KR102183063B1 - Gradation film and preparation method thereof - Google Patents

Abstract

The present invention relates to a gradation film and a method of manufacturing the same, wherein the gradation film may be formed by a roll-to-roll sputtering process to form a single layer or a multi-layered inorganic material deposition layer on one surface of a base film. In addition, when the inorganic material deposition layer is formed, an inorganic material deposition layer having a different composition (component ratio) can be formed because the degree of oxidation of the inorganic material is changed by appropriately controlling the opening and closing area of the injection port through which oxygen gas is injected. The inorganic deposition layer has different colors, but the color variation is small, so it is possible to implement a gradation color. Accordingly, the gradation film can be applied to various fields such as displays, automobiles, and home appliances to improve the aesthetics of the exterior.

Description

Gradation film and its manufacturing method {GRADATION FILM AND PREPARATION METHOD THEREOF}

The present invention relates to a gradient film and a method of manufacturing the same.

The technology in the electric and electronic communication field is changing day by day, and accordingly, electronic products of various designs are being released. In such an electronic product, the case and/or decoration film (hereinafter, referred to as “deco film”) constituting the exterior needs to satisfy designs such as color, pattern, and gloss in consideration of the user's aesthetic as well as its natural protection function.

In the past, most of the deco films that implement only one color have been used, but as the demand for implementing various colors has increased recently, an example of applying a gradation method to a deco film has been introduced (Korean Patent Publication No. 2018-0109360). However, the decor film disclosed in the patent includes a multi-layered gradation layer including a plurality of gradation layers exhibiting different gradation effects, and a color layer must be formed for each of the gradation layers. It is manufactured by separately forming a light reflective layer including, and has a disadvantage in that it not only has a complex structure, but also a process is not simple.

Korean Patent Application Publication No. 2018-0109360

Accordingly, an object of the present invention is to provide a gradation film capable of implementing various colors, and a method of manufacturing the gradation film more simply using a continuous roll-to-roll process.

In order to achieve the above object, in the present invention, in continuously forming an inorganic material deposition layer on one side of the base film by roll-to-roll sputtering a raw material target to the base film,

It provides a method of manufacturing a gradient film in which the composition of the inorganic material deposition layer is varied in the width direction of the base film.

In order to achieve the above other object, the present invention is prepared by the above manufacturing method, (a) a base film and (b) formed on one side of the base film and laminated with an inorganic deposition layer having a different composition in the width direction of the base film. It provides a gradient film, including in the form.

According to the manufacturing method of the gradation film of the present invention, it is possible to form a single layer or a multi-layered inorganic material deposition layer on one surface of a base film by a roll-to-roll sputtering process. In addition, when the inorganic material deposition layer is formed, an inorganic material deposition layer having a different composition (component ratio) can be formed because the degree of oxidation of the inorganic material is changed by appropriately controlling the opening and closing area of the injection port through which oxygen gas is injected. The inorganic deposition layer has different colors, but the color variation is small, so it is possible to implement a gradation color. Accordingly, the gradation film can be applied to various fields such as displays, automobiles, and home appliances to improve the aesthetics of the exterior.

1 is a schematic diagram of a gradient film according to an embodiment of the present invention.
2 is a schematic diagram of a sputtering process for manufacturing a gradation film according to an embodiment of the present invention, showing positions of a base film 300, a raw material target 400, and an oxygen gas inlet block 500.
3 is a schematic diagram showing the degree of opening and closing of the oxygen gas inlet 600 during sputtering, showing a state in which the oxygen gas inlet is fully open 610, a semi-open state 620, and a fully closed state 630.

The present invention is not limited to the contents disclosed below, and may be modified in various forms unless the gist of the invention is changed.

In the present specification, "including" means that other components may be further included unless otherwise specified. In addition, all numbers and expressions representing amounts of components, reaction conditions, and the like described in the present specification are to be understood as being modified by the term "about" in all cases unless otherwise specified.

Manufacturing method

The present invention provides a method for producing a gradient film in which the composition of the inorganic material deposition layer is changed in the width direction of the base film in successively forming an inorganic material deposition layer on one side of the base film by roll-to-roll sputtering a raw material target for a base film. to provide.

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

According to the manufacturing method, oxygen gas is injected into the raw material target 400 during the sputtering, but by varying the amount of oxygen gas in the width direction of the base film 300, the composition of the inorganic material deposition layer is changed to the base film. You can do it differently in the width direction.

Specifically, by gradually increasing or decreasing the amount of oxygen gas in the width direction of the base film 300, the weight ratio of oxygen in the inorganic material deposition layer may be gradually increased or decreased.

More specifically, referring to FIGS. 2 and 3, a plurality of 　 oxygen gas injection ports 　 are located in the width direction of the base film 300 near the raw material target 400, but the opening and closing areas of the oxygen gas injection ports may be different. For example, some of the plurality of oxygen gas inlets may be fully open, some may be half open, and some may be fully closed (see FIG. 3).

