KR20130000557A - A high chroma multilayer using sputtering method - Google Patents

Abstract

PURPOSE: A pigment with high chroma is provided to be used for a field which needs pigments to obtain discoloration accordingly to the angles and high chroma such as the interior and exterior of a vehicle. CONSTITUTION: A pigment with high chroma using a cross evaporation of a metal/dielectric body consists of a dielectric layer and a metal layer around a reflecting layer. The reflecting layer is an aluminum layer. The dielectric layer is a silicon dioxide layer. The metal layer is a chrome layer. The thickness of the reflecting layer, the dielectric layer, and the metal layer are 40-200 nm, 100-500 nm, and 3-20 nm, respectively. A metal material in the metal layer is aluminum, copper, or chrome. A dielectric material in the dielectric layer is alumina, magnesium fluoride, calcium fluoride, cryolite, or silicon dioxide.

Description

Pigment of high saturation using metal / dielectric cross deposition and its manufacturing method {A high chroma multilayer using sputtering method}

The present invention relates to a pigment of high saturation and a method for manufacturing the same, and more particularly, to a metal and a dielectric, which can be applied to a field requiring a pigment capable of realizing discoloration according to high saturation and angle of automobiles, interior and exterior materials, and the like. The present invention relates to a pigment of high saturation, which is cross-deposited using sputtering, and a method for producing the same.

Multi-color pigments or pearl pigments are used for wallpaper, flooring, plastic products, leather coatings, accessories, silk printing, toys, home appliances, ceramics, building materials, industrial products, cosmetics, food contact containers, automotive coatings, photocatalysts, and electromagnetic waves. It is a widely used material for shielding and preventing forgery and alteration of securities.

Such pigments are commonly known as pearlescent, iridescent and metallic pigments, and are mainly produced by hydrothermal synthesis, but are also produced by sputtering or CVD. Among the above methods, the hydrothermal synthesis method has a disadvantage in that the refractive index is low, the surface is not flat, and the particle size distribution is not uniform, so that the gloss is not excellent when coating metals and metal oxides. In addition, the sputtering method and the CVD method has a disadvantage in that the productivity is lower than other processes.

In order to manufacture such pigments more efficiently, many studies have been conducted. For example, in US Pat. Nos. 6,569,529 B1 and 6,991,860 B2, a multilayer that uses Ti2 as a reflector and a high refractive material and SiO2 as a low refractive material is used. An interference pigment is disclosed, and Korean Patent Laid-Open Publication No. 2006-105922 discloses a metallic pearl pigment and a method of manufacturing the same. However, the conventional technologies have problems in terms of process efficiency and colors in terms of viewing angle.

In Korean Patent No. 10-0853693, to which the present applicant is co-owner in order to solve the above problems, a multi-colored pearl pigment having a low refractive index material and a high refractive index material made of an interlayer with a metal layer as a reflective layer and a method of manufacturing the same In another patent application No. 10-0959790, which is the co-owner of the present application, a multi-color pearl pigment using a high refractive index material different from that of the patent No. 10-0853693 and a method of manufacturing the same are disclosed.

However, the patents are thin film deposition by a vacuum deposition method, which is suitable for the above patents, but has a problem in depositing materials to be used in the present invention.

In addition, the present invention relates to the production of pigments using aluminum or chromium, which is a material to be used in the present invention, but US Patent No. 5,569,535 A and Korean Patent Publication No. 10-2000-0065051, the prior art is chromium (Cr) and fluoride Since magnesium (MgF 2) is used, it is difficult to use the sputtering method in the case of the magnesium fluoride, and thus there is a problem that the manufacturing equipment has to be complicated, such as having to equip and equip an electron beam deposition apparatus, a resistive heating deposition apparatus, and the like. This is also shown in the drawings of Korean Patent Publication No. 10-2000-0065051, vacuum chamber, distribution roller, polyester stream, rotating drum, container roller, roller, tension roller, metallization station, high speed vaporizer, second metallization station, irradiation station. It can also confirm with what is provided.

The present invention solves the problems of the prior art as described above, and a pigment of high saturation, which is a multilayer interference pigment composed of a dielectric layer and a metal layer, based on a reflective layer made of a metal layer having excellent reflectance using sputtering vacuum deposition, which is an economical method, and a method of manufacturing the same. The purpose is to provide.

 The present invention to achieve the above object of the present invention;

As a pigment of high saturation using metal / dielectric cross deposition, a pigment of high saturation composed of a dielectric layer and a metal layer with respect to a reflective layer is provided.

In the above, the reflective layer is an aluminum (Al) layer, the dielectric layer is a silicon dioxide (SiO₂) layer, the metal layer is preferably a chromium (Cr) layer, the thickness of each layer is 40 ~ 200nm reflective layer, 100 ~ 500nm dielectric layer The metal layer is preferably 3 to 20 nm.

The invention also;

Applying a release layer comprising a water- or solvent-soluble material to the substrate (S1);

Depositing a metal layer, a dielectric layer, and a reflective layer on the layer (S2);

Here, the outermost metal layer is deposited first, followed by the deposition of the dielectric layer, the reflective layer, the dielectric layer, and the metal layer in order, and adjusts the number of layers as necessary. At this time, the metal layer should be located at the outermost layer, the reflective layer and the dielectric layer should be adjacent to each other, and the reflective layer is formed in the middle of the dielectric layer and the metal layer, that is, the dielectric layer and the metal layer centered on the reflective layer.

