KR100849620B1 - Pigment dispersed solution - Google Patents
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- KR100849620B1 KR100849620B1 KR1020060113117A KR20060113117A KR100849620B1 KR 100849620 B1 KR100849620 B1 KR 100849620B1 KR 1020060113117 A KR1020060113117 A KR 1020060113117A KR 20060113117 A KR20060113117 A KR 20060113117A KR 100849620 B1 KR100849620 B1 KR 100849620B1
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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
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0071—Process features in the making of dyestuff preparations; Dehydrating agents; Dispersing agents; Dustfree compositions
- C09B67/0084—Dispersions of dyes
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/006—Preparation of organic pigments
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- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/0005—Production of optical devices or components in so far as characterised by the lithographic processes or materials used therefor
- G03F7/0007—Filters, e.g. additive colour filters; Components for display devices
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Abstract
색, 휘도, 콘트라스트비와 같은 광학특성과 입자크기, 점도 및 분산안정성과 같은 물리적 성질이 향상되는 안료분산액이 제공된다. 본 발명에 따른 안료분산액은 유기안료, 분산제, 및 유기용제를 포함하는 안료분산액에 있어서, 유기용제는 적어도 2종 이상이 사용되며 분산제의 종류에 종속하여 사용되는 것을 특징으로 한다.There is provided a pigment dispersion which improves optical properties such as color, brightness, contrast ratio and physical properties such as particle size, viscosity and dispersion stability. The pigment dispersion according to the present invention is a pigment dispersion comprising an organic pigment, a dispersant, and an organic solvent, characterized in that at least two or more organic solvents are used depending on the type of dispersant.
컬러필터, 안료분산액, 유기용제, 분산제 Color filter, pigment dispersion, organic solvent, dispersant
Description
도 1은 실시예와 비교예의 색감도를 비교한 도면이다.1 is a view comparing the color sensitivity of the Example and Comparative Example.
도 2는 실시예와 비교예의 휘도를 비교한 도면이다.2 is a view comparing the luminance of the Examples and Comparative Examples.
본 발명은 안료분산액에 관한 것으로서, 보다 상세하게는 휘도 및 콘트라스트비를 향상시킬 수 있는 액정표시장치 컬러필터용 안료분산액에 관한 것이다.The present invention relates to a pigment dispersion, and more particularly, to a pigment dispersion for a liquid crystal display device color filter that can improve the brightness and contrast ratio.
박막 트랜지스터 액정표시장치(TFT-LCD)는 두장의 유리기판 사이에 주입되어 있는 액정의 스위칭 작용에 의해 하부에서 발생되는 빛의 투과율을 조절함으로써 영상정보를 표시하는 장치로서 상부기판에는 RGB 세 가지 색이 각각 서브픽셀을 이루며 각종 컬러를 표시해 주기 위한 컬러필터라는 부재가 사용된다.TFT-LCD is a device that displays image information by controlling the transmittance of light generated at the bottom by the switching action of liquid crystal injected between two glass substrates. Each member forms a subpixel, and a member called a color filter for displaying various colors is used.
컬러필터는 일반적으로 안료(pigment)와 분산제(disperse agent), 및 유기용제를 혼합한 액상형태의 안료분산액을 코팅하는 방식으로 제조되는데, 이러한 안료분산액에 요구되는 물성으로는 분산안정성, 색감, 휘도, 콘트라스트비 및 내구성 등이 있다.A color filter is generally manufactured by coating a pigment dispersion in a liquid form in which a pigment, a disperse agent, and an organic solvent are mixed. The physical properties required for the pigment dispersion include dispersion stability, color, and luminance. , Contrast ratio and durability.
안료분산액이 상기 물성을 만족시키기 위해서는 사용되는 유기안료의 입자크기가 일정하여야 하고, 일반적으로 사용되는 고분자 분산제 또한 사용되는 각 안료의 표면특성에 적합한 분산제를 사용하여야 한다.In order for the pigment dispersion to satisfy the above physical properties, the particle size of the organic pigment used must be constant, and a polymer dispersant generally used must also use a dispersant suitable for the surface properties of each pigment used.
종래의 안료분산액을 제조하는 기술은 페인트나 잉크처럼 바인더 수지를 혼합하여 사용하는데, 이와 같은 제조방법에 의하면 상용성이나 안정성에서 컬러필터의 제조시 사용되는 포토레지스터와 문제(trouble)를 일으킬 수 있고, 특히 단일 유기용제를 사용할 경우 분산제의 역할을 제대로 수행하지 못하여 색과 휘도 특성이나 입자의 크기 및 점도, 분산안정성에 좋지 못한 영향을 미칠 우려가 있다.Conventional techniques for preparing pigment dispersions are used by mixing binder resins like paints and inks, which can lead to problems with photoresists used in the manufacture of color filters in terms of compatibility and stability. In particular, in the case of using a single organic solvent, the dispersant may not function properly, which may adversely affect color and luminance characteristics, particle size and viscosity, and dispersion stability.
