TWI444672B - Color filter and liquid crystal display device - Google Patents
Color filter and liquid crystal display device Download PDFInfo
- Publication number
- TWI444672B TWI444672B TW97132929A TW97132929A TWI444672B TW I444672 B TWI444672 B TW I444672B TW 97132929 A TW97132929 A TW 97132929A TW 97132929 A TW97132929 A TW 97132929A TW I444672 B TWI444672 B TW I444672B
- Authority
- TW
- Taiwan
- Prior art keywords
- pigment
- color filter
- transparent resin
- pigment dispersion
- resin solution
- Prior art date
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- 239000004973 liquid crystal related substance Substances 0.000 title claims description 25
- 239000000049 pigment Substances 0.000 claims description 349
- 229920005989 resin Polymers 0.000 claims description 152
- 239000011347 resin Substances 0.000 claims description 152
- 239000006185 dispersion Substances 0.000 claims description 117
- 239000007788 liquid Substances 0.000 claims description 98
- 238000004519 manufacturing process Methods 0.000 claims description 68
- 239000011248 coating agent Substances 0.000 claims description 63
- 238000000576 coating method Methods 0.000 claims description 63
- 238000000034 method Methods 0.000 claims description 54
- 239000000758 substrate Substances 0.000 claims description 52
- 239000002904 solvent Substances 0.000 claims description 39
- 239000011342 resin composition Substances 0.000 claims description 31
- 238000002156 mixing Methods 0.000 claims description 27
- 125000006850 spacer group Chemical group 0.000 claims description 27
- 238000004040 coloring Methods 0.000 claims description 26
- 239000007787 solid Substances 0.000 claims description 24
- LAVARTIQQDZFNT-UHFFFAOYSA-N 1-(1-methoxypropan-2-yloxy)propan-2-yl acetate Chemical compound COCC(C)OCC(C)OC(C)=O LAVARTIQQDZFNT-UHFFFAOYSA-N 0.000 claims description 17
- 239000000203 mixture Substances 0.000 claims description 16
- 239000002270 dispersing agent Substances 0.000 claims description 14
- VXQBJTKSVGFQOL-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethyl acetate Chemical compound CCCCOCCOCCOC(C)=O VXQBJTKSVGFQOL-UHFFFAOYSA-N 0.000 claims description 7
- 239000000976 ink Substances 0.000 description 113
- 239000010410 layer Substances 0.000 description 94
- 239000000178 monomer Substances 0.000 description 75
- 239000000243 solution Substances 0.000 description 75
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- 229920001577 copolymer Polymers 0.000 description 38
- 125000003700 epoxy group Chemical group 0.000 description 34
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 32
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 27
- 229920001187 thermosetting polymer Polymers 0.000 description 26
- 238000001035 drying Methods 0.000 description 24
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 23
- 229920000642 polymer Polymers 0.000 description 23
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 20
- 230000001588 bifunctional effect Effects 0.000 description 19
- 238000001723 curing Methods 0.000 description 19
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 18
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 18
- 150000001875 compounds Chemical class 0.000 description 18
- 239000001054 red pigment Substances 0.000 description 15
- 239000004793 Polystyrene Substances 0.000 description 14
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- 239000001056 green pigment Substances 0.000 description 14
- 229920002223 polystyrene Polymers 0.000 description 14
- 239000002202 Polyethylene glycol Substances 0.000 description 13
- GCTPMLUUWLLESL-UHFFFAOYSA-N benzyl prop-2-enoate Chemical compound C=CC(=O)OCC1=CC=CC=C1 GCTPMLUUWLLESL-UHFFFAOYSA-N 0.000 description 13
- 239000003795 chemical substances by application Substances 0.000 description 13
- 239000003086 colorant Substances 0.000 description 13
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 13
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- 239000004926 polymethyl methacrylate Substances 0.000 description 13
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 12
- 238000009835 boiling Methods 0.000 description 11
- 125000000524 functional group Chemical group 0.000 description 11
- 239000004094 surface-active agent Substances 0.000 description 11
- AOJOEFVRHOZDFN-UHFFFAOYSA-N benzyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCC1=CC=CC=C1 AOJOEFVRHOZDFN-UHFFFAOYSA-N 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 10
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- 239000003999 initiator Substances 0.000 description 9
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- 239000000654 additive Substances 0.000 description 6
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- 150000001244 carboxylic acid anhydrides Chemical class 0.000 description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 238000011156 evaluation Methods 0.000 description 6
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- UHFFVFAKEGKNAQ-UHFFFAOYSA-N 2-benzyl-2-(dimethylamino)-1-(4-morpholin-4-ylphenyl)butan-1-one Chemical compound C=1C=C(N2CCOCC2)C=CC=1C(=O)C(CC)(N(C)C)CC1=CC=CC=C1 UHFFVFAKEGKNAQ-UHFFFAOYSA-N 0.000 description 5
- MPIAGWXWVAHQBB-UHFFFAOYSA-N [3-prop-2-enoyloxy-2-[[3-prop-2-enoyloxy-2,2-bis(prop-2-enoyloxymethyl)propoxy]methyl]-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(COC(=O)C=C)(COC(=O)C=C)COCC(COC(=O)C=C)(COC(=O)C=C)COC(=O)C=C MPIAGWXWVAHQBB-UHFFFAOYSA-N 0.000 description 5
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- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 4
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- 125000001931 aliphatic group Chemical group 0.000 description 4
- 125000003118 aryl group Chemical group 0.000 description 4
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 description 4
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Classifications
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/20—Filters
- G02B5/22—Absorbing filters
- G02B5/223—Absorbing filters containing organic substances, e.g. dyes, inks or pigments
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/20—Filters
- G02B5/201—Filters in the form of arrays
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/1335—Structural association of cells with optical devices, e.g. polarisers or reflectors
- G02F1/133509—Filters, e.g. light shielding masks
- G02F1/133514—Colour filters
- G02F1/133516—Methods for their manufacture, e.g. printing, electro-deposition or photolithography
Landscapes
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Nonlinear Science (AREA)
- Chemical & Material Sciences (AREA)
- Mathematical Physics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Optical Filters (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
- Liquid Crystal (AREA)
- Ink Jet Recording Methods And Recording Media Thereof (AREA)
Description
本發明係關於形成如畫素部(著色層)般之指定圖型的硬化層所用之彩色濾光片用噴墨油墨,該噴墨用油墨之製造方法,使用該噴墨用油墨製造彩色濾光片之方法,以及使用該彩色濾光片製造液晶顯示裝置之方法。The present invention relates to an inkjet ink for color filter used for forming a hardened layer of a pattern such as a pixel (colored layer), a method for producing the ink for inkjet, and a color filter using the ink for inkjet A method of a light sheet, and a method of manufacturing a liquid crystal display device using the color filter.
近年,隨著個人電腦的發達,特別隨著攜帶用個人電腦的發達,液晶顯示器,尤其是彩色液晶顯示器的需求有增加的傾向。但是,由於此彩色液晶顯示器為昂貴的,故降低費用的要求變高,特別對於費用比重高的彩色濾光片的費用降低之要求高。In recent years, with the development of personal computers, particularly with the development of portable personal computers, the demand for liquid crystal displays, especially color liquid crystal displays, has increased. However, since the color liquid crystal display is expensive, the cost reduction requirement is high, and the cost reduction of the color filter having a high cost ratio is particularly high.
於此類彩色濾光片中,例如於玻璃和塑膠等所形成的透明基板表面,通常形成紅(R)、綠(G)、及藍(B)之三原色的著色層,並於其上視需要形成保護膜構造為一般的。三色著色層為構成各個畫素,將對應各個R、G及B畫素的電極ON、OFF,令液晶以快門型式運作,對各個畫素通過適當的光線,進行彩色顯示。In such a color filter, for example, on the surface of a transparent substrate formed of glass and plastic, a coloring layer of three primary colors of red (R), green (G), and blue (B) is usually formed, and is viewed from above. It is necessary to form a protective film structure as a general one. The three-color coloring layer is used to form each pixel, and the electrodes corresponding to the respective R, G, and B pixels are turned ON and OFF, so that the liquid crystal operates in a shutter mode, and the respective pixels are color-displayed by appropriate light.
又,於畫素間設置遮光層所構成的黑色矩陣。更且,於保護膜上設置ITO膜等所構成的透明電極層。保護膜為將形成著色層之狀態的表面段差予以埋平,並於形成透明電極層之步驟中防止著色層的熱惡化等之目的下形成。Further, a black matrix composed of a light shielding layer is provided between the pixels. Further, a transparent electrode layer made of an ITO film or the like is provided on the protective film. The protective film is formed by burying the surface step difference in a state in which the colored layer is formed, and preventing heat deterioration of the colored layer or the like in the step of forming the transparent electrode layer.
先前進行之彩色濾光片的製造方法可列舉例如染色法。此染色法為首先於玻璃基板上形成染色用材料水溶性高分子材料,並以光蝕刻步驟將其形成所欲形狀之圖型後,將所得之圖型浸漬於染色浴中令其著色取得圖型。將其重複3次則形成R、G、及B的彩色濾光層。The method of producing the color filter previously performed may, for example, be a dyeing method. The dyeing method is to form a water-soluble polymer material for dyeing material on a glass substrate first, and to form a pattern of a desired shape by a photolithography step, and then immersing the obtained pattern in a dyeing bath to obtain a coloring pattern. type. This was repeated three times to form color filter layers of R, G, and B.
又,其他方法有顏料分散法。此方法為首先於基板上形成分散顏料的感光性樹脂層,將其圖型化取得單色之圖型。更且,將此步驟重複3次,則形成R、G、及B的彩色濾光層。Further, other methods include a pigment dispersion method. In this method, a photosensitive resin layer in which a pigment is dispersed is first formed on a substrate, and the pattern is patterned to obtain a monochrome pattern. Further, this step is repeated three times to form color filter layers of R, G, and B.
更且,其他方法可列舉電沉積法、和於熱硬化樹脂中分散顏料並進行R、G、及B之三次印刷後,令樹脂熱硬化的方法等。Further, other methods include a electrodeposition method, a method of dispersing a pigment in a thermosetting resin, and performing three printing of R, G, and B, followed by a method of thermally curing the resin.
但是,任一種方法均為了著色R、G、及B3色,而必須重複3次相同之步驟,具有費用變高的問題,和因重複同樣之步驟而令產率降低的問題。However, any of the methods is to color the R, G, and B3 colors, and the same steps must be repeated three times, which has a problem that the cost becomes high, and the problem that the yield is lowered by repeating the same steps.
作為解決此些問題點之彩色濾光片的製造方法,已提案於基板表面以噴墨方式形成著色層(畫素部)的方法。As a method of manufacturing a color filter that solves such problems, a method of forming a color layer (pixel portion) by inkjet on a substrate surface has been proposed.
以噴墨方式的著色步驟為由噴墨用吐出噴頭的管嘴前端,吐出R、G、或B任一種噴墨,配合圖型將噴墨吹至基板表面,形成著色層。若根據噴墨方式,因可各以1次進行R、G、B的著色步驟,故於削減製造費用方面受到注目。The coloring step in the inkjet method is to discharge any of R, G, or B by the tip end of the nozzle for the inkjet discharge nozzle, and to blow the ink onto the surface of the substrate in accordance with the pattern to form a colored layer. According to the inkjet method, since the coloring steps of R, G, and B can be performed once, the production cost is reduced.
