WO2020114396A1 - 一种颜料的制造方法 - Google Patents
一种颜料的制造方法 Download PDFInfo
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- WO2020114396A1 WO2020114396A1 PCT/CN2019/122760 CN2019122760W WO2020114396A1 WO 2020114396 A1 WO2020114396 A1 WO 2020114396A1 CN 2019122760 W CN2019122760 W CN 2019122760W WO 2020114396 A1 WO2020114396 A1 WO 2020114396A1
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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
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/0015—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
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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
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
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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
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
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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
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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
- C23C14/0005—Separation of the coating from the substrate
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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
- C23C14/0015—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterized by the colour of the layer
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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
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
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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
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/20—Metallic material, boron or silicon on organic substrates
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/04—Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of organic materials, e.g. plastics
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
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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
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
- C09C2200/30—Interference pigments characterised by the thickness of the core or layers thereon or by the total thickness of the final pigment particle
- C09C2200/308—Total thickness of the pigment particle
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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
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
- C09C2200/40—Interference pigments comprising an outermost surface coating
- C09C2200/402—Organic protective coating
- C09C2200/403—Low molecular weight materials, e.g. fatty acids
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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
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C2220/00—Methods of preparing the interference pigments
- C09C2220/20—PVD, CVD methods or coating in a gas-phase using a fluidized bed
Definitions
- the present application relates to the technical field of thin films, in particular to a method for manufacturing pigments.
- Structural color also known as physical color, for example, due to the extremely thin wax layer, engraved dots, grooves or scales on the insect body wall, light waves are refracted, diffusely reflected, diffracted or Various colors produced by interference.
- structural color technology the manufacture of pigments based on optical films is becoming more and more important.
- the manufacturing method of the pigment based on the optical film includes a roll-to-roll winding coating, or a sacrificial layer method of multi-layer stacking and an intermediate space release agent on a box-type coating machine.
- the inventor of the present application discovered during the long-term development process that the equipment for winding the coating is expensive and the production efficiency is low; while the multilayer coating on the box-type coating machine, the sodium chloride stripper in the middle is used as a sacrificial layer to produce During the process, the film layer irregularly fell off, causing production interruption.
- the technical problem mainly solved by the present application is to provide a method for manufacturing pigments, which can avoid irregular peeling of the film layer during the production process without increasing production costs, thereby avoiding production interruption.
- a technical solution adopted by the present application is to provide a method for manufacturing a pigment, the method comprising: providing a substrate; and sequentially forming a plurality of sets of thin films stacked on the substrate, each set of the The thin film includes a sacrificial layer and an optical thin film layer that are sequentially stacked, wherein the sacrificial layer is a mold release agent with low stress or compressive stress; multiple sets of the thin film after the formation are subjected to film release treatment and crushing treatment, respectively, to obtain ⁇ pigment.
- the present application provides a substrate; multiple sets of thin films are sequentially stacked on the substrate, and each set of the thin films includes a sequentially stacked sacrificial layer and an optical thin film layer , Wherein the sacrificial layer is a mold release agent with low stress or compressive stress; a plurality of sets of the formed thin film are subjected to mold release treatment and pulverization treatment to obtain the pigment.
- the sacrificial layer is a mold release agent with low stress or compressive stress
- the sacrificial layer is a release agent with low or compressive stress, and the total stress of the multilayer optical film is tensile stress, the release agent is separated in between, reducing the transfer and accumulation of the tensile stress of the optical film, resulting in The total stress of multiple sets of thin films is reduced to avoid irregular peeling of the film layer during the production process. In this way, the irregular peeling of the film layer during the production process can be avoided on the basis of not increasing the production cost, thereby avoiding production interruption.
- FIG. 1 is a schematic flowchart of an embodiment of a method for manufacturing a pigment of the present application
- FIG. 2 is a schematic flow chart of another embodiment of a method for manufacturing a pigment of the present application.
- FIG. 3 is a schematic diagram of a plurality of stacked sets of films formed in a practical application in step S102 of a method for manufacturing a pigment of the present application.
- Structural color also known as physical color
- the pigment based on the optical film that is, the principle of producing color according to the structural color, is industrially mass-produced by artificial manufacturing to obtain an optical film that can produce color, and then the corresponding pigment.
- Pigments based on optical films currently do not have a unified professional name some are called optically variable pigments, some are called optical interference color-changing pigments and pearlescent pigments.