Oxygen gas may be injected into the raw material target 400 in an amount of 5 to 20 sccm, or 10 to 15 sccm. In this case, the amount of the oxygen gas may vary depending on the opening and closing area of the injection port, the injection time, and the rate at which oxygen gas is injected from the injection port.

As oxygen gas is injected into the raw material target 400 together, the inorganic material is oxidized during sputtering and may be deposited on the base film 300 in an oxide state such as NbO, NbO ₂ , SiO, SiO ₂ , InO, etc. .

The base film 300 is polypropylene (PP), polyethylene (PE), polystyrene (PS), acrylonitrile-butadiene-styrene copolymer (ABS), polycarbonate (PC), polyoxymethylene (POM), Polyamide (PA), polypropylene oxide (PPO), polybutylene terephthalate (PBT), polyethylene terephthalate (PET), polyvinyl chloride (PVC), polymethyl methacrylate (PMMA), polytetrafluoroethylene (PTFE), polyetheretherketone (PEEK), polyphenylene sulfide (PPS), polyimide (PI), polyamide-imide (PAI), and polyethyleneimide (PEI). Can be, specifically, it may be a PET material.

The raw material target 400 may include various inorganic materials, and specifically, may be at least one selected from the group consisting of niobium (Nb), silicon (Si), and indium (In).

The sputtering is, 5 x 10 ^{- 10} torr to about 5 x 10 ^-1 torr and then under a vacuum injection of an inert gas such as argon (Ar), helium (He) to said target material (400), from 5 to 50 KW, Alternatively, it may be performed by applying a voltage of 5 to 30 KW. Under the above conditions, each of the raw materials may be continuously sputtered from the raw material target 400 to one surface of the base film 300 by sputtering to be deposited.

The inorganic deposition layer may be formed as a single layer on one surface of the base film 300, or may be formed as a multilayer by repeatedly performing sputtering by sequentially arranging the raw material targets 400. Alternatively, an inorganic material layer or an inorganic material oxide layer having the same component may be formed by sputtering without applying a mask to the raw material target 400, and then an inorganic material deposited layer may be formed.

The inorganic material deposition layer may be formed more easily and quickly on one surface of the base film 300 by such a continuous roll-to-roll process. In addition, it is possible to form various inorganic material deposition layers having a desired color by simply changing the opening/closing area of the raw material target 400 and the oxygen gas injection port 600.

If necessary, prior to the formation of the inorganic material deposition layer, a metal layer without a component gradient or a metal oxide layer may be formed on one side of the base film 300 through a roll-to-roll sputtering process, and after the formation of the inorganic material deposition layer It can also be formed on the other side of the inorganic material deposition layer.

The manufacturing method of the gradation film may further include the step of forming the shielding layer 100. Since the shielding layer 100 can also be continuously performed by a roll-to-roll process, the process time and workability are not reduced. . The shielding layer 100 may include a material commonly used for shielding purposes, and may have a thickness in a typical range.

gradation film

The present invention is prepared by the method as described above, and includes (a) a base film and (b) an inorganic deposition layer formed on one side of the base film and having a different composition in the width direction of the base film in a laminated form, Provide a film.

The base film (a) serves as a support in the gradation film, and specific types are as listed above. The base film (a) is not limited as long as it can be used in a roll-to-roll process, and may specifically be a film wound in a roll form. The base film (a) may have a thickness of 20 to 100 μm, or 30 to 80 μm.

The gradation film may include a single layer or a multilayer inorganic material deposition layer (b) on one surface of the base film (a). In this case, the inorganic material deposition layer (b) may have a different composition in the width direction of the base film (a) by a roll-to-roll sputtering process as described above.

The inorganic material deposition layer (b) may have a thickness of 50 to 400 nm, 50 to 300 nm, 100 to 300 nm, or 150 to 300 nm.

As described above, the inorganic material deposition layer (b) may include an inorganic material, an inorganic material oxide, or both.

The inorganic material deposition layer (b) may provide various colors by controlling brightness and/or saturation in various ways, as well as provide a gradation effect with little color deviation (see Evaluation Example).

The gradient film may include one or more layers of a metal layer, a metal oxide layer, or both between the base film (a) and the inorganic material deposition layer (b). Alternatively, when the inorganic material deposition layer (b) is included in multiple layers, the metal layer, the metal oxide layer, or both may be included between the plurality of inorganic material deposition layers.

The gradation film may further include a shielding layer on the other surface of the inorganic material deposition layer. The shielding layer may include, without limitation, colored pigments or dyes having a shielding effect at the color or wavelength to be blocked.

For example, according to FIG. 1, in the gradation film, a metal layer or metal oxide layer 220, 230, 240, and an inorganic material deposition layer 210 are sequentially stacked on one surface of the base film 300, and then a shielding layer ( 100) may be additionally stacked.

As described above, according to the method of manufacturing a gradation film of the present invention, it is possible to form a single layer or a multi-layer inorganic deposition layer on one surface of the base film by a roll-to-roll sputtering process. In addition, when the inorganic material deposition layer is formed, since the degree of oxidation of the inorganic material is changed by appropriately controlling the opening and closing area of the injection port through which oxygen gas is injected, an inorganic material deposition layer having different component ratios can be formed. Have different colors, but there is little color deviation, so it is possible to implement a gradation color. Accordingly, the gradation film can be applied to various fields such as displays, automobiles, and home appliances to improve the aesthetics of the exterior.