본 발명이 이루고자 하는 기술적 과제는 종래의 단순한 배합설계를 최적화 시키고 기존의 페인트나 잉크처럼 바인더 수지를 사용하지 않고 유기용제를 최적화 함으로써 색, 휘도, 콘트라스트비와 같은 광학특성과 입자크기, 점도 및 분산안정성과 같은 물리적 성질이 향상되는 안료분산액을 제공하는데에 있다.The technical problem to be achieved by the present invention is to optimize the conventional simple compounding design and to optimize the organic solvent without using a binder resin like conventional paint or ink, optical properties such as color, brightness, contrast ratio and particle size, viscosity and dispersion It is to provide a pigment dispersion in which physical properties such as stability are improved.
본 발명이 이루고자 하는 기술적 과제들은 이상에서 언급한 기술적 과제로 제한되지 않으며, 언급되지 않은 또 다른 기술적 과제들은 아래의 기재로부터 당업자에게 명확하게 이해될 수 있을 것이다.Technical problems to be achieved by the present invention are not limited to the above-mentioned technical problems, and other technical problems not mentioned will be clearly understood by those skilled in the art from the following description.
상기의 기술적 과제를 해결하기 위한 본 발명의 실시예에 따른 안료분산액은 유기안료, 분산제 및 유기용제를 포함하는 안료분산액에 있어서, 유기용제는 적어도 2종 이상이 사용되며 분산제의 종류에 종속하여 사용되는 것을 특징으로 한다.
여기서, 분산제의 종류에 종속하여 사용되는 분산제-유기용제의 조합을 분산액이라 하고, 본 발명에 따른 특정 분산액에 유기안료를 혼합하여 안료분산액을 제조하는 것을 특징으로 한다.In the pigment dispersion according to an embodiment of the present invention for solving the above technical problem, in the pigment dispersion comprising an organic pigment, a dispersant and an organic solvent, at least two or more organic solvents are used depending on the type of dispersant It is characterized by.
Here, the combination of the dispersant-organic solvent used depending on the type of dispersant is called a dispersion, and the pigment dispersion is prepared by mixing an organic pigment with a specific dispersion according to the present invention.
기타 실시예들의 구체적인 사항들은 상세한 설명 및 첨부 도면들에 포함되어 있다.Specific details of other embodiments are included in the detailed description and the accompanying drawings.
본 발명의 이점 및 특징, 그리고 그것들을 달성하는 방법은 첨부되는 도면과 함께 상세하게 후술되어 있는 실시예들을 참조하면 명확해질 것이다. 그러나, 본 발명은 이하에서 개시되는 실시예들에 한정되는 것이 아니라 서로 다른 다양한 형태로 구현될 것이며, 단지 본 실시예들은 본 발명의 개시가 완전하도록 하며, 본 발명이 속하는 기술분야에서 통상의 지식을 가진 자에게 발명의 범주를 완전하게 알려주기 위해 제공되는 것이며, 본 발명은 청구항의 범주에 의해 정의될 뿐이다. Advantages and features of the present invention and methods for achieving them will be apparent with reference to the embodiments described below in detail with the accompanying drawings. However, the present invention is not limited to the embodiments disclosed below, but may be implemented in various different forms, only the present embodiments to make the disclosure of the present invention complete, and common knowledge in the art to which the present invention pertains. It is provided to fully inform the person having the scope of the invention, which is defined only by the scope of the claims.
본 발명에 따른 컬러필터용 안료분산액은 유기안료가 분산제와 유기용제에 분산되어 있다.In the pigment dispersion for color filters according to the present invention, an organic pigment is dispersed in a dispersant and an organic solvent.
유기안료로는 C.I.Pigment RED 254, C.I.Pigment YELLOW 139 등의 안료가 사용되며, 컬러필터에 적합한 색을 조정하기 위해서는 상기 안료들을 단독으로 혹은 혼합하여 사용할 수 있다.As organic pigments, pigments such as C.I. Pigment RED 254 and C.I.Pigment YELLOW 139 may be used. In order to adjust colors suitable for color filters, the pigments may be used alone or in combination.
