CN112095076A - High-saturation optical color-changing material and preparation method thereof - Google Patents

High-saturation optical color-changing material and preparation method thereof Download PDF

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Publication number
CN112095076A
CN112095076A CN201910528224.2A CN201910528224A CN112095076A CN 112095076 A CN112095076 A CN 112095076A CN 201910528224 A CN201910528224 A CN 201910528224A CN 112095076 A CN112095076 A CN 112095076A
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optical color
changing material
changing
color
optically variable
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吴伟才
龙芬
罗华强
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Huizhou Foryou Optical Technology Co ltd
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Huizhou Foryou Optical Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58—After-treatment
    • C23C14/5806—Thermal treatment

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)

Abstract

The application discloses an optical color-changing material and a preparation method thereof, wherein the method comprises the following steps: preparing a first optical color-changing material by adopting a physical vapor deposition method; and carrying out heat treatment on the first optical color-changing material to obtain a second optical color-changing material. Through the mode, the color saturation and brightness of the optical color-changing pigment or the film can be improved, and the performances of acid resistance, alkali resistance and the like can be improved.

Description

High-saturation optical color-changing material and preparation method thereof
Technical Field
The application relates to the technical field of optical color-changing materials, in particular to an optical color-changing material and a preparation method thereof.
Background
The optical color-changing material has a color-changing phenomenon related to an observation angle, and an observer can observe different colors at different angles, particularly, the optical color-changing film can show obviously different colors when the optical color-changing film is observed at an angle of 0 degree or 60 degrees relative to the normal direction of the surface of the optical color-changing film. The optical color-changing material is widely applied to the fields of anti-counterfeiting, printing and the like due to the characteristics.
However, with the increasing requirements in all aspects of production and life, the current photochromic materials have difficulty in meeting the use requirements in many fields in the aspects of acid resistance, alkali resistance, color and the like.
Disclosure of Invention
The technical problem mainly solved by the application is to provide the optical color-changing material and the preparation method thereof, which can improve the performances of the optical color-changing material such as hue saturation, brightness, acid resistance, alkali resistance and the like.
In order to solve the technical problem, the application adopts a technical scheme that: provided is a method for preparing an optically variable material, the method comprising: preparing a first optical color-changing material by adopting a physical vapor deposition method; and carrying out heat treatment on the first optical color-changing material to obtain a second optical color-changing material.
Wherein the step of heat-treating the first optically variable material to obtain a second optically variable material comprises: and carrying out heat treatment on the first optical color-changing material by adopting at least one of high-temperature annealing, electric heating, microwave heating, laser heating and infrared heating to obtain the second optical color-changing material.
Further, the time for carrying out heat treatment on the first optical color changing material is 0-48 h.
Specifically, the time for carrying out heat treatment on the first optical color-changing material is 5 min-24 h.
Further, the temperature for carrying out heat treatment on the first optical color changing material is 100-1600 ℃.
Specifically, the temperature for performing heat treatment on the first optical color-changing material is 300-1200 ℃.
Specifically, the optical color-changing material is at least one of titanium-containing optical color-changing material, chromium-containing optical color-changing material and all-dielectric optical color-changing material.
Further, before the heat treatment of the first optical color-changing material, the method further comprises: crushing the first optical color-changing material to obtain a crushed first optical color-changing material; the step of heat-treating the first optically variable material to obtain the second optically variable material comprises: and carrying out heat treatment on the crushed first optical color changing material to obtain the second optical color changing material.
Wherein the particle size of the first optical color-changing material is 1-5000 μm.
Further, the particle size of the crushed first optical color changing material is 1-100 μm.
In order to solve the above technical problem, another technical solution adopted by the present application is: an optical color-changing material is provided, and the optical color-changing material is prepared by the preparation method.
The beneficial effect of this application is: different from the prior art, the preparation method of the optical color-changing material comprises the following steps: preparing a first optical color-changing material by adopting a physical vapor deposition method, and carrying out heat treatment on the first optical color-changing material to obtain a second optical color-changing material. The optical color-changing material after heat treatment has a more compact structure, thereby improving the performances of color saturation, brightness, acid resistance, alkali resistance and the like of the optical color-changing material.
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 of one embodiment of a method for preparing an optically variable material according to the present disclosure;
FIG. 2 is a schematic flow chart of another embodiment of the process for preparing the photochromic material of the present application.
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.
Referring to fig. 1, fig. 1 is a schematic flow chart of an embodiment of a method for preparing an optical color-changing material according to the present application, the method including:
step S11: preparing a first optical color-changing material by adopting a physical vapor deposition method;
step S12: and carrying out heat treatment on the first optical color changing material to obtain a second optical color changing material.
Specifically, both the first optical color-changing material and the second optical color-changing material may be at least one of a titanium-containing optical color-changing material, a chromium-containing optical color-changing material, an all-dielectric optical color-changing material, and the like, and of course, other optical color-changing materials may also be used, which are not specifically limited herein.
Further, both the first optically variable material and the second optically variable material may be pigments such as powdery, granular, or flaky pigments, or may be films. Specifically, the second optical material prepared by the method can be used in the fields of printing, high-safety anti-counterfeiting, glass pigment, ceramic pigment, injection molding and the like.
The heat treatment of the first photochromic material may include at least one of high temperature annealing, electrical heating, microwave heating, laser heating, infrared heating, and the like.
Specifically, the time for performing the heat treatment on the first optical color-changing material may be 0 to 48 hours, specifically, 5min, 1 hour, 5 hours, 10 hours, 24 hours, 36 hours, 48 hours, and the like, and may be specifically set according to actual requirements, which is not specifically limited herein. Further, the temperature for performing the heat treatment on the first optical color changing material is 100 ℃ to 1600 ℃, specifically, 100 ℃, 300 ℃, 800 ℃, 1200 ℃, 1600 ℃ and the like, which is not limited herein.