- optically variable pigments some are called optical interference color-changing pigments and pearlescent pigments.
- it is divided into two categories commonly known as: chameleon pigment and omnidirectional pigment. Simply put, the color of chameleon pigments is different when viewed at different angles, such as the "100" words of RMB 100 yuan banknotes and US dollar 100 yuan banknotes; and omnidirectional pigments are also called invariant pigments, that is, at different angles The color is close when observed, and the change is small.
- optical film-based pigments The principle of optical film-based pigments is similar to that of pearl gloss.
- Newton's optical theory states that sunlight is composed of many different colors of light. In daylight, a non-transparent substance absorbs or transmits incident light of a certain wavelength, and the reflected light of another wavelength is the color of the object.
- the color of the reflected light from the multilayer optical film varies depending on the number of layers, the thickness of the layer, and the refractive index of the layer. Among them, because these reflected light and transmitted light are from the same light wave, the optical path difference of the two beams decomposed by the incident light is different. When they meet the coherent light conditions, the coherent interference of the light can produce a specific color. That is the principle of optical film pigments.
- the manufacturing method of the pigment based on the optical film includes a roll-to-roll winding coating, or a method of stacking a sacrificial layer of a multi-layered, spaced-in-between release agent on a box-type coating machine.
- the equipment for winding the coating is expensive and the production efficiency is low; on the box coating machine, multiple layers are superimposed, and the sodium chloride stripper in the middle is used as a sacrificial layer.
- the film is irregularly peeled off during the production process, causing production interruption.
- the method for manufacturing a pigment in the present application is a method for manufacturing a pigment based on an optical film. Since the sacrificial layer is a release agent with low stress or compressive stress, the total stress of the multilayer optical film is tensile stress, and the interval of the release agent In the meantime, the release agent isolates, reduces the transmission and accumulation of the tensile stress of the optical film, resulting in the reduction of the total stress of multiple sets of films, avoiding the irregular peeling of the film layer during the production process. In this way, it can increase the production cost without increasing On the basis of this, the film layer can be prevented from falling off irregularly during the production process, thereby avoiding production interruption.
- FIG. 1 is a schematic flowchart of an embodiment of a method for manufacturing a pigment of the present application. The method includes:
- Step S101 Provide a substrate.
- the substrate is often made of polyester, polyester, polyimide, glass, or metal.
- polyester is mostly polyethylene terephthalate (PET)
- polyester is mostly polyvinyl chloride (Polyvinyl chloride, PVC).
- PET polyethylene terephthalate
- PVC polyvinyl chloride
- Step S102 Multiple sets of thin films are sequentially stacked on the substrate, and each set of thin films includes a sacrificial layer and an optical thin film layer that are sequentially stacked, wherein the sacrificial layer is a release agent with low stress or compressive stress.
- the sacrificial layer is a mold release agent having low stress or compressive stress.
- Compressive stress refers to the stress that resists the object's tendency to compress.
- the release agent with low stress or compressive stress can be searched according to the test, or it can be verified by the test after preliminary determination based on experience.
- the sacrificial layer may only include a mold release agent with low stress or a compressive stress release agent, or a mixture of these mold release agents with other mold release materials, and so on. Further, the content and thickness of the release agent are also determined according to specific actual needs, and can be determined by testing twice during the production process.
- the mold release agent is a soluble substance that can generate compressive stress or low stress in the film layer after the evaporation coating.
- the mold release agent may be at least one of inorganic salts, organic acid salts, base salts and the like.
- the inorganic salt may specifically be at least one of hydrochloride, nitrate, sulfate, phosphate, and carbonate
- the organic acid salt may specifically be one of acrylate, acetate, and stearate.
- the base salt may specifically be at least one of NaOH, KOH, Ca(OH) 2 and the like.
- the stripping agent may also be other soluble substances that can generate compressive stress or low stress in the film layer after evaporation coating, which is not specifically limited here.
- the material of the sacrificial layer does not contain a release agent with compressive stress.
- the material that uses sodium chloride as the release agent due to the accumulation of tensile stress during the coating process, results in the irregularity of the coating layer during the coating process Shedding, causing production interruptions and reducing production efficiency.
- the sacrificial layer is a release agent with low stress or compressive stress
- the total stress of the multilayer optical film is tensile stress
- the release agent is spaced in between, the release agent is isolated, and partially offsets the tensile stress of the optical film Transmission and accumulation, resulting in the reduction of the total stress of multiple sets of films, to avoid irregular film shedding during production, in this way, on the basis of not increasing production costs, to avoid irregular film shedding during production, production
- the process is not interrupted, which can improve production efficiency.
