CN111239859A

CN111239859A - Optical film/pigment flake, preparation method and device

Info

Publication number: CN111239859A
Application number: CN201811341757.1A
Authority: CN
Inventors: 马道远
Original assignee: Shenzhen Rongguang Nano Technology Co ltd
Current assignee: Shenzhen Rongguang Nano Technology Co ltd
Priority date: 2018-11-12
Filing date: 2018-11-12
Publication date: 2020-06-05

Abstract

The application discloses an optical thin film/pigment flake, a preparation method and a device, wherein the preparation method comprises the following steps: placing the stripped optical thin film/pigment flake into a container, wherein the gaps of the stripped optical thin film/pigment flake contain ions to be removed, and the ions to be removed comprise release agent ions; adding a solution containing a first ionized substance to the container, wherein the first ionized substance contains a matching ion corresponding to the ion to be removed, so as to combine the ion to be removed with the matching ion in an ionization reaction, thereby removing the ion to be removed from the gap. In this way, the present application can remove ions to be removed from the voids of the optical film/pigment flake, thereby improving the stability and durability of the pigment flake in the coating.

Description

Optical film/pigment flake, preparation method and device

Technical Field

The application relates to the technical field of luminescent pigments, in particular to an optical thin film/pigment flake, a preparation method and a device.

Background

With the widespread use of nanotechnology, various industries began using optical thin films to make pigment flakes. The optical thin film is generally formed on a substrate, the optical thin film and the substrate are separated by a release layer (or a sacrificial layer), the release layer is removed at the later stage to obtain the optical thin film, and the optical thin film is crushed to obtain the pigment flake.

In the long-term research process, the inventor of the present application finds that when the release layer is water-soluble, the method for removing the release layer is generally water washing, the release layer ionizes ions when the release layer is water washed, the ions penetrate into each gap of the optical thin film along with the flow of the aqueous solution, and the ions adversely affect the optical thin film and the pigment flakes prepared subsequently.

Disclosure of Invention

The technical problem that this application mainly solved is to provide an optical thin film/pigment flake, preparation method and device, can remove the ion that will be removed from the space of optical thin film/pigment flake.

In order to solve the technical problem, the application adopts a technical scheme that: a method for preparing an optical film/pigment flake is provided, the method comprising: placing the stripped optical thin film/pigment flake into a container, wherein the gap of the stripped optical thin film/pigment flake contains ions to be removed; adding a solution containing a first ionized substance to the container, wherein the first ionized substance contains a matching ion corresponding to the ion to be removed, so as to combine the ion to be removed with the matching ion in an ionization reaction, thereby removing the ion to be removed from the gap.

Wherein the combining the ions to be removed with the matching ions comprises: the matching ions are combined with the ions to be removed to be precipitated in a precipitate form.

Wherein the adding of the solution containing the first ionized species to the container comprises: dropwise adding the solution containing the first ionized substance to the container under a predetermined stirring speed until no precipitate is precipitated.

Wherein the predetermined stirring speed is 20-60 revolutions per minute.

Wherein the solution containing the first ionized substance is dropwise added into the container under a predetermined stirring speed until no precipitate is precipitated, and thereafter, the preparation method further comprises: stirring is continued for a first predetermined time at a first stirring speed.

Wherein the method further comprises, prior to placing the stripped optical films/pigment flakes in a container: and washing the stripped optical thin film/pigment flake for multiple times by using a first solvent to remove part of ions to be removed.

Wherein the first ionized species ionizes the matched ion and corresponding other ions in an ionization reaction, and the adding a solution containing the first ionized species to the container, the method further comprises: and washing the optical thin film/pigment flake for multiple times by using a second solvent to remove the other ions.

The ions to be removed are ions generated by dissolution of a stripping layer when the optical thin film/pigment flake is stripped, wherein the ions to be removed comprise chloride ions, the first ionized substance comprises silver nitrate, silver ions and nitrate ions are ionized by the silver nitrate in an ionization reaction, and the chloride ions and the silver ions are combined to form silver chloride precipitate.