Removing the formed layer system from the substrate by dissolving the release layer, and washing and drying the resultant plate-shaped interference pigment (S3); And

It provides a high-saturation pigment production method consisting of the step (S4) of obtaining a pigment by grinding and classifying the pigment.

The multi-color pigments produced by the present invention are used in wallpaper, flooring, plastic products, leather coatings, accessories, silk printing, toys, home appliances, ceramics, building materials, etc., but also for automotive coatings, electromagnetic shielding, and securities.・ It can be widely used for preventing tampering.

1 is a schematic diagram of a deposition equipment for producing a conventional pigment.
2 is a schematic diagram of a vacuum deposition equipment for the production of a multilayer interference film according to the present invention.
Figure 3 is a SiO₂ 120nm thick color system and blue-silver color is implemented.
Figure 4 is a SiO 2 265nm thick color system and violet-red-orange color is implemented.
FIG. 5 is a colorimeter with a thickness of SiO 2 300 nm, and a blue-red color is implemented.
Figure 6 is a SiO 2 340nm thick color system, green-blue color is implemented.
Figure 7 is a SiO 2 390nm thick color system and implements gold-green-blue color.
Figure 8 is a SiO 420nm thick colorimeter and red-orange-gold-green-blue color is implemented.
FIG. 9 is a 450 nm thick SiO 2 color and violet-red-orange-gold-green color scheme.
FIG. 10 is a colorimeter with a thickness of SiO 2 500 nm and a blue-violet-red color is implemented.
11 schematically shows the position of the eye according to the angle indicated in the colorimeter.

Hereinafter, the present invention will be described in detail with reference to the accompanying drawings.

As the metal material of the metal layer used for the outermost layer in the present invention, most metals such as aluminum (Al), copper (Cu), and chromium (Cr) may be used, but chromium (Cr) having excellent weather resistance is most preferable. The stable deposition thickness is in the range of about 3 to 20 nm, and when the deposition is more than 20 nm, the final pigment saturation decreases rapidly, and the most preferable deposition thickness is 5 nm.

Titanium dioxide (TiO₂), alumina (Al₂O₃), magnesium fluoride (MgF₂), calcium fluoride (CaF₂), cryolite, silicon dioxide (SiO₂), etc. can be used as dielectric materials. Most preferred is silicon dioxide (refractive index: about 1.45), which is a low refractive index material and a dielectric material capable of sputtering in the form of an oxide. Deposition thickness is determined by the design of the color to be implemented, preferably in the range of about 100-500 nm. The reason is that the thickness of chromaticity and saturation finalized according to the thickness of the silicon dioxide, the dielectric layer, is fixed after fixing the deposition thickness of the outermost layer to about 5 nm (ㅁ 1 nm) and the reflective layer aluminum to about 70 nm (ㅁ 10 nm). Will change. 3 to 10 show relevant color difference values.

In addition, the reflective layer is a metal, and most metals having high reflectivity such as silver (Ag), aluminum (Al), copper (Cu) can be applied, but aluminum is most preferable in consideration of stability and economical efficiency. Aluminum, which is used as a reflective layer, exhibits a translucent property up to about 40 nm, but opaque and high reflectance above. This is a property of opaque and highly reflective bulk aluminum because it shows a value of (0.73, -5.64i) at about 40 nm in complex admittance coordinates and is closer to (0.7, -5.66i), which is the admittance of bulk aluminum. Will have Therefore, aluminum is deposited in the range of 40 nm to 200 nm. In consideration of the strength of the reflective layer, about 70 nm is preferable.

The sputtering deposition apparatus of the present invention is schematically illustrated in FIG. 2 and the roll-shaped film mounted is wound, unrolled and deposited in both directions by rollers 2 and 4 on both sides. The film is deposited in one direction and the desired material is deposited. When the deposition is complete, the film is rewound in the opposite direction and the next material is deposited. This has the advantage of depositing one material at an optimal condition compared to depositing several materials at one time because the conditions for depositing different materials.

[Example]

To use the Tape casting the roll film Uz is applied to a nitro cellulose Roll to Roll Puls by using magnetron sputtering equipment subjected to five layers deposited in a table following conditions chromium (Cr), about 7nm, silicon dioxide (SiO ₂₎ of about 265nm , A multi-layered film of about 70nm of aluminum (Al) was obtained, and a pigment was prepared to realize a violet-red-orange multicolor through pulverization after removing a release layer using acetone.

Table 1

Claims (3)

As a pigment of high saturation using metal / dielectric cross deposition,
A pigment with high saturation, characterized by consisting of a dielectric layer and a metal layer around a reflective layer. The pigment of claim 1, wherein the reflective layer is an aluminum layer, the dielectric layer is a silicon dioxide layer, and the metal layer is a chromium layer. 3. The pigment of claim 2, wherein the reflective layer is 40-200 nm thick, the dielectric layer is 100-500 nm thick, and the metal layer is 3-20 nm.

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