- the optical thin film layer may include at least one of a dielectric layer, a semiconductor layer, and a metal layer.
- the dielectric layer may be formed of silicon oxide, aluminum oxide, titanium oxide, zirconium oxide, etc., and may be formed by vacuum deposition methods such as electron beam heating evaporation, magnetron sputtering evaporation, and resistance heating evaporation;
- the semiconductor layer may be formed of silicon, germanium It is formed by vacuum deposition such as electron beam heating evaporation and resistance heating evaporation;
- the metal layer can be formed by vacuum deposition such as silver, chromium, copper, nickel, aluminum and the like by electron beam heating evaporation and resistance heating evaporation.
- the optical film layer may also include other layers, which is not specifically limited here.
- step S102 may include: sub-step S1021, sub-step S1022, sub-step S1023, and sub-step S1024.
- Sub-step S1021 A stripping agent is evaporated on the substrate to form a sacrificial layer.
- Sub-step S1022 plating an optical film layer on the substrate on which the sacrificial layer is evaporated to obtain the first set of films.
- At least one method of physical vapor deposition (PVD), chemical vapor deposition (CVD), atomic layer deposition (ALD), etc. may be used for plating.
- PVD physical vapor deposition
- CVD chemical vapor deposition
- ALD atomic layer deposition
- at least one method such as resistance thermal evaporation, electron beam evaporation, sputtering, and ion-assisted evaporation can be used. In the actual operation process, it can be selected according to actual needs, which is not specifically limited here.
- Sub-step S1023 repeat the above steps, stack the sacrificial layer and the optical film layer on the first set of films, and then stack the second set of films on the first set of films.
- Sub-step S1024 repeat the above steps, repeatedly superimpose the sacrificial layer and the optical film layer, and then sequentially form a plurality of stacked sets of films on the substrate.
- FIG. 3 is a schematic diagram of a plurality of stacked sets of films formed in an actual application in step S102.
- the sacrificial layer 2 uses the release agent in the above embodiment, and the number of films is 50. Set as an example.
- a layer of sacrificial layer 2 is vapor-deposited on the substrate 1, and an optical film layer 3 is further plated on the substrate 1 with the sacrificial layer 2 evaporated to obtain a first set of films n1, wherein the sacrificial layer 2 and the optical film layer 3 can be formed by vacuum deposition machine; then, repeat the above steps, the sacrificial layer 2 and the optical film layer 3 are superimposed on the first set of thin film n1, and then the second set of thin film n2 is stacked on the first set of thin film n1 Repeat the above steps, repeatedly stack the sacrificial layer 2 and the optical film layer 3, and then form the 50th set of stacked films n50 on the substrate in sequence.
- the substrate in the vacuum chamber of the coating machine evaporate and deposit the release agent to form a sacrificial layer, plate an optical thin film layer on the sacrificial layer, the sacrificial layer and the optical thin film layer form a set of films, and then repeatedly stack multiple sets of the above films ; Because the total stress of the film is tensile stress, and the interval between the release agent, the compressive stress of the release agent partially blocks, offsets the transfer and accumulation of the tensile stress, resulting in the reduction of the total stress of multiple sets of films, avoiding the production process
- the film layer is irregularly peeled, and up to 50 sets of thin films can be deposited.
- a sacrificial layer of sodium chloride with tensile stress is used. Due to the large total stress, the film layer is irregularly dropped, and only about 10 sets of thin films can be deposited.
- the stripping agent has compressive stress or low stress, it can make multiple sets of stacked films not fall off during the coating process, and the production process is not interrupted. Therefore, expensive equipment can be used, and only a common vacuum coating machine can be used to coat multiple sets of stacks. Of the film, thus ensuring no increase in production costs.
- step S102 may specifically be that a box-type vacuum coating machine is used to sequentially form a plurality of stacked thin films on the substrate.
- Step S103 performing film release treatment and crushing treatment on the formed multiple sets of films respectively to obtain pigments.
- the coated multiple sets of thin films are subjected to stripping and crushing treatment, for example, placed in an ultrasonic bath filled with an organic solvent acetone or methyl ethyl ketone solution or water. Generally, the thin films can be broken by ultrasonic for about 30 minutes.