분산제로는 대표적으로 폴리에스터계분산제, 폴리아크릴레이트계 분산제, 폴리우레탄계 분산제 등이 사용되며 전체 안료분산액 100중량부에 대하여 5 내지 80 중량부의 양이 사용된다.As a dispersant, a polyester-based dispersant, a polyacrylate-based dispersant, a polyurethane-based dispersant and the like are typically used, and an amount of 5 to 80 parts by weight is used based on 100 parts by weight of the total pigment dispersion.
본 발명의 안료분산액에 사용되는 유기용제(solvent)는 상기의 분산제로 무엇을 사용했느냐에 따라 결정되며, 프로필렌글리콜모노메틸에테르아세테이트, 프로필렌글리콜모노메틸에테르, 프로필렌글리콜모노에틸에테르아세테이트, 프로필렌글리콜모노에틸에테르, 에톡시프로피온산, 자일렌, 톨루엔, 부틸아세테이트, 사이클로헥사논, 2-부톡시에탄올 및 부탄올 중에서 2종 이상 선택되어 사용되어야 한다.The organic solvent used in the pigment dispersion of the present invention is determined by what is used as the dispersant, and propylene glycol monomethyl ether acetate, propylene glycol monomethyl ether, propylene glycol monoethyl ether acetate, propylene glycol monoethyl At least two selected from ether, ethoxypropionic acid, xylene, toluene, butyl acetate, cyclohexanone, 2-butoxyethanol and butanol should be used.
예컨대, 분산제를 Disperbyk-163(BYK Chemie 사)를 사용할 경우엔 유기용제로는 자일렌, 부틸아세테이트, 프로필렌글리콜모노에테르아세테이트를 혼합하여 제조한 분산액을 사용하는 것이 바람직하다.For example, when using Disperbyk-163 (BYK Chemie Co., Ltd.) as the dispersant, it is preferable to use a dispersion prepared by mixing xylene, butyl acetate, and propylene glycol monoether acetate.
이때, 사용되는 Disperbyk-163은 Disperbyk-162 보다 작은 분자량과 낮은 극성을 갖고 있으며 일반 공업용 도료 및 고농도 착색제에 우선적으로 이용할 수 있다. 또한, Disperbyk-161 , Disperbyk-162 보다 다양한 수지와의 상용성을 가지며, Disperbyk-163은 방향족 용제를 포함하지 않는 제품으로 Disperbyk-167 을 이용할 수 있다.In this case, the used Disperbyk-163 has a lower molecular weight and lower polarity than the Disperbyk-162, and can be preferentially used for general industrial paints and high concentration colorants. In addition, Disperbyk-161, Disperbyk-162 has a compatibility with a variety of resins, Disperbyk-163 can be used Disperbyk-167 as a product that does not contain an aromatic solvent.
이때 주의할 점은 Disperbyk-163과 같은 습윤분산제는 합성수지와 용제를 먼저 혼합한 후 교반하면서 첨가제를 서서히 혼합해야만 한다. 또한, 안료는 첨가제가 적절히 혼합된 후 넣어야 한다.At this time, it should be noted that the wet dispersant such as Disperbyk-163 should be mixed with the resin and the solvent first, and then slowly mixed with the additives while stirring. In addition, the pigment should be added after the additives are properly mixed.
Disperbyk-163 은 첨가중에 Seed 형성을 막기 위하여 수지와 혼합하기 전에 사용 용제로 15%(고형분) 용액으로 희석하여야 하며, 도료 제조 후 발견된 색분리의 교정을 위해서는 Disperbyk-163의 사용량이 적당하며 반드시 고속으로 교반하면서 서서히 첨가하여야 한다.Disperbyk-163 should be diluted with 15% (solid) solution with the solvent used before mixing with the resin to prevent Seed formation during the addition. The use of Disperbyk-163 is appropriate for the correction of color separation found after paint preparation. It should be added slowly while stirring at high speed.
또 다른 분산제를 예를들면 Disperbyk-2001(BYK Chemie 사)를 사용하는 경우 유기용제로 2-부톡시에탄올과 프로필렌글리콜모노메틸에테르아세테이트를 혼합하여 제조한 분산액을 사용하고, EFKA-4046(EFKA 사)를 사용하는 경우 유기용제로 부틸아세테이트와 프로필렌글리콜모노메틸에테르아세테이트를 혼합하여 제조한 분산액을 사용하는 것이 바람직하다. Another dispersant is, for example, Disperbyk-2001 (BYK Chemie Co., Ltd.), when using a dispersion prepared by mixing 2-butoxyethanol and propylene glycol monomethyl ether acetate as an organic solvent, EFKA-4046 (EFKA Co., Ltd.) ), It is preferable to use a dispersion prepared by mixing butyl acetate and propylene glycol monomethyl ether acetate as an organic solvent.