In order to solve the above technical problem, another technical solution adopted by the present application is: an optical film/pigment flake is provided, which is obtained by the method of any of the above embodiments.

In order to solve the above technical problem, the present application adopts another technical solution: an apparatus for making optical films/flakes is provided, the apparatus comprising: the container is used for bearing the optical thin film/pigment flake after demoulding, and the gap of the optical thin film/pigment flake after demoulding contains ions to be removed; a liquid inlet component for adding a solution containing a first ionized substance containing a matching ion corresponding to the ion to be removed into the container to combine the ion to be removed with the matching ion in an ionization reaction, thereby removing the ion to be removed from the gap.

The beneficial effect of this application is: in contrast to the prior art, the present application provides a method for preparing optical films/pigment flakes comprising: adding a solution containing a first ionized substance into a container in which the stripped optical thin film/pigment flake is placed, wherein the first ionized substance contains matching ions corresponding to the ions to be removed, so that the ions to be removed are combined by the matching ions in an ionization reaction, thereby removing the ions to be removed from the gaps, further reducing the adverse effect of the ions to be removed on the optical thin film/pigment flake, and further improving the stability and durability of the pigment flake in the coating layer, wherein the ions to be removed can be releasing agent ions and the like.

Drawings

In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts. Wherein:

FIG. 1 is a schematic flow chart illustrating one embodiment of a method for manufacturing a conventional optical film;

FIG. 2 is a schematic structural diagram of an embodiment corresponding to steps S101-S103 in FIG. 1;

FIG. 3 is a schematic flow chart diagram illustrating one embodiment of a method for making optical films/pigments according to the present disclosure;

fig. 4 is a schematic diagram of an embodiment of an apparatus for making optical films/flakes according to the present disclosure.

Detailed Description

The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.

For ease of understanding, the prior art process flow for making optical films/flakes is first described.

Referring to fig. 1-2, fig. 1 is a schematic flow chart of an embodiment of a method for manufacturing an optical film in the prior art, and fig. 2 is a schematic structural diagram of an embodiment corresponding to steps S101-S103 in fig. 1, where the method includes:

s101: providing a substrate 10;

specifically, in one embodiment, the material of the substrate 10 may be plastic (e.g., polyethylene hard plastic, etc.), glass, mirror stainless steel, etc. with a smooth and flat surface.

S102: forming a first release layer 12 on one side of the substrate 10;

specifically, in one embodiment, the first release layer 12 may be formed by a vacuum evaporation coating method in the related art.

S103: forming a first optical film 14 on the side of the first release layer 12 away from the substrate 10;

specifically, in one embodiment, the first optical film 14 may be formed by using a vacuum coating apparatus, the first optical film 14 may be any one of the prior art, and may be a single-layer or multi-layer film (metal or dielectric film), the total thickness of the first optical film 14 may be 50-1800 nm (e.g., 50, 500, 1000, 1800 nm, etc.), and the first optical film 14 has better optical reflection performance, photochromic performance, appropriate physical strength and chemical stability against corrosion.

In one application scenario, the first optical thin film 14 is a multilayer film, which may be formed sequentially and has a structure of Cr4L Cr4L Cr; wherein, L is silicon dioxide, and the thicknesses are respectively 5 nanometers, 440 nanometers, 20 nanometers, 440 nanometers and 5 nanometers. In another application scenario, the first optical film 14 has a structure of Cr4L Ag 4L Cr, wherein the thicknesses are 5.5 nm, 440 nm, 18 nm, 440 nm, and 5.5 nm, respectively. In other application scenarios, the structure of the first optical film 14 may be other, and the present application is not limited thereto.

S104: the first release layer 12 is removed to peel off the first optical film 14.

Specifically, in one embodiment, the material of the first release layer 12 is water-soluble, and the method for removing the first release layer 12 may be to place the whole in an aqueous solution, and dissolve the first release layer 12 in the aqueous solution, thereby obtaining the first optical film 14.