- Embodiments of the present application provide a substrate; multiple sets of thin films are sequentially stacked on the substrate, and each set of the thin films includes a sequentially stacked sacrificial layer and an optical thin film layer, wherein the sacrificial layer has low stress or compression Stress release agent; perform film release treatment and pulverization treatment on the multiple sets of the formed thin film to obtain the pigment.
- the sacrificial layer is a release agent with low or compressive stress
- the total stress of the film is tensile stress
- the compressive or low stress of the release agent partially blocks the transfer of the tensile stress of the film, resulting in multiple sets
- the total stress of the thin film is reduced to avoid the irregular falling of the film layer during the production process. In this way, the irregular falling of the film layer during the production process can be avoided on the basis of not increasing the production cost, thereby avoiding production interruption.
- the optical thin film is formed by sequentially depositing materials with different refractive indexes on the same carrier under high vacuum conditions in accordance with the requirements of the film system structure.
- the material is evaporated onto the carrier in the form of molecules or atoms.
- the consistency of the evaporation rate must be strictly controlled; and in order to control the color index of the film system, the film thickness error must be Control within the range of Egypt. This shows the precision and particularity of optical film production.
- the ideal optical film is a symmetrical structure, and the thickness of the film system is about 1 micron. Because the film system is made under high vacuum, all the colorless or transparent inorganic materials are used.
- the resulting optical film pigment has stable performance, dense structure, no fading, strong weather resistance, good shear resistance, and can be pressed.
- the particle size requirements of the ink are arbitrarily crushed.
- the number of sets of the above-mentioned multiple sets of films may be 10-55 sets.
- the prior art uses sodium chloride as the material of the sacrificial layer, and the film layer is irregularly peeled off: sometimes 15 sets are superimposed and sometimes 5 sets are superimposed. Interrupt the production process.
- the number of stacked film sets can reach 10-55 sets, or even more than 55 sets.
- the pigment is in the form of flakes.
- the pigment is in the form of flakes with a thickness of 0.015 to 1 micrometer and a length and width of 5 to 200 micrometers.
- the shape and particle size of the pigment are determined according to the actual application scenario or printing and spraying methods.
- the method further includes: determining the thickness of the sacrificial layer in advance.
- the thickness of the sacrificial layer can be determined based on experience, and it is necessary to ensure that the thin film can be separated even if the substrate is separated from the thin film.
- the thickness of the sacrificial layer can also be determined by experiment. That is, the thickness of the sacrificial layer may be determined in advance by adjusting the thickness of the sacrificial layer through multiple tests in advance so that the sacrificial layer can separate the thin film during the film release process. Generally speaking, the thickness of the sacrificial layer can be obtained after 3 trials.
- the prepared pigment can be further surface-treated, that is, the method further includes: performing surface treatment on the pigment after the pulverization treatment.
- the general surface treatment is to put the crushed pigment into a saturated solution of rosin or stearic acid (such as dehydroabietic acid, tetrahydroabietic acid, etc.), stir for more than half an hour, and then precipitate, filter, and bake Just do it.
- the pigment after the above treatment is evenly mixed into the transparent ink binder, and then an appropriate amount of co-solvent and rheology control agent are added.
- Commonly used ink binders include rosin modified phenolic resin, maleic resin and polyamide resin.
- Co-solvents help stabilize or use the composition.
- Co-solvents include glycol ethers, glycol ether acetates, and the like.
- the rheology control agent includes hectorite clay, fumed silica, bentonite clay, cellulose and so on. It should be noted that the addition ratio of the above-mentioned added substances is not limited to the spectral characteristics of the ink.