상기 유기용제는 안료분산액 100중량부에 대하여 10 내지 90 중량부의 양이 사용된다.The organic solvent is used in an amount of 10 to 90 parts by weight based on 100 parts by weight of the pigment dispersion.
유기안료, 분산제, 유기용제를 분산시키면서 혼합하기 위해 사용되는 분산기로는 롤러밀(roller mill), 제트밀(jet mill), 수직비드밀(vertical-bead mill), 수평비드밀(horizontal-bead mill), 초음파 분쇄기 등이 사용될 수 있으며, 분쇄 및 분산된 후 안료분산액의 최종 입도(particle size)는 50~100nm 사이가 되도록 하는 것이 바람직하다.Dispersers used to disperse and mix organic pigments, dispersants, and organic solvents include roller mills, jet mills, vertical-bead mills, and horizontal-bead mills. ), An ultrasonic grinder or the like may be used, and the final particle size of the pigment dispersion after grinding and dispersing is preferably 50 to 100 nm.
또한, 분쇄 및 분산 후 안료분산액의 최종 점도는 상온 25℃에서 5~20cP 인 것이 바람직하다.In addition, the final viscosity of the pigment dispersion after grinding and dispersion is preferably 5 ~ 20 cP at room temperature 25 ℃.
이하에서는 본 발명의 실시예에 따른 안료분산액의 경우 입자분포, 점도, 색특성, 휘도, 및 콘트라스트비가 우수하다는 것을 구체적인 실험예들을 들어 설명한다. 여기에 기재되지 않은 내용은 이 기술 분야에서 숙련된 자이면 충분히 기술적으로 유추할 수 있는 것이므로 그 설명을 생략한다.Hereinafter, the pigment dispersion according to the embodiment of the present invention will be described with specific experimental examples that the particle distribution, viscosity, color characteristics, brightness, and contrast ratio is excellent. Details not described herein are omitted because they can be sufficiently inferred by those skilled in the art.
<< 실시예1Example 1 >>
자일렌, 부틸아세테이트, 프로필렌글리콜모노에테르아세테이트를 각각 3:1:1의 비율로 혼합하여 전체 110g을 제조한다. 여기에 분산제로서 Disperbyk-163 17g을 넣고 30분간 교반(stirring)한 후 분산조제인 solosperse 22000 1.5g을 넣고 추 가적으로 30분간 교반한다.Xylene, butyl acetate, and propylene glycol monoether acetate are mixed at a ratio of 3: 1: 1, respectively, to prepare a total of 110 g. Add 17 g of Disperbyk-163 as a dispersant and stir for 30 minutes, and then add 1.5 g of dispersing agent solosperse 22000 and stir for an additional 30 minutes.
그 후, 마지막으로 C.I.Pigment RED 254 22.5g을 넣고 1시간 동안 기계적 교반기(Mechanical stirrer)로 교반 해준 후, 이트륨지르코늄비드를 상기 혼합용액과 같은 부피 첨가하여 2시간 동안 2000~2500rpm으로 분산시켜 안료분산액을 제조하였다.Then, 22.5 g of CIPigment RED 254 was added and stirred with a mechanical stirrer for 1 hour. Then, yttrium zirconium beads were added in the same volume as the mixed solution and dispersed at 2000 to 2500 rpm for 2 hours to disperse the pigment dispersion. Was prepared.
제조된 안료분산액의 입자크기는 OTSUKA 사의 ELS-8000 입도분석기로, 점도는 Brookfield사의 Viscometer DV-1, Spindle 18로, 색과 휘도는 OTSUKA 사의 MCPD-3000으로, 콘트라스트비는 TSUBOSAKA 사의 CT-1으로 각각 측정하였다.The particle size of the pigment dispersion prepared was OTSUKA ELS-8000 particle size analyzer, viscosity was Viscometer DV-1, Spindle 18 of Brookfield, color and brightness of MCPD-3000 of OTSUKA, and CT-1 of TSUBOSAKA. Each was measured.
그 결과 최종 평균입도는 65nm. 최종 평균점도는 8.0cP 값을 나타내었다.As a result, the final average particle size is 65nm. Final mean viscosity was 8.0 cP.
<< 비교예Comparative example >>
유기용제가 프로필렌글리콜모노에테르아세테이트 단독으로 사용되는 것을 제외하고는 실시예 1과 동일하다.Except that the organic solvent is used alone propylene glycol monoether acetate is the same as in Example 1.