以噴墨方式將油墨配合正確圖型吹送形成畫素上,要求由吐出噴頭吐出時之油墨的直進性、安定性。但是,油墨的蒸發速度若過早,則吐出噴頭之管嘴前端的油墨黏度急劇增加,發生油墨滴的飛行彎曲,並且若隔開時間間歇性吐出,則有引起孔堵塞且無法再吐出之情況。又,彩色濾光片的著色劑多使用顏料,若彩色濾光片用油墨的顏料分散性差,則經由顏料粒子彼此的凝集而在吐出噴頭的管嘴部引起孔堵塞。因此,於使用顏料作為著色劑之情形中,顏料分散性亦對油墨的吐出性能造成影響。The ink is blown to the correct pattern by the ink jet method to form a pixel, and the ink is required to be straightforward and stable when discharged from the discharge head. However, if the evaporation speed of the ink is too early, the ink viscosity at the tip end of the nozzle of the discharge head sharply increases, and the ink droplets are flying and bent. If the ink is intermittently discharged at intervals, the hole may be clogged and the discharge may not be discharged. . Further, a pigment is often used for the color filter of the color filter, and if the pigment dispersion property of the color filter ink is poor, the pores are clogged at the nozzle portion of the discharge head through the aggregation of the pigment particles. Therefore, in the case of using a pigment as a colorant, the pigment dispersibility also affects the discharge performance of the ink.
於專利文獻1中,記載以噴墨方式吹送著色油墨形成著色層(畫素部),製造彩色濾光片的方法中,亦可使用具有經由可見光線和紫外線等之放射線硬化性的樹脂(光硬化性樹脂),作為黏合樹脂的著色油墨(光硬化性油墨)。但是,若將此類先前的光硬化性油墨,就其原樣使用於噴墨方式,則在吹送著色油墨當中,於噴墨的噴頭前端油墨進行乾燥且慢慢令黏度上升,使得吐出性變差。其結果,著色油墨的吐出量和吐出方向不安定,恐於噴墨噴頭中發生孔堵塞。如此,使用含有著色劑和黏合成分的油墨時,經由油墨固黏於管嘴內,使得噴墨的吐出安定性降低,嚴重情況為具有不能馬上吐出的問題。In Patent Document 1, it is described that a coloring layer (pixel portion) is formed by blowing a coloring ink by an inkjet method, and a resin having a radiation curable property such as visible light and ultraviolet rays can be used in the method of producing a color filter. A curable resin) is a coloring ink (photocurable ink) of a binder resin. However, when such a conventional photocurable ink is used as it is in the ink jet method, in the blown colored ink, the ink is dried at the tip of the ink jet head and the viscosity is gradually increased, so that the discharge property is deteriorated. . As a result, the discharge amount of the colored ink and the discharge direction are unstable, and the clogging of the holes in the ink jet head may occur. As described above, when an ink containing a coloring agent and a binder component is used, it is fixed in the nozzle via the ink, so that the discharge stability of the inkjet is lowered, and in serious cases, there is a problem that it cannot be discharged immediately.
於專利文獻2中,揭示於透明基板上形成具有油墨吸收能力的樹脂組成物層,並於該樹脂組成物層,以噴墨方式沿著指定的著色圖型賦予油墨著色,作成著色樹脂組成物層之步驟重複進行2次以上,將複數的著色樹脂組成物層層合形成著色層為其特徵之彩色濾光片的製造方法。但是,此處所揭示之製造方法中,因為著色油墨的顏料濃度低,故為了取得作為彩色濾光片的色純度、色再現性,乃必須重複油墨充填步驟的複雜步驟,產率降低。Patent Document 2 discloses that a resin composition layer having an ink absorbing ability is formed on a transparent substrate, and ink is colored on the resin composition layer along a predetermined color pattern by an inkjet method to form a colored resin composition. The step of layering is repeated two or more times, and a plurality of colored resin composition layers are laminated to form a color filter having a coloring layer. However, in the production method disclosed herein, since the pigment concentration of the colored ink is low, in order to obtain color purity and color reproducibility as a color filter, it is necessary to repeat the complicated steps of the ink filling step, and the yield is lowered.
構成液晶元件的彩色濾光片,要求色純度及色再現性高,即著色部的著色劑濃度高者,以噴墨方式製造此類彩色濾光片上,可列舉令賦予的油墨份量增加的方法,但是若賦予的油墨份量增加,則難抑制油墨摻出所發生的混色,無法以良好產率製造彩色濾光片。The color filter constituting the liquid crystal element is required to have high color purity and color reproducibility, that is, a colorant having a high coloring agent concentration in the colored portion, and such a color filter is produced by an inkjet method, and the amount of the ink to be applied is increased. However, if the amount of the ink to be applied is increased, it is difficult to suppress the color mixture which occurs in the ink doping, and the color filter cannot be produced in good yield.
如上述,以噴墨方式形著色層製造彩色濾光片的方法,由噴墨管嘴之噴頭吐出時之直進行、安定性優良,且以1次之著色成分塗佈可取得高色純度、色再現性的方法,仍未取得。As described above, the method of producing a color filter by the inkjet type colored layer is straightforward when discharged from the nozzle of the ink jet nozzle, and the stability is excellent, and high color purity can be obtained by applying the color component once. The method of color reproducibility has not yet been achieved.
[專利文獻1]特開平11-295520號公報[Patent Document 1] JP-A-11-295520
[專利文獻2]特開2002-311224號公報[Patent Document 2] JP-A-2002-311224
本發明為以提供由噴頭吐出時之直進性及安定性優良,著彈的油墨滴可輕易廣泛濕潤至油墨層形成區域全體的各個角落,且以1次之著色成分塗佈即可供給高色純度及色再現性之使用噴墨油墨之彩色濾光片的製造方法,使用該噴墨油墨之彩色濾光片的製造方法,及使用該彩色濾光片之製造方法之液晶顯示裝置的製造方法。The present invention is excellent in straightness and stability when the nozzle is discharged, and the ink droplets that are springed can be easily wetted to all corners of the entire ink layer forming region, and can be supplied with high color by coating with one color component. Method for producing color filter using inkjet ink for purity and color reproducibility, method for producing color filter using inkjet ink, and method for manufacturing liquid crystal display device using method for producing color filter .
本發明者等人為了解決上述課題而致力檢討之結果,發現將著色成分之顏料和黏合成分之透明樹脂分別於顏料分散液和透明樹脂溶液中以比例塗佈,則可解決上述課題,並且達成本發明。In order to solve the above problems, the inventors of the present invention have found that the above-mentioned problems can be solved by the fact that the pigment of the coloring component and the transparent resin of the binder component are applied in a ratio between the pigment dispersion liquid and the transparent resin solution, respectively. this invention.
即,本發明為下列(1)~(9)所示之彩色濾光片之製造方法及使用其之液晶顯示裝置。That is, the present invention is a method for producing a color filter shown in the following (1) to (9) and a liquid crystal display device using the same.
(1)一種彩色濾光片之製造方法,其特徵為包含於透明性絕緣基板上之間隔部的間隙,以噴墨方式選擇性塗佈顏料分散液之步驟(顏料分散液塗佈步驟),和在前述顏料分散液塗佈步驟後,於前述間隔部的間隙以噴墨方式選擇性塗佈透明樹脂溶液,並於該間隙內混合顏料分散液和透明樹脂溶液之步驟(透明樹脂溶液塗佈步驟),和令前述透明樹脂溶液塗佈步驟所形成之顏料分散液和透明樹脂溶液的混合液層硬化之步驟(硬化步驟)。(1) A method of producing a color filter, comprising the step of selectively coating a pigment dispersion liquid by a liquid-jet method in a gap of a spacer portion on a transparent insulating substrate (pigment dispersion coating step), And a step of selectively coating the transparent resin solution by the inkjet method in the gap of the aforementioned spacer after the coating step of the pigment dispersion, and mixing the pigment dispersion and the transparent resin solution in the gap (transparent resin solution coating) And a step of hardening the mixed layer of the pigment dispersion liquid and the transparent resin solution formed by the aforementioned transparent resin solution coating step (hardening step).
(2)如申請項1記載之彩色濾光片之製造方法,其中以前述顏料分散液塗佈步驟所形成之著色液層的膜厚為0.4~2μm。(2) The method for producing a color filter according to the first aspect of the invention, wherein the thickness of the coloring liquid layer formed by the pigment dispersion coating step is 0.4 to 2 μm.
(3)如申請項1或2記載之彩色濾光片之製造方法,其中前述混合液層為以與前述間隔部相同膜厚形成。(3) The method of producing a color filter according to claim 1 or 2, wherein the mixed liquid layer is formed to have the same film thickness as the spacer.
(4)如申請項1~3中任一項記載之彩色濾光片之製造方法,其中前述顏料分散液塗佈步驟中,將塗佈顏料分散液所形成之著色液層以40~160℃之溫度乾燥。(4) The method for producing a color filter according to any one of claims 1 to 3, wherein in the pigment dispersion coating step, the coloring liquid layer formed by coating the pigment dispersion liquid is 40 to 160 ° C The temperature is dry.
(5)如申請項1~4中任一項記載之彩色濾光片之製造方法,其中前述透明樹脂溶液塗佈步驟中,將混合顏料分散液和透明樹脂溶液所得之混合液層以80~200℃之溫度乾燥。(5) The method for producing a color filter according to any one of claims 1 to 4, wherein in the step of applying the transparent resin solution, the mixed liquid layer obtained by mixing the pigment dispersion liquid and the transparent resin solution is 80 to 80 Dry at 200 ° C.
(6)如申請項1~5中任一項記載之彩色濾光片之製造方法,其中令前述混合液層硬化後之該混合液層中,顏料與透明樹脂之固形成分比率為1:0.4~1。(6) The method for producing a color filter according to any one of claims 1 to 5, wherein a solid content ratio of the pigment to the transparent resin in the mixed liquid layer obtained by curing the mixed liquid layer is 1:0.4 ~1.
(7)如申請項1~6中任一項記載之彩色濾光片之製造方法,其中前述顏料分散液至少由顏料、顏料分散劑、及溶劑所構成,且該溶劑之沸點為200℃以上。(7) The method for producing a color filter according to any one of claims 1 to 6, wherein the pigment dispersion liquid is composed of at least a pigment, a pigment dispersant, and a solvent, and the boiling point of the solvent is 200 ° C or higher. .
(8)如申請項1~7中任一項記載之彩色濾光片之製造方法,其中透明樹脂溶液中所含之透明樹脂組成物為由光硬化型樹脂組成物所構成。(8) The method for producing a color filter according to any one of claims 1 to 7, wherein the transparent resin composition contained in the transparent resin solution is composed of a photocurable resin composition.
(9)一種液晶顯示裝置,其特徵為具備根據如申請項1~8項中任一項記載之製造方法所製造的彩色濾光片,和對向基板,和於前述彩色濾光片與前述對向基板之間所夾住的液晶組成物。(9) A liquid crystal display device comprising the color filter manufactured by the manufacturing method according to any one of claims 1 to 8, and a counter substrate, and the color filter and the foregoing A liquid crystal composition sandwiched between the opposing substrates.
若根據本發明,將著色成分之顏料與黏合成分所構成的透明樹脂,分別於較低黏度之顏料分散液和透明樹脂溶液中以比例調製,並將各液以個別之步驟於透明性絕緣基板上塗佈,則可取得下列所示之效果。According to the present invention, the pigment of the coloring component and the transparent resin composed of the binder component are respectively proportioned in a pigment dispersion liquid of a lower viscosity and a transparent resin solution, and each liquid is applied to the transparent insulating substrate in a separate step. When applied, the following effects can be obtained.
(1)因為顏料分散液與透明樹脂溶液具有適度的黏度,故由吐出噴頭吐出時的直進性、安定性優良。因此,不會發生吐出噴頭之管嘴前端的油墨黏度急劇增加且油墨滴的飛行彎曲,並且若隔開時間間歇性吐出時不會引起孔堵塞且無法再吐出,形成著色層的作業性優良。(1) Since the pigment dispersion liquid and the transparent resin solution have an appropriate viscosity, the straightness and stability at the time of discharge from the discharge head are excellent. Therefore, the ink viscosity at the tip end of the nozzle of the discharge head does not increase sharply, and the flying of the ink droplets is sharply bent. When the discharge is intermittently intermittent, the hole is not clogged and the ink can be discharged again, and the workability of forming the colored layer is excellent.