In other embodiments, to improve production efficiency, a multilayer optical film may be prepared on the substrate 10. Before the step S104, the method for manufacturing an optical film provided by the present application further includes: A. forming a second release layer 16 on the side of the first optical film 14 away from the first release layer 12, wherein the first release layer 12 and the second release layer 16 are made of the same or different materials; B. and a second optical film 18 is formed on the side of the second release layer 16 far away from the first optical film 14, and the second optical film 18 is made of the same material as the first optical film 14. Repeating the steps A and B to obtain the multilayer optical film laminated structure. And finally, placing the multilayer optical film laminated structure in an aqueous solution to obtain the multilayer optical film.

In other embodiments, the multilayer optical film can be peeled to obtain a pigment flake, which can be pulverized to form a pigment flake. For example, the solution with the multilayer optical film can be placed in an ultrasonic solution and sonicated to fragment the multilayer optical film into pigment flakes.

As can be seen from the above-mentioned preparation methods, the existing methods for preparing optical films or pigment flakes do not recognize that when the release layer is removed by water washing, if the release layer is an ionizable substance, the release layer undergoes an ionization reaction after entering the aqueous solution, and the ionized ions penetrate into the voids of the optical films or pigment flakes along with the flow of the aqueous solution, thereby adversely affecting the optical films/pigment flakes. Referring to fig. 3, fig. 3 is a schematic flow chart of an embodiment of a method for preparing an optical film/pigment flake according to the present application, in which the optical film is obtained after stripping, and the steps shown in fig. 3 can be performed on the optical film, or the steps shown in fig. 3 can be performed on the pigment flake after the pigment flake is made from the optical film. Specifically, the method provided by the application comprises the following steps:

s201: placing the stripped optical thin film/pigment flake into a container, wherein the gap of the stripped optical thin film/pigment flake contains ions to be removed;

specifically, in this embodiment, before the step S201, the method for obtaining the optical thin film or the pigment flake can be referred to the above embodiments, and is not described herein again. In this embodiment, the optical thin film/pigment flakes after being removed or the solution in which the optical thin film/pigment flakes are mixed may be placed in a container, which may be a conventional reaction vessel such as a flask.

In an application scenario, in order to reduce difficulty in subsequent processing of ions to be removed, before step S201, the preparation method provided by the present application further includes: and washing the stripped optical thin film/pigment flake for multiple times by using a first solvent to remove part of ions to be removed. The first solvent may be water, etc., and for example, the stripped optical film/pigment flakes may be washed with water and suction filtered 2 times, 3 times, etc. to remove a portion of the ions to be removed.

S202: adding a solution containing a first ionized substance containing a matching ion corresponding to the ion to be removed to the container to bind the ion to be removed with the matching ion in an ionization reaction, thereby removing the ion to be removed from the void.

Specifically, in the present embodiment, the matching ions contained in the first ionized substance are precipitated in the form of precipitates in combination with the ions to be removed, and the ions to be removed are removed from the gaps. Of course, in other embodiments, other forms are possible, for example, forms in which the matching ions form complexes with the ions to be removed.

In an application scenario, the adding the solution containing the first ionized substance into the container in step S202 specifically includes: the solution containing the first ionised species is added dropwise to the vessel at a predetermined stirring rate until no precipitate is formed. The stirring is provided for fully reacting the matching ions with the ions to be removed, and the dropwise adding is performed for increasing the pressure for subsequently removing the redundant first ionized substances in order to avoid the excessive adding amount of the first ionized substances. The means for providing a predetermined stirring speed in the present application may be a mechanical stirring device, a magnetic stirring device, etc., and the predetermined stirring speed may be 20 rpm to 60 rpm, for example, 20 rpm, 40 rpm, 60 rpm, etc. The apparatus for providing the condition of dropwise addition may be a constant pressure burette, a fully automatic burette or the like, and the rate of addition may be set according to the actual circumstances, for example, 40ml/h, 50ml/h or the like.