It should be noted that, in the related art, the optical color-changing pigment can be prepared only by physical vapor deposition, however, the optical color-changing material prepared only by physical vapor deposition has relatively poor resistance (such as acid resistance, alkali resistance, etc.), and cannot meet the use requirement to a certain extent; in another preparation method, a chemical liquid phase deposition method can be adopted, and a high-temperature calcination method is further adopted for preparation, but the optical color-changing pigment prepared by the method has low saturation and large pigment particle size; there is also a way to produce them by chemical vapour deposition in a fluidised bed, which, however, is highly demanding with respect to raw materials and with respect to equipment.
In the embodiment, the first optical color-changing material is further subjected to heat treatment on the basis of the preparation of the first optical color-changing material by the physical vapor deposition method, so that the structure of the obtained second optical color-changing material is more compact, the acid resistance and alkali resistance of the optical color-changing pigment are improved, the brightness is higher, the color is brighter, and the use requirement is met.
Further, referring to fig. 2, in one embodiment, a method for preparing an optical color-changing material includes:
step S21: preparing a first optical color-changing material by adopting a physical vapor deposition method;
step S22: crushing the first optical color-changing material to obtain a crushed first optical color-changing material;
step S23: and carrying out heat treatment on the crushed first optical color changing material to obtain a second optical color changing material.
It is to be noted that the first optically variable material prepared in the present embodiment may be an optically variable film, and after being pulverized, a granular optically variable pigment is obtained.
Wherein the particle size of the first optical discoloration material after being crushed can be 1-5000 μm, or can also be 1-100 μm, or 10-30 μm, etc.
Other relevant contents are similar to step S11 and step S12 in the above embodiment, and please refer to the above embodiment for relevant details, which are not described herein again.
The present application further provides an optical color-changing material, which can be prepared by the method in the above embodiment of the preparation method of the optical color-changing material, and for related preparation methods, reference is made to the above embodiment of the preparation method, and details are not repeated here.
The optical color-changing material in the present embodiment is a second optical color-changing material obtained by heat treatment in the embodiment of the optical color-changing material production method. The optical material can be a pigment, such as a powdery, granular or flaky pigment, or can also be a film, and the like, and can be particularly used in the fields of printing, high-safety anti-counterfeiting, glass pigment, ceramic pigment, injection molding and the like. It is noted that the optical color-changing material has a more compact structure due to heat treatment, so that the optical color-changing material has more excellent acid resistance and alkali resistance, and has higher brightness and more bright color.
The above embodiments of the present application will be described below with reference to specific examples.
1. The titanium-containing optical color-changing film is prepared by a vacuum physical vapor deposition method, the optical color-changing film is vertically observed to be green, the optical color-changing film is observed to be pink at an angle of 60 degrees, and the obtained optical color-changing film is marked as a No. 1 sample.
2. And (3) carrying out electric heating treatment on the optical color-changing film prepared in the step (1), specifically, treating at 1000 ℃ for 2h, then slowly cooling to room temperature to obtain a transparent optical color-changing film with a green front color and a pink side color, and marking the obtained optical color-changing film as a No. 2 sample.
3. The optically variable film prepared in step 1 was pulverized into an optically variable pigment having a particle diameter of (10-30) μm, and the resulting optically variable pigment was designated as sample # 3.
4. And (3) performing electric heating treatment on the optical color-changing pigment prepared in the step (3), specifically treating at 700 ℃ for 30min, then slowly cooling to room temperature to obtain a semitransparent optical color-changing pigment with green front color and pink side color, and marking the obtained optical color-changing pigment as a No. 4 sample.
5. And (3) carrying out infrared heating treatment on the optical color changing pigment prepared in the step (3), specifically, treating at 400 ℃ for 3h, then slowly cooling to room temperature to obtain the optical color changing pigment with the front color being green and the side color being pink, and marking the obtained optical color changing pigment as a No. 5 sample.
6. A commercially available all-dielectric optically variable pigment was used as sample # 6.
The following tests were carried out on the above samples:
a. acid and alkali resistance test: respectively carrying out acid and alkali resistance tests on 1#, 2#, 3#, 4#, 5# and 6# samples by using the national standard (GB/T5211.5-2008);
b. and (3) testing the reflectivity and the saturation: respectively testing the reflectivity and the saturation of samples 1#, 2#, 3#, 4#, 5# and 6# by using a data color photometer;
d. specific surface test: the 3# and 4# samples were tested for specific surface area using static liquid nitrogen test.
Wherein, in the above test, the test results of acid resistance, alkali resistance, reflectivity and saturation are as the following table 1:
table 1 results of performance testing of various samples
Sample (I) Acid resistance Alkali resistance Reflectivity/%) Degree of saturation
1# 4 stage Grade 3 25.01 34.24
2# (4-5) stage (4-5) stage 54.85 47.52
3# (3-4) grade Grade 3 35.81 41.90
4# (4-5) stage (4-5) stage 52.88 49.37
5# 4 stage 4 stage 45.31 48.25
6# Grade 3 Grade 3 35.33 16.36
Wherein, the acid resistance grade: and 5, stage: approximation; 4, level: slightly different; and 3, level: a clear difference; and 2, stage: only traces are present; level 1: disappearance; alkali resistance series: and 5, stage: approximation; 4, level: slightly different; and 3, level: a clear difference; and 2, stage: only traces are present; level 1: and (4) disappearing.
The specific surface test results are shown in table 2 below:
TABLE 2 specific surface area test results of the pigments before and after the treatment
Sample (I) BET specific surface area method Aperture (sample inside)
3# 4.087m2/g 2.146nm
4# 3.097m2/g 2.066nm
As can be seen from Table 1, the acid and alkali resistances of the No. 2, No. 4 and No. 5 samples after heat treatment are improved compared with those of the No. 1 and No. 3 samples without heat treatment and the No. 6 sample on the market, and are improved by 1 to 2 grades, and meanwhile, the reflectivity and the saturation value are also obviously increased. Therefore, the optical color-changing material obtained by the method has better acid resistance and alkali resistance, higher brightness and more bright color.
From the specific surface area comparison in table 2, it was found that the specific surface area of the sample # 3 which was not heat-treated was larger than that of the sample # 4 which was heat-treated, indicating that the pigment was more dense after heat treatment.
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 (10)