(2)因為可低黏度下印寫高顏料濃度的顏料分散液,放在取得作為彩色濾光片的色純度、色再現性上,不需要塗佈數次著色成分,且可以1次之著色成分塗佈步驟塗佈必要的著色成分量,可以更良好產率製造彩色顯示特性優良的液晶元件。(2) Since a pigment dispersion having a high pigment concentration can be printed at a low viscosity, it is not necessary to apply a plurality of coloring components for color purity and color reproducibility as a color filter, and it is possible to color one time. The component coating step applies a necessary amount of the coloring component, and a liquid crystal element excellent in color display characteristics can be produced in a more favorable yield.
(3)不會發生混色等問題,著彈的油墨滴可輕易廣泛濕潤至油墨層形成區域全體的各個角落。(3) There is no problem such as color mixing, and the ink droplets of the shot can be easily wetted to all corners of the entire ink layer forming region.
因此,若根據本發明,則可廉價製造性能更優良之信賴性高的彩色濾光片。特別,以穿透濃度大且均勻,並且無脫色的畫素部可精密地形成,可製造亮度提高的彩色濾光片。又,若根據本發明,由於使用性能更良好的彩色濾光片,故可以良好產率提供彩色顯示特性優良的液晶顯示元件,且可製造高品質的液晶顯示裝置。Therefore, according to the present invention, it is possible to inexpensively manufacture a color filter having high reliability and high reliability. In particular, a pixel portion having a large penetration density and uniformity and no discoloration can be precisely formed, and a color filter having improved brightness can be manufactured. Moreover, according to the present invention, since a color filter having better performance is used, a liquid crystal display element excellent in color display characteristics can be provided in a good yield, and a high-quality liquid crystal display device can be manufactured.
本發明之彩色濾光片之製造方法為包含於透明性絕緣基板上之間隔部的間隙,以噴霧方式選擇性塗佈顏料分散液之步驟(顏料分散液塗佈步驟),和在前述顏料分散液塗佈步驟後,於前述間隔部的間隙以噴墨方式選擇性塗佈透明樹脂溶液,並於該間隙內混合顏料分散液和透明樹脂溶液之步驟(透明樹脂溶液塗佈步驟),和令前述透明樹脂溶液塗佈步驟所形成之顏料分散液和透明樹脂溶液的混合液層硬化之步驟(硬化步驟)。The method for producing a color filter of the present invention is a step of selectively coating a pigment dispersion liquid by a spray on a gap portion of a spacer provided on a transparent insulating substrate (pigment dispersion coating step), and dispersing the pigment in the foregoing After the liquid coating step, a step of selectively coating the transparent resin solution by the inkjet method in the gap of the spacer portion, and mixing the pigment dispersion liquid and the transparent resin solution in the gap (transparent resin solution coating step), and The step of hardening the mixed layer of the pigment dispersion liquid and the transparent resin solution formed by the transparent resin solution coating step (hardening step).
於本發明之製造方法中,顏料分散液塗佈步驟所用之顏料分散液,至少由顏料和溶劑所構成,視需要配合其他成分。In the production method of the present invention, the pigment dispersion liquid used in the step of coating the pigment dispersion liquid is composed of at least a pigment and a solvent, and other components are blended as needed.
作為著色劑的顏料為配合畫素(畫素部)之R、G、B等和黑色矩陣層之所要求的顏色,由有機著色劑及無機著色劑中選出使用任意物質。有機著色劑可使用例如,染料、有機顏料、天然色素等。又,無機著色劑可使用例如,無機顏料、體質顏料等。The pigment as a coloring agent is a color required for the R, G, B, and the like of the pixel (pixel portion) and the black matrix layer, and any of the organic coloring agent and the inorganic coloring agent is selected and used. As the organic colorant, for example, a dye, an organic pigment, a natural pigment, or the like can be used. Further, as the inorganic colorant, for example, an inorganic pigment, an extender pigment or the like can be used.
其中以有機顏料為發色性高,且耐熱性亦高,故較佳使用。有機顏料可列舉例如色彩指數(C.I.;The Society of Dyers and Colourist公司發行)中被分類成顏料(Pigment)的化合物,具體而言,加以如下述色彩指數(C.I.)編號者。Among them, organic pigments are preferably used because of their high color developability and high heat resistance. The organic pigment may, for example, be a compound classified as a pigment in a color index (C.I.; issued by The Society of Dyers and Colourist Co., Ltd.), specifically, a color index (C.I.) as described below.
C.I.顏料黃1、C.I.顏料黃3、C.I.顏料黃12、C.I.顏料黃13、C.I.顏料黃14、C.I.顏料黃15、C.I.顏料黃16、C.I.顏料黃17、C.1.顏料黃20、C.I.顏料黃24、C.I.顏料黃31、C.I.顏料黃55、C.I.顏料黃60、C.I.顏料黃61、C.I.顏料黃65、C.I.顏料黃71、C.I.顏料黃73、C.I.顏料黃74、C.I.顏料黃81、C.I.顏料黃83、C.I.顏料黃93、C.I.顏料黃95、C.I.顏料黃97、C.I.顏料黃98、C.I.顏料黃100、C.I.顏料黃101、C.I.顏料黃104、C.I.顏料黃106、C.I.顏料黃108、C.I.顏料黃109、C.I.顏料黃110、C.I.顏料黃113、C.I.顏料黃114、C.I.顏料黃116、C.I.顏料黃117、C.I.顏料黃119、C.I.顏料黃120、C.I.顏料黃126、C.I.顏料黃127、C.I.顏料黃128、C.I.顏料黃129、C.I.顏料黃138、C.I.顏料黃139、C.I.顏料黃150、C.I.顏料黃151、C.I.顏料黃152、C.I.顏料黃153、C.I.顏料黃154、C.I.顏料黃155、C.I.顏料黃156、C.I.顏料黃166、C.I.顏料黃168、C.I.顏料黃175;CI Pigment Yellow 1, CI Pigment Yellow 3, CI Pigment Yellow 12, CI Pigment Yellow 13, CI Pigment Yellow 14, CI Pigment Yellow 15, CI Pigment Yellow 16, CI Pigment Yellow 17, C. 1. Pigment Yellow 20, CI Pigment Yellow 24, CI Pigment Yellow 31, CI Pigment Yellow 55, CI Pigment Yellow 60, CI Pigment Yellow 61, CI Pigment Yellow 65, CI Pigment Yellow 71, CI Pigment Yellow 73, CI Pigment Yellow 74, CI Pigment Yellow 81, CI Pigment Yellow 83, CI Pigment Yellow 93, CI Pigment Yellow 95, CI Pigment Yellow 97, CI Pigment Yellow 98, CI Pigment Yellow 100, CI Pigment Yellow 101, CI Pigment Yellow 104, CI Pigment Yellow 106, CI Pigment Yellow 108, CI Pigment Huang 109, CI Pigment Yellow 110, CI Pigment Yellow 113, CI Pigment Yellow 114, CI Pigment Yellow 116, CI Pigment Yellow 117, CI Pigment Yellow 119, CI Pigment Yellow 120, CI Pigment Yellow 126, CI Pigment Yellow 127, CI Pigment Yellow 128, CI Pigment Yellow 129, CI Pigment Yellow 138, CI Pigment Yellow 139, CI Pigment Yellow 150, CI Pigment Yellow 151, CI Pigment Yellow 152, CI Pigment Yellow 153, CI Pigment Yellow 154, CI Pigment Yellow 155, CI Pigment Yellow 156, CI Pigment Yellow 166, CI Pigment Yellow 168, CI Pigment Yellow 175;
C.I.顏料橙1、C.I.顏料橙5、C.I.顏料橙13、C.I.顏料橙14、C.I.顏料橙16、C.I.顏料橙17、C.I.顏料橙24、C.I.顏料橙34、C.I.顏料橙36、C.I.顏料橙38、C.I.顏料橙40、C.I.顏料橙43、C.I.顏料橙46、C.I.顏料橙49、C.I.顏料橙51、C.I.顏料橙61、C.I.顏料橙63、C.I.顏料橙64、C.I.顏料橙71、C.I.顏料橙73;C.I.顏料紫1、C.I.顏料紫19、C.I.顏料紫23、C.I.顏料紫29、C.I.顏料紫32、C.I.顏料紫36、C.I.顏料紫38;CI Pigment Orange 1, CI Pigment Orange 5, CI Pigment Orange 13, CI Pigment Orange 14, CI Pigment Orange 16, CI Pigment Orange 17, CI Pigment Orange 24, CI Pigment Orange 34, CI Pigment Orange 36, CI Pigment Orange 38, CI Pigment Orange 40, CI Pigment Orange 43, CI Pigment Orange 46, CI Pigment Orange 49, CI Pigment Orange 51, CI Pigment Orange 61, CI Pigment Orange 63, CI Pigment Orange 64, CI Pigment Orange 71, CI Pigment Orange 73; CI pigment violet 1, CI pigment violet 19, CI pigment violet 23, CI pigment violet 29, CI pigment violet 32, CI pigment violet 36, CI pigment violet 38;
C.I.顏料紅I、C.I.顏料紅2、C.I.顏料紅3、C.I.顏料紅4、C.I.顏料紅5、C.I.顏料紅6、C.I.顏料紅7、C.I.顏料紅8、C.I.顏料紅9、C.I.顏料紅10、C.I.顏料紅11、C.I.顏料紅12、C.I.顏料紅14、C.I.顏料紅15、C.I.顏料紅16、C.I.顏料紅17、C.I.顏料紅18、C.I.顏料紅19、C.I.顏料紅21、C.I.顏料紅22、C.I.顏料紅23、C.I.顏料紅30、C.I.顏料紅31、C.I.顏料紅32、C.I.顏料紅37、C.I.顏料紅38、C.I.顏料紅40、C.I.顏料紅41、C.I.顏料紅42、C.I.顏料紅48:1、C.I.顏料紅48:2、C.I.顏料紅48:3、C.I.顏料紅48:4、C.I.顏料紅49:1、C.I.顏料紅49:2、C.I.顏料紅50:1、C.I.顏料紅52:1、C.I.顏料紅53:1、C.I.顏料紅57、C.I.顏料紅57:1、C.I.顏料紅57:2、C.I.顏料紅58:2、C.I.顏料紅58:4、C.I.顏料紅60:1、C.I.顏料紅63:1、C.I.顏料紅63:2、C.I.顏料紅64:1、C.I.顏料紅81:1、C.I.顏料紅83、C.I.顏料紅88、C.I.顏料紅90:1、C.I.顏料紅97、C.I.顏料紅101、C.I.顏料紅102、C.I.顏料紅104、C.I.顏料紅105、C.I.顏料紅106、C.I.顏料紅108、C.I.顏料紅112、C.I.顏料紅113、C.I.顏料紅114、C.I.顏料紅122、C.I.顏料紅123、C.I.顏料紅144、C.I.顏料紅146、C.I.顏料紅149、C.I.顏料紅150、C.I.顏料紅151、C.I.顏料紅166、C.I.顏料紅168、C.I.顏料紅170、C.I.顏料紅171、C.I.顏料紅172、C.I.顏料紅174、C.I.顏料紅175、C.I.顏料紅176、C.I.顏料紅177、C.I.顏料紅178、C.I.顏料紅179、C.I.顏料紅180、C.I.顏料紅185、C.I.顏料紅187、C.I.顏料紅188、C.I.顏料紅190、C.I.顏料紅193、C.I.顏料紅194、C.I.顏料紅202、C.I.顏料紅206、C.I.顏料紅207、C.I.顏料紅208、C.I.顏料紅209、C.I.顏料紅215、C.I.顏料紅216、C.I.顏料紅220、C.I.顏料紅224、C.I.顏料紅226、C.I.顏料紅242、C.I.顏料紅243、C.I.顏料紅245、C.I.顏料紅254、C.I.顏料紅255、C.I.顏料紅264、C.I.