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Abstract
一种颜料的制造方法,该方法包括:提供衬底;在衬底上依次形成叠加的多套薄膜,每套薄膜包括依次叠加的牺牲层和光学薄膜层,其中,牺牲层是具有应力或低应力的脱膜剂;对形成后的多套薄膜分别进行脱膜处理和粉碎处理,得到颜料。该方法能够在不增加生产成本的基础上,避免生产过程中膜层不规则脱落,从而避免生产中断。
Description
本申请涉及薄膜技术领域,特别是涉及一种颜料的制造方法。
结构色(structural color),又称物理色(physical color),例如由于昆虫体壁上有极薄的蜡层、刻点、沟缝或鳞片等细微结构,使光波发生折射、漫反射、衍射或干涉而产生的各种颜色。随着结构色技术的产品化,基于光学薄膜的颜料的制造越来越重要。
现有技术中,基于光学薄膜的颜料的制造方法,包括卷对卷的卷绕镀膜,或者在箱式镀膜机上多层叠加、中间间隔脱膜剂的牺牲层办法。但是,本申请的发明人在长期的研发过程中发现:卷绕镀膜的设备昂贵、生产效率低;而箱式镀膜机上多层叠加,中间间隔氯化钠脱膜剂作牺牲层的办法,生产过程中膜层不规则脱落、造成生产中断。
【发明内容】
本申请主要解决的技术问题是提供一种颜料的制造方法,能够在不增加生产成本的基础上,避免生产过程中膜层不规则脱落,从而避免生产中断。
为解决上述技术问题,本申请采用的一个技术方案是:提供一种颜料的制造方法,所述方法包括:提供衬底;在所述衬底上依次形成叠加的多套薄膜,每套所述薄膜包括依次叠加的牺牲层和光学薄膜层,其中,所述牺牲层是具有低应力或压应力的脱膜剂;对形成后的多套所述薄膜分别进行脱膜处理和粉碎处理,得到所述颜料。
本申请的有益效果是:区别于现有技术的情况,本申请提供衬底;在所述衬底上依次形成叠加的多套薄膜,每套所述薄膜包括依次叠加的牺牲层和光学薄膜层,其中,所述牺牲层是具有低应力或压应力的脱膜剂;对形成后的多套 所述薄膜分别进行脱膜处理和粉碎处理,得到所述颜料。由于牺牲层是具有低应力或压应力的脱膜剂,而多层光学薄膜的总应力是张应力,脱膜剂间隔其间,脱膜剂隔离、降低了光学薄膜张应力的传递和积累,导致多套薄膜的总应力减小,避免生产过程中膜层不规则脱落,通过这种方式,能够在不增加生产成本的基础上,避免生产过程中膜层不规则脱落,从而避免生产中断。
图1是本申请一种颜料的制造方法一实施方式的流程示意图;
图2是本申请一种颜料的制造方法又一实施方式的流程示意图;
图3是本申请一种颜料的制造方法步骤S102在一实际应用中形成的叠加的多套薄膜的示意图。
在详细说明本申请的方法之前,先介绍一下与本申请相关的基础知识以及现有技术情况。
结构色(structural color),又称物理色(physical color),是一种由光与结构相互作用而引发的光泽,比如由于昆虫体壁上有极薄的蜡层、刻点、沟缝或鳞片等细微结构,使光波发生折射、漫反射、衍射或干涉而产生的各种颜色。基于光学薄膜的颜料,即根据结构色产生颜色的原理,采用人工制造的方式工业化大规模生产得到可以产生颜色的光学薄膜,并进而得到的对应颜料。
基于光学薄膜的颜料,目前没有一个统一的专业称呼,有称为光变颜料,也有称为光干涉变色颜料还有珠光颜料。对于这一类颜料,市场上根据颜料性能,分为两大类俗称:变色龙颜料和全向色颜料。简单来说,变色龙颜料在不同的角度观察时颜色各不相同,例如人民币100元纸币、美元100元纸币的“100”字样;而全向色颜料又称为不变色颜料,即在不同的角度观察时颜色接近,变化小。