The above will be described in more detail by the following examples. However, the following examples are for illustrative purposes only, and the scope of the examples is not limited thereto.

Example : gradation Production of film

A polyethylene terephthalate (PET) film (50 μm, U483, Toray) was prepared as a base film.

As a raw material target, a niobium target 5, an indium target 4, a niobium target 3, a silicon target 2, and a niobium target 1 were prepared and sequentially arranged. At the time of sputtering from the last niobium target 1, the degree of opening and closing of the oxygen gas injection port was adjusted to be full open, half open, and full closed (see FIG. 3).

After the base film was introduced into a roll-to-roll machine, it was pumped for 3 hours, and when the degree of vacuum reached 5 x 10 ^-6 torr, a total of 3,000 sccm was added by 600 sccm of argon (Ar) to each of the raw material targets. Then, film running was started, and as shown in Table 1 below, oxygen was added while voltage was applied to adjust the thickness of each to form a deposition layer to prepare a gradient film.

Raw material target Voltage(KW) Oxygen amount (sccm) Thickness (nm) Middle layer One Niobium 26 14 61 NbO _x (0≤x≤1) 2 silicon 8 10 9 SiO 3 Niobium 16 14 39 NbO 4 indium 5 0 30 In 5 Niobium 15 13 30 NbO

Evaluation example : Color coordinates evaluation

For the gradation film prepared in the above example, the reflected light of the inorganic material deposition layer was measured using the CM3600D model of Konica Minolta, and the result was expressed in color coordinates.

Nozzle opening and closing degree
Outermost inorganic material vapor deposition layer
(NbO _x layer) composition Color coordinates L* a* b* Condition 1 Closed Nb 63 -One 22 Condition 2 Half closed NbO _{0 .5} 56 8 10 Condition 3 Open NbO 49 17 -2

Looking at the results of Table 2, L* (brightness-related constant) showed a deviation within 15, indicating some difference in brightness, and a*(+red/green-) and b*(+yellow/blue-) indicating color values. ) Values represent relatively large deviations of 18 and 24, respectively, indicating both red and green, yellow and blue colors, so it can be seen that various colors are implemented.

100: shielding layer
210: inorganic material deposition layer
220, 230, 240: metal layer or metal oxide layer
300: base film
400: raw material target
500: oxygen gas inlet block
600: oxygen gas inlet
610: full open, 620: half open, 630: full closed

Claims (13)

In successively forming an inorganic material deposition layer on one side of the base film by roll-to-roll sputtering of the raw material target to the base film,
During the sputtering, oxygen gas is injected into the raw material target, and a plurality of oxygen gas injection ports are positioned near the raw material target in the width direction of the base film, and the amount of oxygen gas is determined by varying the opening and closing areas of the oxygen gas injection ports. By variously changing in the width direction of, the composition of the inorganic material deposition layer is changed in the width direction of the base film. delete The method of claim 1,
By gradually increasing or decreasing the amount of the oxygen gas in the width direction of the base film, the weight ratio of oxygen in the inorganic material deposition layer is gradually increased or decreased. The method of claim 1,
Injecting the oxygen gas into the raw material target in an amount of 5 to 20 sccm, a method for producing a gradient film. delete The method of claim 1,
The base film is polypropylene (PP), polyethylene (PE), polystyrene (PS), acrylonitrile-butadiene-styrene copolymer (ABS), polycarbonate (PC), polyoxymethylene (POM), polyamide ( PA), polypropylene oxide (PPO), polybutylene terephthalate (PBT), polyethylene terephthalate (PET), polyvinyl chloride (PVC), polymethyl methacrylate (PMMA), polytetrafluoroethylene (PTFE) , Polyetheretherketone (PEEK), polyphenylene sulfide (PPS), polyimide (PI), polyamide-imide (PAI) and polyethyleneimide (PEI) containing at least one selected from the group consisting of, gradient Method of making a film. The method of claim 1,
The raw material target is at least one selected from the group consisting of niobium (Nb), silicon (Si) and indium (In), a method for producing a gradient film. The method of claim 1,
The sputtering is performed by injecting an inert gas into the raw material target under vacuum and then applying a voltage of 5 to 30 KW to produce a gradient film. The method of claim 1,
A method for producing a gradient film, in which the inorganic material deposited layer is formed as a single layer or multiple layers. A gradation film prepared by the manufacturing method of claim 1 and comprising (a) a base film and (b) an inorganic deposition layer formed on one side of the base film and having a different composition in the width direction of the base film in a laminated form. The method of claim 10,
The gradient film comprises at least one layer of a metal layer, a metal oxide layer, or both between the base film and the inorganic material deposition layer. The method of claim 10,
The inorganic material deposited layer has a thickness of 50 to 400 nm, a gradient film. The method of claim 10,
The gradient film further includes a shielding layer on the other surface of the inorganic material deposition layer.

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