顏料紅265;CI Pigment Red I, CI Pigment Red 2, CI Pigment Red 3, CI Pigment Red 4, CI Pigment Red 5, CI Pigment Red 6, CI Pigment Red 7, CI Pigment Red 8, CI Pigment Red 9, CI Pigment Red 10, CI Pigment Red 11, CI Pigment Red 12, CI Pigment Red 14, CI Pigment Red 15, CI Pigment Red 16, CI Pigment Red 17, CI Pigment Red 18, CI Pigment Red 19, CI Pigment Red 21, CI Pigment Red 22, CI Pigment Red 23, CI Pigment Red 30, CI Pigment Red 31, CI Pigment Red 32, CI Pigment Red 37, CI Pigment Red 38, CI Pigment Red 40, CI Pigment Red 41, CI Pigment Red 42, CI Pigment Red 48: 1. CI Pigment Red 48:2, CI Pigment Red 48:3, CI Pigment Red 48:4, CI Pigment Red 49:1, CI Pigment Red 49:2, CI Pigment Red 50:1, CI Pigment Red 52:1 , CI Pigment Red 53:1, CI Pigment Red 57, CI Pigment Red 57:1, CI Pigment Red 57:2, CI Pigment Red 58:2, CI Pigment Red 58:4, CI Pigment Red 60:1, CI Pigment Red 63:1, CI Pigment Red 63:2, CI Pigment Red 64:1, CI Pigment Red 81:1, CI Pigment Red 83, CI Pigment Red 88, CI Pigment Red 90:1, CI Pigment Red 97 , CI Pigment Red 101, CI Pigment Red 102, CI Pigment Red 104, CI Pigment Red 105, CI Pigment Red 106, CI Pigment Red 108, CI Pigment Red 112, CI Pigment Red 113, CI Pigment Red 114, CI Pigment Red 122 , CI Pigment Red 123, CI Pigment Red 144, CI Pigment Red 146, CI Pigment Red 149, CI Pigment Red 150, CI Pigment Red 151, CI Pigment Red 166, CI Pigment Red 168, CI Pigment Red 170, CI Pigment Red 171 , CI Pigment Red 172, CI Pigment Red 174, CI Pigment Red 175, CI Pigment Red 176, CI Pigment Red 177, CI Pigment Red 178, CI Pigment Red 179, CI Pigment Red 180, CI Pigment Red 185, CI Pigment Red 187 , CI Pigment Red 188, CI Pigment Red 190, CI Pigment Red 193, CI Pigment Red 194, CI Pigment Red 202, CI Pigment Red 206, CI Pigment Red 207, CI Pigment Red 208, CI Pigment Red 209, CI Pigment Red 215 , CI Pigment Red 216, CI Pigment Red 220, CI Pigment Red 224, CI Pigment Red 226, CI Pigment Red 242, CI Pigment Red 243, CI Pigment Red 245, CI Pigment Red 254, CI Pigment Red 255, CI Pigment Red 264 , CI Pigment Red 265;
C.I.顏料藍15、C.I.顏料藍15:3、C.I.顏料藍15:4、C.I.顏料藍15:6、C.I.顏料藍60;C.I.顏料綠7、C.I.顏料綠36;C.I.顏料棕23、C.I.顏料棕25、C.I.顏料黑1、C.I.顏料黑7。CI Pigment Blue 15, CI Pigment Blue 15:3, CI Pigment Blue 15:4, CI Pigment Blue 15:6, CI Pigment Blue 60; CI Pigment Green 7, CI Pigment Green 36; CI Pigment Brown 23, CI Pigment Brown 25 , CI Pigment Black 1, CI Pigment Black 7.
又,前述無機顏料或體質顏料的具體例可列舉氧化鈦、硫酸鋇、碳酸鈣、鉛白、硫酸鉛、黃色鉛、紅色氧化鐵(紅色氧化鐵(III))、鎘紅、群青、紺青、氧化鉻綠、鈷綠、琥珀、鈦黑、合成鐵黑、碳黑等。於本發明中,顏料可單獨或混合使用二種以上。Further, specific examples of the inorganic pigment or the extender pigment include titanium oxide, barium sulfate, calcium carbonate, lead white, lead sulfate, yellow lead, red iron oxide (red iron oxide (III)), cadmium red, ultramarine blue, indigo, Chromium oxide green, cobalt green, amber, titanium black, synthetic iron black, carbon black, and the like. In the present invention, the pigment may be used alone or in combination of two or more.
於形成畫素之情形中,將顏料相對於噴墨油墨之固形成分全量,通常為以1~60重量%、較佳為以15~40重量%之比例配合。顏料若過少,則恐噴墨油墨對指定膜厚(通常為0.1~2.0μm)塗佈時的穿透濃度不夠充分。又,顏料若過多,則噴墨油墨對基板上塗佈硬化時之對於基板的密合性、硬化膜之表面粗糙、塗膜硬度等之塗膜特性恐不夠充分。In the case of forming a pixel, the pigment is formed in a solid amount relative to the inkjet ink, and is usually blended at a ratio of 1 to 60% by weight, preferably 15 to 40% by weight. If the amount of the pigment is too small, it is feared that the penetration density of the inkjet ink at the time of coating a predetermined film thickness (usually 0.1 to 2.0 μm) is insufficient. In addition, if the amount of the pigment is too large, the coating properties of the inkjet ink on the substrate, such as the adhesion to the substrate, the surface roughness of the cured film, and the hardness of the coating film, may not be sufficient.
本發明所用之顏料分散液的溶劑為根據噴墨裝置的印刷適性而選擇。較佳為由沸點200℃以上、更佳為由240℃以上之溶劑中選擇。經由前述溶劑的沸點為200℃,具有適度的乾燥性及蒸發性,故由噴頭吐出時的直進性、安定性優良,可更有效率乾燥,且著彈的油墨滴可輕易廣泛濕潤性油墨層形成區域全體的各個角落。其結果,即使對於多樣化之基板,亦可令著彈之油墨廣泛濕潤至黑色矩陣的邊緣為止,可防止畫素的脫色和亮度降低。沸點若未滿200℃則於管嘴附近的乾燥性顯著降低,其結果有時導致管嘴堵塞等之不良情況發生。The solvent of the pigment dispersion used in the present invention is selected in accordance with the printability of the ink jet apparatus. It is preferably selected from solvents having a boiling point of 200 ° C or higher, more preferably 240 ° C or higher. Since the boiling point of the solvent is 200° C., and has moderate drying property and evaporability, it is excellent in straightness and stability when discharged from the head, and can be dried more efficiently, and the ink droplets can be easily wetted by the ink layer. Form all corners of the entire area. As a result, even for a variety of substrates, the ink of the bomb can be widely wetted to the edge of the black matrix, and the discoloration and brightness reduction of the pixels can be prevented. When the boiling point is less than 200 ° C, the drying property in the vicinity of the nozzle is remarkably lowered, and as a result, problems such as clogging of the nozzle may occur.
又,前述溶劑以使用表面張力範圍為25~35mN/m者為佳,且更佳為26~32mN/m者。表面張力若過高,則對於噴墨吐出時之點形狀的安定性造成顯著不良影響,或者於間隔部間隙內發生油墨不會濕潤擴展的決定。表面張力若過低,則對於噴墨吐出時之點形狀的安定性造成顯著不良影響,或者發生油墨超越間隔部且擴散混色之可能性變高的缺點。Further, the solvent is preferably a surface tension of 25 to 35 mN/m, and more preferably 26 to 32 mN/m. If the surface tension is too high, the stability of the dot shape at the time of inkjet discharge is remarkably adversely affected, or the ink does not wet and expand in the gap of the spacer. When the surface tension is too low, there is a significant adverse effect on the stability of the dot shape at the time of inkjet discharge, or a possibility that the ink passes over the spacer and the possibility of diffusing color mixture becomes high.
滿足此些條件的溶劑,具體而言,可使用二乙二醇乙醚、二乙二醇正丁醚、二乙二醇正丁醚醋酸酯、二乙二醇己醚、二丙二醇甲醚醋酸酯、二丙二醇正丙醚、二丙二醇正丁醚等。又,視需要可將二種以上之溶劑配合前述條件混合,且調整供使用。其中特佳溶劑可列舉二丙二醇甲醚醋酸酯、二乙二醇正丁醚醋酸酯。A solvent satisfying such conditions, specifically, diethylene glycol diethyl ether, diethylene glycol n-butyl ether, diethylene glycol n-butyl ether acetate, diethylene glycol hexyl ether, dipropylene glycol methyl ether acetate, and the like Propylene glycol n-propyl ether, dipropylene glycol n-butyl ether and the like. Further, two or more kinds of solvents may be mixed as described above, and adjusted for use. Among them, a particularly preferred solvent is dipropylene glycol methyl ether acetate or diethylene glycol n-butyl ether acetate.
於本發明之顏料分散液中,可配合作為其他成分的顏料分散劑、填充劑、黏合聚合物以外的高分子化合物防凝集劑等。In the pigment dispersion liquid of the present invention, a pigment dispersant, a filler, a polymer compound anti-aggregation agent other than the binder polymer, and the like can be blended.
顏料分散劑為令顏料於油墨中良好分散而視需要配合。顏料分散劑例如可使用陽離子系、陰離子系、非離子系、兩性、聚矽氧系、氟系等之界面活性劑。界面活性劑中亦以如下例示之高分子界面活性劑(高分子分散劑)為佳。即,以聚氧乙烯月桂醚、聚氧乙烯硬脂醚、聚氧乙烯油醚等之聚氧乙烯烷醚類;聚氧乙烯辛基苯醚、聚氧乙烯壬基苯醚等之聚氧乙烯烷基苯醚類;聚乙二醇二月桂酸酯、聚乙二醇二硬酸酯等之聚乙二醇二酯類;山梨糖醇酐脂肪酸酯類;脂肪酸改性聚酯類;三級胺改性聚胺基甲酸酯類等之高分子界面活性劑為較佳使用。The pigment dispersant is such that the pigment is well dispersed in the ink and optionally blended. As the pigment dispersant, for example, a surfactant such as a cationic system, an anionic system, a nonionic system, an amphoteric, a polyfluorene-based or a fluorine-based surfactant can be used. Among the surfactants, a polymer surfactant (polymer dispersant) exemplified below is also preferred. That is, a polyoxyethylene alkyl ether such as polyoxyethylene lauryl ether, polyoxyethylene stearyl ether or polyoxyethylene oleyl ether; polyoxyethylene such as polyoxyethylene octyl phenyl ether or polyoxyethylene decyl phenyl ether; Alkyl phenyl ethers; polyethylene glycol diesters such as polyethylene glycol dilaurate, polyethylene glycol distearate; sorbitan fatty acid esters; fatty acid modified polyesters; A polymer surfactant such as an amine-modified polyurethane is preferably used.
本發明之透明樹脂溶液塗佈步驟所用之透明樹脂溶液至少由透明樹脂成分和溶劑所構成,視需要配合其他成分。透明樹脂成分可列舉光硬化型樹脂組成物、熱硬化型樹脂組成物等。The transparent resin solution used in the coating step of the transparent resin solution of the present invention is composed of at least a transparent resin component and a solvent, and other components are blended as needed. Examples of the transparent resin component include a photocurable resin composition, a thermosetting resin composition, and the like.