基于光学薄膜颜料的原理与珍珠光泽的原理相似。牛顿的光学理论指出阳光是由许多颜色不同的光组成的。在日光下,非透明物质吸收或透过了某一波长的入射光,反射出来的另一波长的光便是该物体呈现的颜色。对于多层光学薄膜最终出来的反射光的颜色因膜层数、膜层的厚度、膜层的折射率等不同而异。其中,由于这些反射光和透射光都来自同一光波,入射光分解出的两束光的光程差不同,当它们满足相干光条件时,即可产生光的相干干涉而产生特定的颜色,此即为光学薄膜颜料的原理。
现有技术中,基于光学薄膜的颜料的制造方法,包括卷对卷的卷绕镀膜,或者在箱式镀膜机上多层叠加、中间间隔脱膜剂的牺牲层的办法。但是,卷绕镀膜的设备昂贵、生产效率低;而箱式镀膜机上多层叠加,中间间隔氯化钠脱膜剂作牺牲层的办法,生产过程中膜层不规则脱落、造成生产中断。
本申请一种颜料的制造方法即为基于光学薄膜的颜料的制造方法,由于牺牲层是具有低应力或压应力的脱膜剂,而多层光学薄膜的总应力是张应力,脱膜剂间隔其间,脱膜剂隔离、降低了光学薄膜张应力的传递和积累,导致多套薄膜的总应力减小,避免生产过程中膜层不规则脱落,通过这种方式,能够在不增加生产成本的基础上,避免生产过程中膜层不规则脱落,从而避免生产中断。
下面具体介绍本申请的内容:
参阅图1,图1是本申请一种颜料的制造方法一实施方式的流程示意图,该方法包括:
步骤S101:提供衬底。
衬底常常采用聚酯、涤纶、聚酰亚胺、玻璃或金属等材料。具体地,聚酯多采用聚对苯二甲酸乙二酯(PET),涤纶多采用聚氯乙烯((Polyvinyl chloride,PVC)。衬底的选择可依实际生产来确定。
步骤S102:在衬底上依次形成叠加的多套薄膜,每套薄膜包括依次叠加的牺牲层和光学薄膜层,其中,牺牲层是具有低应力或压应力的脱膜剂。
在本实施方式中,牺牲层是具有低应力或压应力的脱膜剂。压应力就是指抵抗物体有压缩趋势的应力。在具体的实际应用中,具有低应力或压应力的脱膜剂可以根据试验进行查找,或者根据经验初步确定后再通过试验验证。具体地,在本实施方式中,牺牲层可以是仅仅包括具有低应力的脱膜剂或压应力的脱膜剂,也可以是这些脱膜剂与其他脱膜材料的混合物,等等。进一步,脱膜剂的含量及厚度也是依具体的实际需要来确定,生产过程中试验两次即可确定。在一实施方式中,脱膜剂是通过蒸发镀膜之后在膜层中能产生压应力或低应力的可溶性物质。
其中,脱膜剂可以是无机盐、有机酸盐、碱基盐等中的至少一种。其中,所述无机盐具体可以是盐酸盐、硝酸盐、硫酸盐、磷酸盐、碳酸盐中的至少一种,有机酸盐具体可以是丙烯酸盐、醋酸盐、硬脂酸盐中的至少一种,所述碱基盐具体可以是NaOH、KOH及Ca(OH)
2等中的至少一种。
当然,脱膜剂还可以是其它通过蒸发镀膜之后在膜层中能产生压应力或低应力的可溶性物质,此处不做具体限定。
现有技术中,牺牲层的材料中不包含具有压应力的脱膜剂,例如,采用氯化钠作为脱膜剂的材料,由于镀膜过程中产生张应力积累,导致镀膜过程中膜层不规则脱落,造成生产中断,降低生产效率。本实施方式中,牺牲层是具有低应力或压应力的脱膜剂,而多层光学薄膜的总应力是张应力,脱膜剂间隔其间,脱膜剂隔离、部分抵消了光学薄膜张应力的传递和积累,导致多套薄膜的总应力减小,避免生产过程中膜层不规则脱落,通过这种方式,能够在不增加生产成本的基础上,避免生产过程中膜层不规则脱落,生产过程不中断,从而可以提高生产效率。
在一个应用场景中,光学薄膜层可以包括介质层、半导体层和金属层等中的至少一种。具体地,介质层可由氧化硅、氧化铝、氧化钛、氧化锆等形成,具体可采用电子束加热蒸发、磁控溅射蒸发、电阻加热蒸发等真空沉积方式形成;半导体层可以由硅、锗等采用电子束加热蒸发、电阻加热蒸发等的真空沉 积方式形成;金属层则可以采用银、铬、铜、镍、铝等通过电子束加热蒸发、电阻加热蒸发等真空沉积的方式形成。当然,光学薄膜层还可以包括其它层,此处不做具体限定。
具体地,参见图2,步骤S102可以包括:子步骤S1021、子步骤S1022、子步骤S1023以及子步骤S1024。