In another application scenario, in order to make the reaction between the ions to be removed and the matching ions more complete, after the step of "adding dropwise the solution containing the first ionized substance to the container at the predetermined stirring speed until no precipitate is precipitated", the preparation method provided by the present application further comprises: stirring is continued for a first predetermined time at a first stirring speed. The first predetermined time may be 2 to 4 hours, for example, 2 hours, 3 hours, 4 hours, and the like. And the first stirring speed in this step may be the same as or different from the predetermined stirring speed, which is not limited in this application.

In another embodiment, the first ionized substance may ionize a matching ion and also ionize other corresponding ions in an ionization reaction, and after step S202, the method further includes: the optical film/pigment flakes are washed multiple times with a second solvent to remove other ions. The second solvent can be water or the like, for example, the optical film/pigment flakes can be washed with water and suction filtered 2 times, 3 times, etc. to remove other ions.

In a specific application scenario, the ions to be removed are ions generated by dissolving a stripping layer when the optical thin film/pigment flake is stripped, and the ions to be removed comprise chloride ions; for example, when the release layer is sodium chloride, the sodium chloride ionizes chloride ions and sodium ions during water elution, and the chloride ions permeate into the respective voids of the optical film with the flow of water, adversely affecting the optical film and the pigment flakes formed by crushing the optical film. This is because chloride ions are strongly polar ions and corrosive, and when the optical thin film is crushed to form pigment flakes, they corrode the flakes; in addition, since chloride ions are strongly polar ions, they are liable to react with functional groups of organic substances, which results in deterioration of stability and durability of a coating material prepared from the pigment flakes. Therefore, it is necessary to remove the chloride ions at the optical thin film stage or the pigment flake stage. The process of removing chloride ions from the voids of the optical film/pigment flake using the preparation method provided herein will be described in detail.

A. Cleaning with water, and filtering the optical thin film/pigment flake after demoulding for 2 times;

B. placing the optical film/pigment flake in a container, and dropwise adding an aqueous solution containing a first ionized substance silver nitrate under the stirring condition until no white flocculent precipitate is generated; in this example, silver nitrate undergoes an ionization reaction in an aqueous solution to ionize silver ions and nitrate ions, and chloride ions combine with silver ions to form a silver chloride precipitate, and the chemical reaction equation is as follows:

NaCl+AgNO₃＝NaNO₃+AgCl↓。

of course, in other embodiments, the first ionized substance may be other substances, for example, a substance containing mercurous ions, cadmium ions, etc., and both the mercurous ions and the cadmium ions may form a precipitate with the chloride ions to be precipitated from the solution.

C. Stirring for 2 hours;

D. the mixed solution containing the optical thin film/pigment flakes was washed with water and suction-filtered 3 times to remove nitrate ions.

The amount of ions to be removed contained in the gaps of the optical thin film/pigment flake obtained after the treatment by the method is greatly reduced, the corrosivity of the ions to be removed to the optical thin film is greatly reduced, and the stability and the durability of the coating prepared by the pigment flake are also greatly improved.

Referring to fig. 4, fig. 4 is a schematic structural diagram of an embodiment of an apparatus for preparing optical thin films/pigment flakes according to the present disclosure, the apparatus 2 comprising:

a container 20 for carrying the optical thin film/pigment flake after the film is removed, wherein the gap of the optical thin film/pigment flake after the film is removed contains ions to be removed; in one embodiment, the container 20 may be a flask or the like, e.g., a 2-neck flask, a 3-neck flask, or the like.

And the liquid inlet component 22 is used for adding a solution containing a first ionized substance into the container 20, wherein the first ionized substance contains matched ions corresponding to the ions to be removed, so that the matched ions are combined with the ions to be removed in an ionization reaction, and the ions to be removed are removed from the gaps. In one embodiment, the inlet assembly 22 includes a constant pressure dropping funnel or the like. In other embodiments, the inlet assembly 22 may be other, such as a burette or the like.