비교예에 의해 제조된 안료분산액의 최종 입도와 점도는 각각 85nm, 10.7cP이다.The final particle size and viscosity of the pigment dispersion prepared in Comparative Example are 85 nm and 10.7 cP, respectively.
상기와 같이 제조한 실시예와 비교예에 대하여 색감도, 휘도, 및 콘트라스트비를 측정하였으며, 이들은 각각 도 1, 도 2, 및 표 3에 나타내었다.Color sensitivity, brightness, and contrast ratio were measured for the Examples and Comparative Examples prepared as described above, which are shown in FIGS. 1, 2, and 3, respectively.
도 1은 상기 실시예와 비교예에 의해 제조된 안료분산액의 색감도를 테스트한 결과를 나타내는 그래프이다.1 is a graph showing the results of testing the color sensitivity of the pigment dispersion prepared in Examples and Comparative Examples.
도 1을 참조하면 비교예의 값이 실시예의 값보다 위에 있음을 알 수 있는 데, 이는 Ry값이 크다는 의미로서, 색이 밝다는 것을 의미한다. 따라서, 도 1상으로 볼때는 비교예가 실시예보다 색감이 밝음을 알 수 있다.Referring to Figure 1 it can be seen that the value of the comparative example is above the value of the embodiment, which means that the Ry value is large, which means that the color is bright. Therefore, as seen in FIG. 1, it can be seen that the comparative example is brighter in color than the example.
도 2는 상기 실시예와 비교예에 의해 제조된 안료분산액의 휘도를 테스트한 결과를 나타내는 그래프이다.2 is a graph showing the results of testing the luminance of the pigment dispersion prepared by the above Examples and Comparative Examples.
도 2를 참조하면 비교예가 색이 밝은 데도 불구하고 실시예가 휘도가 높다는 것을 알 수 있다. 원래 색이 밝으면 휘도가 높은 것이 일반적이나 색이 실시예가 비교예보다 어두움에도 불구하고 휘도가 높다는 것을 알 수 있다.Referring to FIG. 2, it can be seen that although the Comparative Example is bright in color, the Example has high luminance. If the original color is bright, the luminance is generally high, but it can be seen that the luminance is higher despite the fact that the color is darker than the comparative example.
표 1은 실시예와 비교예의 콘트라스트비(CR)를 비교한 표이다.Table 1 is a table comparing the contrast ratio (CR) of the Examples and Comparative Examples.
표 1은 상기의 실시예와 비교예에 대하여 동일 Rx 값에 대한 콘트라스트비(CR; Contrast ratio)를 나타내는데, 표 1에서 보는 바와 같이 동일한 Rx 값에 대하여 실시예가 비교예보다 300 이상의 높은 값을 나타내고 있음을 알 수 있다.Table 1 shows the contrast ratio (CR) for the same Rx value with respect to the above Examples and Comparative Examples. As shown in Table 1, the Example shows a value of 300 or more higher than the Comparative Example for the same Rx value. It can be seen that.
이상 본 발명의 실시예들을 설명하였으나, 본 발명은 상기 실시예에 한정되는 것이 아니라 서로 다른 다양한 형태로 제조될 수 있으며, 본 발명이 속하는 기술분야에서 통상의 지식을 가진 자는 본 발명의 기술적 사상이나 필수적인 특징을 변경하지 않고서 다른 구체적인 형태로 실시될 수 있다는 것을 이해할 수 있을 것이다. 그러므로 이상에서 기술한 실시예들은 모든 면에서 예시적인 것이며 한정적이 아닌 것으로 이해해야만 한다.Although the embodiments of the present invention have been described above, the present invention is not limited to the above embodiments, and may be manufactured in various forms, and a person of ordinary skill in the art to which the present invention belongs may have It will be understood that other specific forms may be practiced without changing the essential features. Therefore, it should be understood that the embodiments described above are exemplary in all respects and not restrictive.
본 발명의 실시예에 따른 안료분산액에 의하면 휘도 및 콘트라스트비가 향상되고, 입자크기의 균일성, 저장안정성, 및 분산안정성 측면에서도 종래의 단일 유기용제를 사용하는 것에 비해 크게 향상되었음을 알 수 있다.According to the pigment dispersion according to the embodiment of the present invention, it can be seen that the luminance and contrast ratio are improved, and the particle size uniformity, storage stability, and dispersion stability are significantly improved compared with those of the conventional single organic solvent.
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| KR20050103910A (en) * | 2003-01-30 | 2005-11-01 | 신닛테츠가가쿠 가부시키가이샤 | Pigment dispersion, color filter composition and color filter |
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