子步骤S1021:在衬底上蒸镀脱膜剂以形成一层牺牲层。
子步骤S1022:在蒸镀有牺牲层的衬底上镀制光学薄膜层,获得第一套薄膜。
具体地,在镀制光学薄膜层时,可以采用物理气相沉积(PVD)、化学气相沉积(CVD)、原子层沉积(ALD)等中的至少一种方法进行镀制。其中,采用物理气相沉积进行镀制时,具体可以采用电阻热蒸镀、电子束蒸镀、溅射及离子辅助蒸发等的至少一种方法进行。在实际操作过程中可根据实际需求进行选择,此处不做具体限定。
子步骤S1023:重复上述步骤,在第一套薄膜上叠加牺牲层和光学薄膜层,进而在第一套薄膜上叠加第二套薄膜。
子步骤S1024:重复上述步骤,反复叠加牺牲层和光学薄膜层,进而在衬底上依次形成叠加的多套薄膜。
例如,参见图3,图3是步骤S102在一实际应用中形成的叠加的多套薄膜的示意图,在该实际应用中,牺牲层2采用上述实施方式中的脱膜剂,薄膜的套数以50套为例。在衬底1上蒸镀一层牺牲层2,并进一步在蒸镀有牺牲层2的衬底1上镀制光学薄膜层3,获得第一套薄膜n1,其中,牺牲层2和光学薄膜层3均可采用真空镀膜机蒸镀而成;然后,重复上述步骤,在第一套薄膜n1上叠加牺牲层2和光学薄膜层3,进而在1第一套薄膜n1上叠加第二套薄膜n2,重复上述步骤,反复叠加牺牲层2和光学薄膜层3,进而在衬底上依次形成叠加的第50套薄膜n50。
将衬底放入镀膜机真空室内,蒸发沉积脱膜剂以形成牺牲层,在牺牲层上镀制光学薄膜层,牺牲层和光学薄膜层构成一套薄膜,然后反复叠加镀制多套 上述薄膜;由于薄膜的总应力是张应力,而脱膜剂间隔其间,该脱膜剂的压应力部分阻断、抵消张应力的传递、积累,导致多套薄膜的总应力减小,避免生产过程中膜层不规则脱落,可以沉积多达50套薄膜;而现有技术中,采用具有张应力的氯化钠牺牲层,由于总应力大,膜层不规则脱落,只能沉积10套左右薄膜。
由于脱膜剂具有压应力或低应力,可以使多套叠加的薄膜在镀膜过程中不脱落,生产过程不中断,因此可以不采用昂贵的设备,仅采用普通的真空镀膜机镀制多套叠加的薄膜,从而保证不增加生产成本。
进一步,步骤S102具体可以是采用箱式真空镀膜机在衬底上依次形成叠加的多套薄膜。
步骤S103:对形成后的多套薄膜分别进行脱膜处理和粉碎处理,得到颜料。
将镀制好的多套薄膜进行脱膜粉碎处理,例如放入装有有机溶剂丙酮或甲乙酮溶液或水的超声槽中,一般超声30分钟左右即可使薄膜碎化。
本申请实施方式提供衬底;在所述衬底上依次形成叠加的多套薄膜,每套所述薄膜包括依次叠加的牺牲层和光学薄膜层,其中,所述牺牲层是具有低应力或压应力的脱膜剂;对形成后的多套所述薄膜分别进行脱膜处理和粉碎处理,得到所述颜料。由于牺牲层是具有低应力或压应力的脱膜剂,薄膜的总应力是张应力,脱膜剂间隔其间,脱膜剂的压应力或低应力部分阻断薄膜张应力的传递,导致多套薄膜的总应力减小,避免生产过程中膜层不规则脱落,通过这种方式,能够在不增加生产成本的基础上,避免生产过程中膜层不规则脱落,从而避免生产中断。
光学薄膜是按膜系结构的要求,在高真空条件下把不同折射率的材料依次交替淀积在同一载体上形成。材料是以分子或原子的形式被蒸发到载体上,为保证膜层的均匀性和致密性,必须严格控制蒸发速率的一致性;而为了控制膜系的颜色指标,必须将膜层厚度的误差控制在埃的范围内。由此可见光学薄膜生产的精密性和特殊性。目前较理想的光学薄膜为对称式结构,膜系厚度在1 微米左右。由于膜系在高真空下制成,使用的全是无色或透明的无机材料,生成的光学薄膜颜料性能稳定、结构致密、不会褪色、耐候性极强、抗剪切性好、可按油墨对粒径的要求任意粉碎。
进一步,上述叠加形成的多套薄膜的套数可以是10-55套。
现有技术采用氯化钠作为牺牲层的材料,膜层不规则脱落:有时是叠加15套脱落,有时是叠加5套脱落,这样给光学薄膜的生产过程带来困扰,容易频繁且不规则的中断生产过程。本实施方式薄膜叠加的套数可以达到10-55套,甚至55套以上。