光硬化型樹脂組成物為由分子量較高之聚合物(高分子量聚合物),具有2個以上光聚合性官能基的多官能單體、低聚物、具有2個光聚合性官能基之二官能單體、具有1個光聚合性官能基之單官能單體和經由光活化之光聚合啟始劑所構成。又,亦可配合較低黏度之反應性單體作為反應性稀釋劑。其他之添加劑可列舉例如,填充劑、黏合聚合物以外之高分子化合物、界面活性劑、密合促進劑、防凝集劑、有機酸、硬化劑等。界面活性劑可列舉例如,非離子系界面活性劑、陽離子系界面活性劑、陰離子系界面活性劑及兩性界面活性劑等。The photocurable resin composition is a polymer having a relatively high molecular weight (high molecular weight polymer), a polyfunctional monomer having two or more photopolymerizable functional groups, an oligomer, and two photopolymerizable functional groups. A functional monomer, a monofunctional monomer having one photopolymerizable functional group, and a photopolymerization initiator via photoactivation. Further, a reactive monomer having a lower viscosity may be blended as a reactive diluent. Examples of the other additives include a filler, a polymer compound other than the binder polymer, a surfactant, an adhesion promoter, an anti-agglomerating agent, an organic acid, a curing agent, and the like. Examples of the surfactant include a nonionic surfactant, a cationic surfactant, an anionic surfactant, and an amphoteric surfactant.
所謂分子量較高的聚合物(高分子量聚合物),係指比所謂之單體和低聚物更高分子量者,大致標準為重量平均分子量5,000以上。前述聚合物可使用其本身為無聚合反應性之聚合物,及,其本身為具有聚合反應系之聚合物之任一者,又,亦可組合使用二種以上。The polymer having a relatively high molecular weight (high molecular weight polymer) means a higher molecular weight than the so-called monomer and oligomer, and the approximate standard is a weight average molecular weight of 5,000 or more. The polymer may be any polymer which is not polymerizable, and may be any polymer having a polymerization reaction system, or two or more kinds thereof may be used in combination.
前述聚合物相對於透明樹脂溶液之固形成分全量,通常,以1~50重量%之比例配合。此處,所謂特定配合比例之油墨的固形成分,包含除了溶劑的全部成分,且液狀之聚合性單體等亦被包含於固形成分。The solid content of the polymer relative to the transparent resin solution is usually a ratio of 1 to 50% by weight. Here, the solid content of the ink in a specific blending ratio includes all components other than the solvent, and a liquid polymerizable monomer or the like is also contained in the solid component.
於本發明中,於彩色濾光片用透明樹脂溶液中,配合分子量較高的聚合物。其中,以本身具有聚合反應性聚合物的低聚物,於市場中最容易取得,例如,可例示酯丙烯酸酯類、醚丙烯酸酯類、胺基甲酸酯丙烯酸酯類、環氧丙烯酸酯類、胺基樹脂丙烯酸酯類、丙烯酸系樹脂丙烯酸酯類、不飽和聚酯類等。In the present invention, a polymer having a relatively high molecular weight is blended in a transparent resin solution for a color filter. Among them, an oligomer having a polymerizable reactive polymer itself is most easily obtained in the market, and examples thereof include ester acrylates, ether acrylates, urethane acrylates, and epoxy acrylates. Amino resin acrylates, acrylic resin acrylates, unsaturated polyesters, and the like.
為了令本發明油墨之黏度不會過高且不會對噴頭之吐出性造成不良影響上,使用作為本身具有聚合反應性之聚合物之含有乙烯性雙鍵化合物的分子量,以重量平均分子量為25,000以下為佳。In order to prevent the viscosity of the ink of the present invention from being excessively high and not adversely affecting the discharge property of the head, the molecular weight of the ethylenic double bond-containing compound which is a polymer having polymerization reactivity itself is used, and the weight average molecular weight is 25,000. The following is better.
本身無聚合反應性之聚合物可使用例如,下列二種以上單體所構成的共聚物:丙烯酸、甲基丙烯酸、丙烯酸甲酯、甲基丙烯酸甲酯、丙烯酸2-羥乙酯、甲基丙烯酸2-羥乙酯、丙烯酸苄酯、甲基丙烯酸苄酯、苯乙烯、聚苯乙烯巨大單體、及聚甲基丙烯酸甲酯巨大單體。As the polymer which is not polymerizable by itself, for example, a copolymer composed of two or more kinds of monomers: acrylic acid, methacrylic acid, methyl acrylate, methyl methacrylate, 2-hydroxyethyl acrylate, methacrylic acid can be used. 2-Hydroxyethyl ester, benzyl acrylate, benzyl methacrylate, styrene, polystyrene macromonomer, and polymethyl methacrylate macromonomer.
更具體而言,可使用丙烯酸/丙烯酸苄酯共聚物、丙烯酸/丙烯酸甲酯/苯乙烯共聚物、丙烯酸/丙烯酸苄酯/苯乙烯共聚物、丙烯酸/丙烯酸甲酯/聚苯乙烯巨大單體共聚物、丙烯酸/丙烯酸甲酯/聚甲基丙烯酸甲酯巨大單體共聚物、丙烯酸/丙烯酸苄酯/聚苯乙烯巨大單體共聚物、丙烯酸/丙烯酸苄酯/聚甲基丙烯酸甲酯巨大單體共聚物、丙烯酸/丙烯酸2-羥乙酯/丙烯酸苄酯/聚苯乙烯巨大單體共聚物、丙烯酸/丙烯酸2-羥乙酯/丙烯酸苄酯/聚甲基丙烯酸甲酯巨大單體共聚物、丙烯酸/甲基丙烯酸苄酯共聚物、丙烯酸/甲基丙烯酸甲酯/苯乙烯共聚物、丙烯酸/甲基丙烯酸苄酯/苯乙烯共聚物、丙烯酸/甲基丙烯酸甲酯/聚苯乙烯巨大單體共聚物、丙烯酸/甲基丙烯酸甲酯/聚甲基丙烯酸甲酯巨大單體共聚物、丙烯酸/甲基丙烯酸苄酯/聚苯乙烯巨大單體共聚物、丙烯酸/甲基丙烯酸苄酯/聚甲基丙烯酸甲酯巨大單體共聚物、丙烯酸/甲基丙烯酸2-羥乙酯/甲基丙烯酸苄酯/聚苯乙烯巨大單體共聚物、丙烯酸/甲基丙烯酸2-乙酯/甲基丙烯酸苄酯/聚甲基丙烯酸甲酯巨大單體共聚物等之丙烯酸共聚物類。More specifically, acrylic acid/benzyl acrylate copolymer, acrylic acid/methyl acrylate/styrene copolymer, acrylic acid/benzyl acrylate/styrene copolymer, acrylic acid/methyl acrylate/polystyrene macromonomer copolymerization may be used. , acrylic acid / methyl acrylate / polymethyl methacrylate huge monomer copolymer, acrylic acid / benzyl acrylate / polystyrene giant monomer copolymer, acrylic acid / benzyl acrylate / polymethyl methacrylate huge monomer Copolymer, acrylic acid / 2-hydroxyethyl acrylate / benzyl acrylate / polystyrene giant monomer copolymer, acrylic acid / 2-hydroxyethyl acrylate / benzyl acrylate / polymethyl methacrylate huge monomer copolymer, Acrylic/benzyl methacrylate copolymer, acrylic acid/methyl methacrylate/styrene copolymer, acrylic acid/benzyl methacrylate/styrene copolymer, acrylic acid/methyl methacrylate/polystyrene giant monomer Copolymer, acrylic acid / methyl methacrylate / polymethyl methacrylate huge monomer copolymer, acrylic acid / benzyl methacrylate / polystyrene giant monomer copolymer, acrylic / methacrylic acid Ester/polymethyl methacrylate huge monomer copolymer, acrylic acid / 2-hydroxyethyl methacrylate / benzyl methacrylate / polystyrene giant monomer copolymer, acrylic acid / 2-ethyl methacrylate / Acrylic copolymers such as benzyl methacrylate/polymethyl methacrylate macromonomer copolymer.
若繼續列出具體例,則可列舉甲基丙烯酸/丙烯酸苄酯共聚物、甲基丙烯酸/丙烯酸甲酯/苯乙烯共聚物、甲基丙烯酸/丙烯酸苄酯/苯乙烯共聚物、甲基丙烯酸/丙烯酸甲酯/聚苯乙烯巨大單體共聚物、甲基丙烯酸/丙烯酸甲酯/聚甲基丙烯酸甲酯巨大單體共聚物、甲基丙烯酸/丙烯酸苄酯/聚苯乙烯巨大單體共聚物、甲基丙烯酸/丙烯酸苄酯/聚甲基丙烯酸甲酯巨大單體共聚物、甲基丙烯酸/丙烯酸2-羥乙酯/丙烯酸苄酯/聚苯乙烯巨大單體共聚物、甲基丙烯酸/丙烯酸2-羥乙酯/丙烯酸苄酯/聚甲丙烯酸甲酯巨大單體共聚物、甲基丙烯酸/甲基丙烯酸苄酯共聚物、甲基丙烯酸/丙烯酸甲酯/苯乙烯共聚物、甲基丙烯酸/甲基丙烯酸苄酯/苯乙烯共聚物、甲基丙烯酸/甲基丙烯酸甲酯/聚苯乙烯巨大單體共聚物、甲基丙烯酸/甲基丙烯酸甲酯/聚甲基丙烯酸甲酯巨大單體共聚物、甲基丙烯酸/甲基丙烯酸苄酯/聚苯乙烯巨大單體共聚物、甲基丙烯酸/甲基丙烯酸苄酯/甲基丙烯酸甲酯巨大單體共聚物、甲基丙烯酸/甲基丙烯酸2-羥乙酯/甲基丙烯酸苄酯/聚苯乙烯巨大單體共聚物、甲基丙烯酸/甲基丙烯酸2-羥乙酯/甲基丙烯酸苄酯/聚甲基丙烯酸甲酯巨大單體共聚物等之甲基丙烯酸共聚物類等。If specific examples continue to be listed, methacrylic acid/benzyl acrylate copolymer, methacrylic acid/methyl acrylate/styrene copolymer, methacrylic acid/benzyl acrylate/styrene copolymer, methacrylic acid/ Methyl acrylate/polystyrene macromonomer copolymer, methacrylic acid/methyl acrylate/polymethyl methacrylate giant monomer copolymer, methacrylic acid/benzyl acrylate/polystyrene macromonomer copolymer, Methacrylic acid / benzyl acrylate / polymethyl methacrylate huge monomer copolymer, methacrylic acid / 2-hydroxyethyl acrylate / benzyl acrylate / polystyrene giant monomer copolymer, methacrylic acid / acrylic acid 2 -Hydroxyethyl ester / benzyl acrylate / polymethyl methacrylate huge monomer copolymer, methacrylic acid / benzyl methacrylate copolymer, methacrylic acid / methyl acrylate / styrene copolymer, methacrylic / armor Benzyl acrylate/styrene copolymer, methacrylic acid/methyl methacrylate/polystyrene macromonomer copolymer, methacrylic acid/methyl methacrylate/polymethyl methacrylate macromonomer copolymer ,methyl Acrylic acid/benzyl methacrylate/polystyrene macromonomer copolymer, methacrylic acid/benzyl methacrylate/methyl methacrylate huge monomer copolymer, methacrylic acid/2-acrylic acid 2-hydroxyethyl Ester / benzyl methacrylate / polystyrene giant monomer copolymer, methacrylic acid / 2-hydroxyethyl methacrylate / benzyl methacrylate / polymethyl methacrylate huge monomer copolymer Acrylic copolymers and the like.
於本發明中,於前述透明樹脂溶液中,配合多官能單體。自以往,為了提高光硬化性組成物硬化所得之硬化層的膜強度和對於基板之密合性,乃於光硬化性組成物中配合具有2個以上聚合性官能基的單體(多官能單體),而為了取得充分的膜強度和密合性,通常使用3官能以上的多官能單體。In the present invention, a polyfunctional monomer is blended in the aforementioned transparent resin solution. In order to improve the film strength of the hardened layer obtained by curing the photocurable composition and the adhesion to the substrate, a monomer having two or more polymerizable functional groups is added to the photocurable composition (multifunctional single) In order to obtain sufficient film strength and adhesion, a trifunctional or higher polyfunctional monomer is usually used.