1. A method for preparing an optically variable material, comprising:
preparing a first optical color-changing material by adopting a physical vapor deposition method;
and carrying out heat treatment on the first optical color-changing material to obtain a second optical color-changing material.
2. The method of claim 1, wherein the step of heat treating the first optically variable material to obtain a second optically variable material comprises:
and carrying out heat treatment on the first optical color-changing material by adopting at least one of high-temperature annealing, electric heating, microwave heating, laser heating and infrared heating to obtain the second optical color-changing material.
3. The method according to claim 1, wherein the first photochromic material is heat-treated for 0 to 48 hours.
4. The method according to claim 3, wherein the first photochromic material is heat-treated for 5min to 24 hours.
5. The method of claim 1, wherein the temperature for heat treating the first optically variable material is from 100 ℃ to 1600 ℃.
6. The method of claim 5, wherein the temperature for heat-treating the first optically variable material is 300 ℃ to 1200 ℃.
7. The method of claim 1, wherein the optical color-changing material is at least one of a titanium-containing optical color-changing material, a chromium-containing optical color-changing material, and an all-dielectric optical color-changing material.
8. The method of claim 1, wherein prior to thermally treating the first optically variable material, the method further comprises:
crushing the first optical color-changing material to obtain a crushed first optical color-changing material;
the step of heat-treating the first optically variable material to obtain the second optically variable material comprises:
and carrying out heat treatment on the crushed first optical color changing material to obtain the second optical color changing material.
9. The method of claim 8, wherein the particle size of the pulverized first optically variable material is 1 μ ι η to 5000 μ ι η, or 1 μ ι η to 100 μ ι η.
10. An optically variable material produced by the production method according to any one of claims 1 to 9.
CN201910528224.2A 2019-06-18 2019-06-18 High-saturation optical color-changing material and preparation method thereof Pending CN112095076A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114134464A (en) * 2021-10-26 2022-03-04 惠州市华阳光学技术有限公司 Structural color pigment and preparation method thereof

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JP2014113800A (en) * 2012-12-12 2014-06-26 Pilot Ink Co Ltd Applicator of color change material and color change material set
CN104559425A (en) * 2015-01-03 2015-04-29 中山市天键金属材料有限公司 Preparation method for surface-coated magnesium fluoride laser aluminum powder
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CN1693388A (en) * 2005-06-09 2005-11-09 上海印钞厂 Optical disclour pigment with polarization effect, its preparation process and manufactured printing ink
JP2014113800A (en) * 2012-12-12 2014-06-26 Pilot Ink Co Ltd Applicator of color change material and color change material set
CN104559425A (en) * 2015-01-03 2015-04-29 中山市天键金属材料有限公司 Preparation method for surface-coated magnesium fluoride laser aluminum powder
CN108752977A (en) * 2018-06-29 2018-11-06 林中 There is the pigment and preparation method thereof of high brightness, excitation purity and covering effect simultaneously
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Publication number Priority date Publication date Assignee Title
CN114134464A (en) * 2021-10-26 2022-03-04 惠州市华阳光学技术有限公司 Structural color pigment and preparation method thereof

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