在一实施方式中,颜料呈片状。
进一步,在一应用中,颜料呈0.015~1微米厚、5~200微米长宽的薄片状。
需要说明的是,颜料的形状、粒径等依实际的应用场景或者印刷、喷涂方式等来确定。
其中,该方法还包括:预先确定牺牲层的厚度。
牺牲层的厚度可以根据经验来确定,需要确保可以分离薄膜,即使衬底与薄膜分离。
牺牲层的厚度也可以根据试验来确定。即,预先确定牺牲层的厚度,可以是:预先通过多次试验调整牺牲层的厚度,以在脱膜处理时牺牲层可以分离薄膜。一般来说,试验3次即可获得牺牲层的厚度。
其中,经过粉碎处理后,如果颜料不容易在油墨连接料中得到很好的分散,可以对制得的颜料进一步进行表面处理,即该方法还包括:对粉碎处理完毕后的颜料进行表面处理。
例如:一般的表面处理是将粉碎处理后的颜料投入到松香或硬脂酸(如:脱氢松香酸、四氢化松香酸等)的饱和溶液中,搅拌半小时以上,然后沉淀、过滤、烘干即可。将上述处理后的颜料均匀掺入透明的油墨连接料中,再加入适量的助溶剂和流变控制剂即可。常用的油墨连接料包括松香改性酚醛树脂、马来酸树脂和聚酰胺树脂等。助溶剂有助于组合物的稳定或使用,助溶剂包括 二醇醚、二醇醚乙酸酯等。在颜料中加入少量流变控制剂对改善油墨性能是必要的,流变控制剂包括水辉石黏土、烘制二氧化硅、膨润土黏土、纤维素类等等。需要说明的是,上述添加物质的加入比例以不影响油墨的光谱特征为限。
以上仅为本发明的实施方式,并非因此限制本发明的专利范围,凡是利用本发明说明书及附图内容所作的等效结构或等效流程变换,或直接或间接运用在其他相关的技术领域,均同理包括在本发明的专利保护范围内。
Claims (10)
- 一种颜料的制造方法,其特征在于,所述方法包括:提供衬底;在所述衬底上依次形成叠加的多套薄膜,每套所述薄膜包括依次叠加的牺牲层和光学薄膜层,其中,所述牺牲层是具有压应力或低应力的脱膜剂;对形成后的多套所述薄膜分别进行脱膜处理和粉碎处理,得到所述颜料。
- 根据权利要求1所述的方法,其特征在于,所述脱膜剂是通过蒸发镀膜之后在膜层中能产生压应力或低应力的可溶性物质。
- 根据权利要求2所述的方法,其特征在于,所述脱膜剂是无机盐、有机酸盐、碱基盐中的至少一种。
- 根据权利要求3所述的方法,其特征在于,所述无机盐为盐酸盐、硝酸盐、硫酸盐、磷酸盐、碳酸盐中的至少一种;所述有机酸盐为丙烯酸盐、醋酸盐、硬脂酸盐中的至少一种;所述碱基盐为NaOH、KOH、Ca(OH) 2中的至少一种。
- 根据权利要求1所述的方法,其特征在于,所述在所述衬底上依次形成叠加的多套薄膜,包括:在所述衬底上蒸镀脱膜剂以形成一层牺牲层;在蒸镀有所述牺牲层的衬底上镀制光学薄膜层,获得第一套所述薄膜;重复上述步骤,在第一套所述薄膜上叠加牺牲层和光学薄膜层,进而在所述第一套薄膜上叠加第二套薄膜。重复上述步骤,反复叠加牺牲层和光学薄膜层,进而在所述衬底上依次形成叠加的多套薄膜。
- 根据权利要求5所述的方法,其特征在于,所述在蒸镀有所述牺牲层的衬底上镀制光学薄膜层时,镀制所述光学薄膜层的方法包含物理气相沉积、化学气相沉积、原子层沉积中的至少一种。
- 根据权利要求6所述的方法,其特征在于,所述物理气相沉积为电阻热 蒸镀、电子束蒸镀、溅射及离子辅助蒸发中的至少一种。
- 根据权利要求5所述的方法,其特征在于,所述叠加的多套薄膜的套数是10-55套。
- 根据权利要求1所述的方法,其特征在于,所述光学薄膜层包括介质层、半导体层和金属层中的至少一种。
- 根据权利要求1所述的方法,其特征在于,所述方法还包括:预先通过多次试验调整所述牺牲层的厚度,以在脱膜处理时所述牺牲层可以分离所述薄膜。
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