但是,若將多官能基數自大的多官能單體,配合於光硬化性組成物並以噴墨方式吹送到基板上,則在吹送作業期間,於噴墨噴頭前端部分的油墨乾燥且黏度慢慢變大,油墨的吐出性變差。However, when a polyfunctional monomer having a large number of polyfunctional groups is blended on the substrate by an inkjet method, the ink is dried and the viscosity is slow at the tip end portion of the ink jet head during the blowing operation. The slowness becomes larger, and the discharge property of the ink deteriorates.
多官能單體的配合比例,相對於透明樹脂溶液之固形成分全量,通常,以20~70重量%之比例配合。The mixing ratio of the polyfunctional monomer is usually 20 to 70% by weight based on the total amount of the solid content of the transparent resin solution.
此處,前述多官能單體之配合比例未達全固形成分之20重量%的情形中,塗膜的交聯密度變低,塗膜的耐溶劑性、密合性、硬度差,恐無法取得充分之特性。又,前述多官能單體之配合比例超過全固形成分之70重量%的情形中,油墨組成物(透明樹脂溶液)無法經單體充分稀釋,令油墨黏度由開始變高或於溶劑揮發後變高,恐引起噴墨噴頭的孔堵塞。Here, in the case where the mixing ratio of the polyfunctional monomer is less than 20% by weight of the total solid content, the crosslinking density of the coating film is lowered, and the solvent resistance, adhesion, and hardness of the coating film are poor, and the film may not be obtained. Fully characterized. Further, in the case where the blending ratio of the polyfunctional monomer exceeds 70% by weight of the total solid content, the ink composition (transparent resin solution) cannot be sufficiently diluted with the monomer, so that the viscosity of the ink becomes higher from the beginning or becomes more volatile after the solvent evaporates. High, it may cause the hole of the inkjet nozzle to be blocked.
單官能單體(單官能聚合性化合物)可列舉例如壬苯基卡必醇丙烯酸酯、丙烯酸2-羥基-3-苯氧丙酯、2-乙基乙基卡必醇丙烯酸酯、丙烯酸2-羥乙酯、N-乙烯基吡咯烷酮等。The monofunctional monomer (monofunctional polymerizable compound) may, for example, be decyl carbitol acrylate, 2-hydroxy-3-phenoxypropyl acrylate, 2-ethylethyl carbitol acrylate, or acrylic acid 2- Hydroxyethyl ester, N-vinylpyrrolidone, and the like.
具有2個以上光聚合性官能基之多官能單體,可列舉2官能單體和3官能以上之多官能單體。Examples of the polyfunctional monomer having two or more photopolymerizable functional groups include a bifunctional monomer and a trifunctional or higher polyfunctional monomer.
2官能單體可列舉例如,1,6-己二醇二丙烯酸酯、1,6-己二醇二甲基丙烯酸酯、1,9-壬二醇二丙烯酸酯、1,9-壬二醇二甲基丙烯酸酯、1,10-癸二醇二丙烯酸酯、1,10-癸二醇二甲基丙烯酸酯、乙二醇二丙烯酸酯、乙二醇二甲基丙烯酸酯、羥基特戊酸新戊二醇二丙烯酸酯、羥基特戊酸新戊二醇二甲基丙烯酸酯、聚丁二醇二丙烯酸酯、聚丁二醇二甲基丙烯酸酯、二乙二醇二丙烯酸酯、二乙二醇二甲基丙烯酸酯、三丙二醇二丙烯酸酯、三丙二醇二甲基丙烯酸酯、新戊二醇二丙烯酸酯、新戊二醇二甲基丙烯酸酯、三乙二醇二丙烯酸酯、三乙二醇二甲基丙烯酸酯、聚乙二醇(200)二丙烯酸酯、聚乙二醇(200)二甲基丙烯酸酯、聚乙二醇(400)二丙烯酸酯、聚乙二醇(400)二甲基丙烯酸酯、聚二醇(600)二丙烯酸酯、聚乙二醇(600)二甲基丙烯酸酯、雙酚A之雙(丙烯醯氧乙基)醚、3-甲基戊二醇二丙烯酸酯、3-甲基戊二醇二甲基丙烯酸酯、二羥甲基-三環癸烷二丙烯酸酯、二羥甲基-三環癸烷二甲基丙烯酸酯等。Examples of the bifunctional monomer include 1,6-hexanediol diacrylate, 1,6-hexanediol dimethacrylate, 1,9-nonanediol diacrylate, and 1,9-nonanediol. Dimethacrylate, 1,10-nonanediol diacrylate, 1,10-nonanediol dimethacrylate, ethylene glycol diacrylate, ethylene glycol dimethacrylate, hydroxypivalic acid Neopentyl glycol diacrylate, hydroxypivalic acid neopentyl glycol dimethacrylate, polybutylene glycol diacrylate, polybutylene glycol dimethacrylate, diethylene glycol diacrylate, diethyl Diol dimethacrylate, tripropylene glycol diacrylate, tripropylene glycol dimethacrylate, neopentyl glycol diacrylate, neopentyl glycol dimethacrylate, triethylene glycol diacrylate, triethyl Glycol dimethacrylate, polyethylene glycol (200) diacrylate, polyethylene glycol (200) dimethacrylate, polyethylene glycol (400) diacrylate, polyethylene glycol (400) Dimethacrylate, polyglycol (600) diacrylate, polyethylene glycol (600) dimethacrylate, bisphenol A bis(propylene oxiranyl) ether, 3-methyl pentyl Glycol diacrylate, 3-methyl-pentanediol dimethacrylate, dimethylol - tricyclodecane diacrylate, dimethylol - tricyclodecane dimethacrylate and the like.
3官能以上之多官能單體可列舉例如,三羥甲基丙烷三丙烯酸酯、三羥甲基丙烷三甲基丙烯酸酯、環氧乙烷改性三甲基丙烷三丙烯酸酯、環氧乙烷改性三甲基丙烷三甲基丙烯酸酯、季戊四醇三丙烯酸酯、季戊四醇三甲基丙烯酸酯、三(2-羥乙基)三聚異氰酸酯三丙烯酸酯、三(2-羥乙基)三聚異氰酸酯三甲基丙烯酸酯、丙氧基化甘油基三丙烯酸酯、丙氧基化甘油基三甲基丙烯酸酯、季戊四醇四丙烯酸酯、季戊四醇四甲基丙烯酸酯、二(三羥甲基)丙烷四丙烯酸酯、二(三羥甲基)丙烷四甲基丙烯酸酯、乙氧基化季戊四醇四丙烯酸酯、乙氧基化季戊四醇四甲基丙烯酸酯、二季戊四醇羥基五丙烯酸酯、二季戊四醇羥基五甲基丙烯酸酯、二季戊四醇六丙烯酸酯、二季戊四醇六甲基丙烯酸酯等。Examples of the trifunctional or higher polyfunctional monomer include trimethylolpropane triacrylate, trimethylolpropane trimethacrylate, ethylene oxide-modified trimethylpropane triacrylate, and ethylene oxide. Modified trimethylpropane trimethacrylate, pentaerythritol triacrylate, pentaerythritol trimethacrylate, tris(2-hydroxyethyl)trimeric isocyanate triacrylate, tris(2-hydroxyethyl)trimeric isocyanate Trimethacrylate, propoxylated glyceryl triacrylate, propoxylated glyceryl trimethacrylate, pentaerythritol tetraacrylate, pentaerythritol tetramethacrylate, bis(trimethylol)propane tetraacrylic acid Ester, bis(trimethylol)propane tetramethacrylate, ethoxylated pentaerythritol tetraacrylate, ethoxylated pentaerythritol tetramethacrylate, dipentaerythritol hydroxypentaacrylate, dipentaerythritol hydroxypentamethacrylic acid Ester, dipentaerythritol hexaacrylate, dipentaerythritol hexamethacrylate, and the like.
所謂「反應性稀釋劑」,係指分子中於分子末端具有1個以上雙鍵之反應基的單體。反應性稀釋劑可列舉例如,單官能之己內酯丙烯酸酯、丙烯酸十三烷酯、丙烯酸異癸酯、丙烯酸異辛酯、丙烯酸異肉豆蔻酯、丙烯酸異硬脂酯、二乙二醇丙烯酸2-乙基己酯、丙烯酸2-羥丁酯、2-丙烯醯氧乙基六氫酞酸、新戊二醇丙烯酸苯甲酸酯、丙烯酸異戊酯、丙烯酸月桂酯、丙烯酸硬脂酯、丙烯酸丁氧乙酯、乙氧基-二乙二醇丙烯酸酯、甲氧基-三乙二醇丙烯酸酯、甲氧基-聚乙二醇丙烯酸酯、甲氧基二丙二醇丙烯酸酯、丙烯酸苯氧乙酯、苯氧基-聚乙二醇丙烯酸酯、壬基苯酚環氧乙烷加成物丙烯酸酯、丙烯酸四氫糠酯、丙烯酸異冰片酯、丙烯酸2-羥乙酯、丙烯酸2-羥丙酯、丙烯酸2-羥基-3-苯氧丙酯、琥珀酸2-丙烯醯氧乙酯、酞酸2-丙烯醯氧乙酯、酞酸2-丙烯醯氧乙基-2-羥乙酯。The "reactive diluent" refers to a monomer having a reactive group having one or more double bonds at the molecular terminal in the molecule. The reactive diluent may, for example, be monofunctional caprolactone acrylate, tridecyl acrylate, isodecyl acrylate, isooctyl acrylate, isomyristyl acrylate, isostearyl acrylate, diethylene glycol acrylic acid. 2-ethylhexyl ester, 2-hydroxybutyl acrylate, 2-propenyl oxiranyl hexahydrophthalic acid, neopentyl glycol acrylate, isoamyl acrylate, lauryl acrylate, stearyl acrylate, Butyloxyethyl acrylate, ethoxy-diethylene glycol acrylate, methoxy-triethylene glycol acrylate, methoxy-polyethylene glycol acrylate, methoxydipropylene glycol acrylate, phenoxy acrylate Ethyl ester, phenoxy-polyethylene glycol acrylate, nonylphenol ethylene oxide adduct acrylate, tetrahydrofurfuryl acrylate, isobornyl acrylate, 2-hydroxyethyl acrylate, 2-hydroxy propyl acrylate Ester, 2-hydroxy-3-phenoxypropyl acrylate, 2-propenyloxyethyl succinate, 2-propenyloxyethyl phthalate, 2-propenyl oxiranyl 2-hydroxyethyl phthalate.
光聚合啟始劑為考慮較高分子量之聚合物、多官能單體、2官能單體和單官能單體之反應形式的不同(例如自由基聚合和陽離子聚合等),和各材料之種類而適當選擇,為了令著色的油墨硬化,視需要添加。The photopolymerization initiator is a reaction form considering a higher molecular weight polymer, a polyfunctional monomer, a bifunctional monomer, and a monofunctional monomer (for example, radical polymerization and cationic polymerization, etc.), and types of materials. Appropriately selected, in order to harden the colored ink, add it as needed.
光聚合啟始劑可列舉經由光和熱發生活性自由基的活性自由基發生劑。光聚合啟始劑可列舉例如乙醯苯系化合物、苯偶姻系化合物、二苯酮系化合物、噻噸酮系化合物、三嗪系化合物等。The photopolymerization initiator may be an active radical generator which generates active radicals via light and heat. Examples of the photopolymerization initiator include an acetophenone-based compound, a benzoin-based compound, a benzophenone-based compound, a thioxanthone-based compound, and a triazine-based compound.