With continued reference to fig. 4, the apparatus provided herein further includes a stirring assembly 24, wherein the stirring assembly 24 includes a stirring rod 240 and a driving member 242 connected to an end of the stirring rod 240; the driving member 242 may drive the stirring rod 240 to rotate at a predetermined stirring speed. Of course, in other embodiments, the stirring assembly 24 may also include a magneton and a driving member associated with the magneton.

To secure the container 20 and the inlet assembly 22, referring again to fig. 4, the apparatus provided by the present application further includes a securing assembly 26, and in one embodiment, the securing assembly 26 includes a stand 260 and a clip 262. The iron stand 260 includes a base plate 2600 and a rod portion 2602, one end of the rod portion 2602 is fixedly connected to the base plate 2600, one end of the iron clamp 262 is fixedly connected to the rod portion 2602, and the other end of the iron clamp 262 is fixedly connected to one end of the container 20.

In summary, unlike the prior art, the present application provides a method for making optical films/pigment flakes comprising: adding a solution containing a first ionized substance containing matching ions corresponding to the ions to be removed into a container in which the optical thin film/pigment flake is placed after the film is removed, so that the ions to be removed (for example, release agent ions) are combined by the matching ions in an ionization reaction, thereby removing the ions to be removed from the gaps, further reducing the adverse effect of the ions to be removed on the optical thin film/pigment flake, and further improving the stability and durability of the pigment flake in the coating.

The above description is only for the purpose of illustrating embodiments of the present application and is not intended to limit the scope of the present application, and all modifications of equivalent structures and equivalent processes, which are made by the contents of the specification and the drawings of the present application or are directly or indirectly applied to other related technical fields, are also included in the scope of the present application.

Claims

1. A method of making an optical film/pigment flake, the method comprising:

placing the stripped optical thin film/pigment flake into a container, wherein the gap of the stripped optical thin film/pigment flake contains ions to be removed;

adding a solution containing a first ionized substance to the container, wherein the first ionized substance contains a matching ion corresponding to the ion to be removed, so as to combine the ion to be removed with the matching ion in an ionization reaction, thereby removing the ion to be removed from the gap.

2. The method according to claim 1, wherein the combining the ions to be removed with the matching ions comprises:

the matching ions are combined with the ions to be removed to be precipitated in a precipitate form.

3. The method of claim 2, wherein the adding a solution containing a first ionized species to the container comprises:

dropwise adding the solution containing the first ionized substance to the container under a predetermined stirring speed until no precipitate is precipitated.

4. The production method according to claim 3,

the preset stirring speed is 20-60 revolutions per minute.

5. The method of claim 3, wherein the solution containing the first ionizable substance is added dropwise to the vessel at a predetermined stirring speed until no precipitate precipitates, and thereafter, the method further comprises:

stirring is continued for a first predetermined time at a first stirring speed.

6. The method of claim 1, wherein the step of placing the stripped optical film/pigment flakes in a container further comprises:

and washing the stripped optical thin film/pigment flake for multiple times by using a first solvent to remove part of ions to be removed.

7. A method of producing as claimed in claim 1 wherein the first ionised species ionises the matching ion and corresponding further ions in an ionisation reaction, and wherein the adding of the solution containing the first ionised species to the vessel thereafter further comprises:

and washing the optical thin film/pigment flake for multiple times by using a second solvent to remove the other ions.

8. The production method according to claim 1,

9. An optical film/pigment flake obtained by the method of any one of claims 1 to 8.

10. An apparatus for making optical films/flakes, comprising:

the container is used for bearing the optical thin film/pigment flake after demoulding, and the gap of the optical thin film/pigment flake after demoulding contains ions to be removed;

a liquid inlet component for adding a solution containing a first ionized substance containing a matching ion corresponding to the ion to be removed into the container to combine the ion to be removed with the matching ion in an ionization reaction, thereby removing the ion to be removed from the gap.