826393A (en) * | 2003-06-17 | 2006-08-30 | 伊利诺斯大学理事会 | Polyelectrolyte ink |
| CN107099288A (en) * | 2017-04-01 | 2017-08-29 | 深圳市华星光电技术有限公司 | The preparation method and carbon point laminated film of carbon point laminated film |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1826393A (en) * | 2003-06-17 | 2006-08-30 | 伊利诺斯大学理事会 | Polyelectrolyte ink |
| CN107099288A (en) * | 2017-04-01 | 2017-08-29 | 深圳市华星光电技术有限公司 | The preparation method and carbon point laminated film of carbon point laminated film |
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