乙醯苯系化合物可列舉例如,二乙氧基乙醯苯、2-羥基-2-甲基-1-苯基丙烷-1-酮、苄基二甲基縮酮、2-羥基-2-甲基-1-[4-(2-羥乙氧基)苯基]丙烷-1-酮、1-羥基環己基苯基酮、2-甲基-2-嗎啉基-1-(4-甲硫苯基)丙烷-1-酮、2-苄基-2-二甲胺基-1-(4-嗎啉苯基)丁烷-1-酮、2-羥基-2-甲基-1-[4-(1-甲基乙烯基)苯基]丙烷-1-酮之低聚物等。Examples of the acetophenone-based compound include diethoxyacetamidine, 2-hydroxy-2-methyl-1-phenylpropan-1-one, benzyldimethylketal, and 2-hydroxy-2-. Methyl-1-[4-(2-hydroxyethoxy)phenyl]propan-1-one, 1-hydroxycyclohexyl phenyl ketone, 2-methyl-2-morpholinyl-1-(4- Methylthiophenyl)propan-1-one, 2-benzyl-2-dimethylamino-1-(4-morpholinylphenyl)butan-1-one, 2-hydroxy-2-methyl-1 - oligomer of [4-(1-methylvinyl)phenyl]propan-1-one, and the like.
苯偶姻系化合物可列舉例如,苯偶姻、苯偶姻甲醚、苯偶姻乙醚、苯偶姻異丙醚、苯偶姻異丁醚等。Examples of the benzoin-based compound include benzoin, benzoin methyl ether, benzoin ethyl ether, benzoin isopropyl ether, and benzoin isobutyl ether.
二苯酮系化合物可列舉例如,二苯酮、鄰-苯甲醯苯甲酸甲酯、4-苯基二苯酮、4-苯甲醯-4’-甲基二硫苯、3,3’,4,4’-四(第三丁基過氧羰基)二苯酮、2,4,6-三甲基二苯酮等。Examples of the benzophenone-based compound include benzophenone, methyl ortho-benzoic acid benzoate, 4-phenylbenzophenone, 4-benzylidene-4'-methyldithiobenzene, and 3,3'. 4,4'-tetrakis(t-butylperoxycarbonyl)benzophenone, 2,4,6-trimethylbenzophenone and the like.
噻噸酮系化合物可列舉例如,2-異丙基噻噸酮、4-異丙基噻噸酮、2,4-二乙基噻噸酮、2,4-二氯基噻噸酮、1-氯基-4-丙氧基噻噸酮等。Examples of the thioxanthone-based compound include 2-isopropylthioxanthone, 4-isopropylthioxanthone, 2,4-diethylthioxanthone, 2,4-dichlorothioxanthone, and 1 -Chloro-4-propoxythioxanthone and the like.
三嗪系化合物可列舉例如,2,4-雙(三氯甲基)-6-(4-甲氧苯基)-1,3,5-三嗪、2,4-雙(三氯甲基)-6-(4-甲氧萘基)-1,3,5-三嗪、2,4-雙(三氯甲基)-6-胡椒基-1,3,5-三嗪、2,4-雙(三氯甲基)-6-(4-甲氧基苯乙烯基)-1,3,5-三嗪、2,4-雙(三氯甲基)-6-[2-(5-甲基呋喃-2-基)乙烯基]-1,3,5-三嗪、2,4-雙(三氯甲基)-6-[2-(呋喃-2-基)乙烯基]-1,3,5-三嗪、2,4-雙(三氯甲基)-6-[2-(4-二乙胺基-2-甲基苯基)乙烯基]-1,3,5-三嗪、2,4-雙(三氯甲基)-6-[2-(3,4-二甲氧苯基)乙烯基]-1,3,5-三嗪等。The triazine-based compound may, for example, be 2,4-bis(trichloromethyl)-6-(4-methoxyphenyl)-1,3,5-triazine or 2,4-bis(trichloromethyl). - 6-(4-methoxynaphthyl)-1,3,5-triazine, 2,4-bis(trichloromethyl)-6-piperidin-1,3,5-triazine, 2, 4-bis(trichloromethyl)-6-(4-methoxystyryl)-1,3,5-triazine, 2,4-bis(trichloromethyl)-6-[2-( 5-methylfuran-2-yl)vinyl]-1,3,5-triazine, 2,4-bis(trichloromethyl)-6-[2-(furan-2-yl)vinyl] -1,3,5-triazine, 2,4-bis(trichloromethyl)-6-[2-(4-diethylamino-2-methylphenyl)vinyl]-1,3, 5-triazine, 2,4-bis(trichloromethyl)-6-[2-(3,4-dimethoxyphenyl)vinyl]-1,3,5-triazine, and the like.
活性自由基發生劑亦可使用例如,2,4,6-三甲基苯甲醯二苯基氧化膦、2,2’-雙(鄰-氯苯基)-4,4’,5,5’-四苯基-1,2’-雙咪唑、10-丁基-2-氯基吖啶酮、2-乙基蒽醌、苄基、9,10-菲醌、樟腦醌、苯基乙醛酸甲酯、二茂鈦化合物等。As the active radical generator, for example, 2,4,6-trimethylbenzimidium diphenylphosphine oxide, 2,2'-bis(o-chlorophenyl)-4,4',5,5 can also be used. '-Tetraphenyl-1,2'-bisimidazole, 10-butyl-2-chloroacridone, 2-ethylhydrazine, benzyl, 9,10-phenanthrenequinone, camphorquinone, phenylethyl Methyl aldehyde, titanium titanate, and the like.
活性自由基發生劑亦可使用市售物質。市售之聚合啟始劑可列舉例如,商品名「Irgacure-369」(乙醯苯系光聚合啟始劑、Ciba Specialty Chemicals公司製)等。A commercially available substance can also be used as the active radical generator. The commercially available polymerization initiator is, for example, a product name "Irgacure-369" (a phthalic acid photopolymerization initiator, manufactured by Ciba Specialty Chemicals Co., Ltd.).
熱聚合啟始劑可列舉偶氮系化合物、過氧化物系化合物等。偶氮系化合物可列舉2,2’-偶氮雙(4-甲氧基-2,4-二甲基戊腈)、2,2’-偶氮雙(4-甲基-2,4-二甲基戊腈)、2,2’-偶氮雙(2-甲基丙酸)二甲酯、2,2’-偶氮雙(2-甲基丁腈)、1,1’-偶氮雙(環己烷-1-腈)、2,2’-偶氮雙[N-2(丙烯基)-2-甲基-丙醯胺]、1-[(氰基-1-甲基乙基)偶氮]甲醯胺、2,2’-偶氮雙(N-丁基-2-甲基丙醯胺)、2,2’-偶氮雙(N-環己基-2-甲基丙醯胺)、含有聚二甲基矽氧烷次單元之高分子偶氮聚合啟始劑(和光純藥工業、VPS系列)、含有聚乙二醇單元之高分子聚合啟始劑(和光純藥工業、VPE系列)等。Examples of the thermal polymerization initiator include an azo compound and a peroxide compound. Examples of the azo compound include 2,2'-azobis(4-methoxy-2,4-dimethylvaleronitrile) and 2,2'-azobis(4-methyl-2,4- Dimethylvaleronitrile), 2,2'-azobis(2-methylpropionic acid) dimethyl ester, 2,2'-azobis(2-methylbutyronitrile), 1,1'-even Nitrogen bis(cyclohexane-1-carbonitrile), 2,2'-azobis[N-2(propenyl)-2-methyl-propanamide], 1-[(cyano-1-methyl) Ethyl)azo]carbamamine, 2,2'-azobis(N-butyl-2-methylpropionamide), 2,2'-azobis(N-cyclohexyl-2-methyl) Propylamine, a polymeric azo polymerization initiator containing a polydimethylsiloxane subunit (Wako Pure Chemical Industries, VPS series), a polymeric polymerization initiator containing polyethylene glycol units (and Guangchun Pharmaceutical Industry, VPE Series), etc.
過氧化物化合物可列舉過氧基縮酮、過氧化氫、過氧化二烷基、過氧化二醯、過氧基二碳酸酯、過氧基酯。過氧基酯可列舉第三丁基過氧基乳酸酯(日本油脂(股)製、商品名「Perbutyl L」)、第三丁基過氧基-3,5,5-三甲基己酸酯(日本油脂(股)製、商品名「Perbutyl 355」)、第三己基過氧基-異丙基-單碳酸酯(日本油脂(股)製、商品名「Perbutyl I」)等。Examples of the peroxide compound include peroxyketal, hydrogen peroxide, dialkyl peroxide, dioxane peroxide, peroxydicarbonate, and peroxy ester. Examples of the peroxy ester include a tert-butylperoxylactate (manufactured by Nippon Oil Co., Ltd., trade name "Perbutyl L"), and a tert-butylperoxy-3,5,5-trimethyl group. An acid ester (manufactured by Nippon Oil & Fats Co., Ltd., trade name "Perbutyl 355"), a third hexylperoxy-isopropyl-monocarbonate (manufactured by Nippon Oil & Fats Co., Ltd., trade name "Perbutyl I"), and the like.
此等聚合啟始劑可分別單獨或組合使用2種以上。聚合啟始劑之使用量為相對於黏合聚合物及聚合性化合物之合計量100質量份,通常以1質量份以上30質量份以下,較佳為3質量份以上20質量份以下。These polymerization initiators may be used alone or in combination of two or more. The amount of the polymerization initiator to be used is usually 1 part by mass or more and 30 parts by mass or less, preferably 3 parts by mass or more and 20 parts by mass or less based on 100 parts by mass of the total of the binder polymer and the polymerizable compound.
其他之添加劑可列舉例如,填充劑、黏合聚合物以外之高分子化合物、界面活性劑、密合促進劑、防凝集劑、有機酸、硬化劑等。界面活性劑可列舉例如,非離子系界面活性劑、陽離子系界面活性劑、陰離子系界面活性劑及兩性界面活性劑等。密合促進劑可列舉例如,乙烯基三甲氧基矽烷、乙烯基三乙氧基矽烷、乙烯基三(2-甲氧乙氧基)矽烷、N-(2-胺乙基)-3-胺丙基甲基二甲氧基矽烷、N-(2-胺乙基)-3-胺丙基三甲氧基矽烷、3-胺丙基三乙氧基矽烷、3-環氧丙氧丙基三甲氧基矽烷、3-環氧丙氧丙基甲基二甲氧基矽烷、2-(3,1-環氧環己基)乙基三甲氧基矽烷、3-氯丙基甲基二甲氧基矽烷、3-氯丙基三甲氧基矽烷、3-甲基丙烯氧丙基三甲氧基矽烷、3-氫硫丙基三甲氧基矽烷等。Examples of the other additives include a filler, a polymer compound other than the binder polymer, a surfactant, an adhesion promoter, an anti-agglomerating agent, an organic acid, a curing agent, and the like. Examples of the surfactant include a nonionic surfactant, a cationic surfactant, an anionic surfactant, and an amphoteric surfactant. Examples of the adhesion promoter include vinyl trimethoxy decane, vinyl triethoxy decane, vinyl tris(2-methoxyethoxy) decane, and N-(2-aminoethyl)-3-amine. Propylmethyldimethoxydecane, N-(2-aminoethyl)-3-aminopropyltrimethoxydecane, 3-aminopropyltriethoxydecane, 3-glycidoxypropyltrimethyl Oxydecane, 3-glycidoxypropylmethyldimethoxydecane, 2-(3,1-epoxycyclohexyl)ethyltrimethoxydecane, 3-chloropropylmethyldimethoxy Decane, 3-chloropropyltrimethoxydecane, 3-methylpropoxypropyltrimethoxydecane, 3-hydrothiopropyltrimethoxydecane, and the like.
本發明之熱硬化型樹脂組成物其特徵為至少含有熱聚合性黏合劑和2官能至3官能之含有環氧基的單體。於熱硬化型樹脂組成物中,視需要亦可配合著色劑、分散劑、硬化促進劑、或、其他添加劑。又,於熱硬化性透明樹脂組成物,為了賦予適用於噴墨方式的適切流動性、吐出性,亦可將上述各成分於溶劑(稀釋劑)中溶解或分散。又,2官能至3官能之含有環氧基之單體、與4官能以上之含有環氧基之樹脂組合使用亦可。The thermosetting resin composition of the present invention is characterized by comprising at least a thermopolymerizable binder and a bifunctional to trifunctional epoxy group-containing monomer. A coloring agent, a dispersing agent, a hardening accelerator, or other additives may be blended in the thermosetting resin composition as needed. Further, in order to impart suitable fluidity and discharge property to the inkjet method, the thermosetting transparent resin composition may be dissolved or dispersed in a solvent (diluent). Further, a bifunctional to trifunctional epoxy group-containing monomer may be used in combination with a tetrafunctional or higher epoxy group-containing resin.
熱聚合性之黏合劑可使用例如,令如下所示之乙烯性不飽和鍵與1種或2種以上含有環氧基之單體聚合的單聚物或共聚物:丙烯酸縮水甘油酯、甲基丙烯酸縮水甘油酯、α-乙基丙烯酸縮水甘油酯、α-正丙基丙烯酸縮水甘油酯、α-正丁基丙烯酸縮水甘油酯、丙烯酸-3,4-環氧丁酯、甲基丙烯酸-3,4-環氧丁酯、甲基丙烯酸-4,5-環氧戊酯、丙烯酸-6,7-環氧庚酯、甲基丙烯酸-6,7-環氧庚酯、α-乙基丙烯酸-6,7-環氧庚酯等之(甲基)丙烯酸酯類;鄰-乙烯苯基縮水甘油醚、間-乙烯苯基縮水甘油醚、對-乙烯苯基縮水甘油醚、鄰-乙烯苄基縮水甘油醚、間-乙烯苄基縮水甘油醚、對-乙烯苄基縮水甘油醚等之乙烯基縮水甘油醚類;2,3-二環氧丙氧基苯乙烯、3,4-二環氧丙氧基苯乙烯、2,4-二環氧丙氧基苯乙烯、3,5-二環氧丙氧基苯乙烯、2,6-二環氧丙氧基苯乙烯、5-乙烯基焦棓酚三縮水甘油醚、4-乙烯基焦棓酚三縮水甘油醚、乙烯基氟基甘胺醇三縮水甘油醚、2,3-二羥甲基苯乙烯二縮水甘油醚、3,4-二羥甲基苯乙烯二縮水甘油醚、2,4-二羥甲基苯乙烯二縮水甘油醚、3,5-二羥甲基苯乙烯二縮水甘油醚、2,6-二羥甲基苯乙烯二縮水甘油醚、2,3,4-三羥甲基苯乙烯三縮水甘油醚、及、1,3,5-三羥甲基苯乙烯三縮水甘油醚。As the binder for the thermal polymerization, for example, a monomer or a copolymer obtained by polymerizing an ethylenically unsaturated bond shown below with one or more epoxy group-containing monomers: glycidyl acrylate, methyl group can be used. Glycidyl acrylate, glycidyl α-ethyl acrylate, glycidyl α-n-propyl acrylate, glycidyl α-n-butyl acrylate, 3,4-butyl butyl acrylate, methacrylic acid-3 , 4-epoxybutyl acrylate, methacrylic acid-4,5-epoxypentyl acrylate, acrylate-6,7-epoxyheptyl ester, methacrylic acid-6,7-epoxyheptyl ester, α-ethyl acrylate (meth) acrylates such as -6,7-epoxyheptyl ester; o-vinyl phenyl glycidyl ether, m-vinyl phenyl glycidyl ether, p-vinyl phenyl glycidyl ether, o-vinyl benzyl ether Vinyl glycidyl ethers such as glycidyl ether, m-vinylbenzyl glycidyl ether, p-vinylbenzyl glycidyl ether, etc.; 2,3-diepoxypropoxystyrene, 3,4-bicyclo Oxypropoxystyrene, 2,4-diepoxypropoxystyrene, 3,5-diepoxypropoxystyrene, 2,6-diepoxypropoxystyrene, 5-vinyl Pyrogallol triple shrinkage Oleic ether, 4-vinylpyrrolol triglycidyl ether, vinyl fluoroglycolamine triglycidyl ether, 2,3-dimethylol styrene diglycidyl ether, 3,4-dimethylol Styrene diglycidyl ether, 2,4-dimethylol styrene diglycidyl ether, 3,5-dimethylol styrene diglycidyl ether, 2,6-dimethylol styrene diglycidyl Ether, 2,3,4-trishydroxymethylstyrene triglycidyl ether, and 1,3,5-trishydroxymethylstyrene triglycidyl ether.
又,如上述之乙烯性不飽和鍵和1種或2種以上含有環氧基之單體,與如下述不含有環氧基之單體聚合的共聚物,亦可使用作為熱聚合性之黏合劑:丙烯酸、甲基丙烯酸、丙烯酸甲酯、甲基丙烯酸甲酯、丙烯酸2-羥乙酯、甲基丙烯酸2-羥乙酯、丙烯酸苄酯、甲基丙烯酸苄酯、苯乙烯、聚苯乙烯巨大單體、及聚甲基丙烯酸甲酯巨大單體。Further, the above-mentioned ethylenically unsaturated bond and one or more epoxy group-containing monomers may be copolymerized with a monomer having no epoxy group as described below, and may be used as a thermopolymerizable bond. Agent: acrylic acid, methacrylic acid, methyl acrylate, methyl methacrylate, 2-hydroxyethyl acrylate, 2-hydroxyethyl methacrylate, benzyl acrylate, benzyl methacrylate, styrene, polystyrene Huge monomer, and polymethyl methacrylate huge monomer.
黏合劑相對於熱硬化型樹脂組成物之固形成分全量,通常,以1~50重量%之比例配合。此處,所謂特定配合比例之熱硬化型樹脂組成物的固形成分,為包含除了溶劑的全部成分,且液狀之聚合性單體亦被包含於固形成分。The binder is usually added in an amount of from 1 to 50% by weight based on the total amount of the solid solution of the thermosetting resin composition. Here, the solid content of the thermosetting resin composition having a specific blending ratio is that all the components other than the solvent are contained, and the liquid polymerizable monomer is also contained in the solid component.
黏合劑之配合量未達上述範圍,則塗膜的耐溶劑性、密合性、硬度差,有時發生無法取得充分特性之缺點。若超過上述範圍,則油墨組成物(透明樹脂溶液)不被單體充分稀釋,且油墨黏度由開始變高或者於溶劑揮發後變高,恐引起噴墨噴頭的孔堵塞。When the amount of the binder is less than the above range, the solvent resistance, adhesion, and hardness of the coating film are inferior, and there is a disadvantage that sufficient characteristics cannot be obtained. When it exceeds the above range, the ink composition (transparent resin solution) is not sufficiently diluted by the monomer, and the viscosity of the ink becomes high from the beginning or becomes high after the solvent evaporates, which may cause clogging of the pores of the ink jet head.
於上述熱硬化型樹脂組成物中,使用1種或組合2種以上2官能至3官能之含有環氧基之單體,作為熱硬化性成分。2官能至3官能之含有環氧基之單體即使為熱硬化性樹脂亦為較低黏度,加上因乾燥而令黏度上升少,故將此類2官能至3官能之含有環氧基之單體使用作為熱硬化成分的油墨,在以噴墨方式吹送之作業中,難引起噴頭前端的黏度上升,不會發生噴頭的孔堵塞,於作業中令油墨的吐出性安定。因此,令油墨的吐出量和吐出方向保持一定,油墨於基板上可如指定圖型般正確,且,均勻附著。In the thermosetting resin composition, one or a combination of two or more bifunctional to trifunctional epoxy group-containing monomers is used as the thermosetting component. Since the bifunctional to trifunctional epoxy group-containing monomer has a lower viscosity even if it is a thermosetting resin, and the viscosity is less increased by drying, such a bifunctional to trifunctional epoxy group-containing monomer is used. When the ink which is a thermosetting component is used as a monomer, it is difficult to cause the viscosity of the tip of the head to rise in the operation of the ink jet method, and the clogging of the nozzle is not caused, and the discharge property of the ink is stabilized during the operation. Therefore, the discharge amount and the discharge direction of the ink are kept constant, and the ink can be properly formed on the substrate as the specified pattern, and uniformly adhered.
2官能至3官能之含有環氧基之單體可例示例如,聚丙二醇二縮水甘油醚、新戊二醇二縮水甘油醚、聚乙二醇二縮水甘油醚、聚丙二醇二縮水甘油醚、三羥甲基丙烷聚縮水甘油醚、2,3-二環氧丙氧基苯乙烯、3,4-二環氧丙氧基苯乙烯、2,4-二環氧丙氧基苯乙烯、3,5-二環氧丙氧基苯乙烯、2,6-二環氧丙氧基苯乙烯、5-乙烯基焦棓酚三縮水甘油醚、4-乙烯基集棓酚三縮水甘油醚、乙烯基氟基甘胺醇三縮水甘油醚、2,3-二羥甲基苯乙烯二縮水甘油醚、3,4-二羥甲基苯乙烯二縮水甘油醚、2,4-二羥甲基苯乙烯二縮水甘油醚、3,5-二羥甲基苯乙烯二縮水甘油醚、2,6-二羥甲基苯乙烯二縮水甘油醚、2,3,4-三羥甲基苯乙烯三縮水甘油醚、1,3,5-三羥甲基苯乙烯三縮水甘油醚等,且其可單獨1種或組合使用2種以上。The bifunctional to trifunctional epoxy group-containing monomer can be exemplified by, for example, polypropylene glycol diglycidyl ether, neopentyl glycol diglycidyl ether, polyethylene glycol diglycidyl ether, polypropylene glycol diglycidyl ether, and the like. Hydroxymethylpropane polyglycidyl ether, 2,3-diepoxypropoxystyrene, 3,4-diepoxypropoxystyrene, 2,4-diepoxypropoxystyrene, 3, 5-diepoxypropoxystyrene, 2,6-diepoxypropoxystyrene, 5-vinylpyrrolol triglycidyl ether, 4-vinylcarboxol triglycidyl ether, vinyl Fluoroglycine alcohol triglycidyl ether, 2,3-dimethylol styrene diglycidyl ether, 3,4-dimethylol styrene diglycidyl ether, 2,4-dimethylol styrene Diglycidyl ether, 3,5-dimethylol styrene diglycidyl ether, 2,6-dimethylol styrene diglycidyl ether, 2,3,4-trishydroxymethyl styrene triglycidyl Ether, 1,3,5-trimethylol styrene triglycidyl ether, etc., may be used alone or in combination of two or more.
2官能至3官能之含有環氧基之單體的配合比例,相對於熱硬化型樹脂組成物之固形成分全量,通常,以20~70重量%之比例配合。The blending ratio of the bifunctional to trifunctional epoxy group-containing monomer is usually 20 to 70% by weight based on the total solid content of the thermosetting resin composition.
此處,2官能至3官能之含有環氧基之單體的配合比例未達全固形成分(溶劑以外之全部成分)的20重量%時,透明樹脂溶液不被單體充分稀釋,且油墨黏度由開始變高或者於溶劑揮發後變高,恐引起噴墨噴頭的孔堵塞。又,2官能至3官能之含有環氧基之單體的配合比例為超過全固形成分之70重量%時,塗膜之交聯密度變低,塗膜之耐溶劑性、密合性、硬度差,恐無法取得充分之特性。Here, when the mixing ratio of the bifunctional to trifunctional epoxy group-containing monomer is less than 20% by weight of the total solid content (all components other than the solvent), the transparent resin solution is not sufficiently diluted by the monomer, and the ink viscosity is It becomes high from the beginning or becomes high after the solvent evaporates, which may cause clogging of the pores of the ink jet head. Further, when the mixing ratio of the bifunctional to trifunctional epoxy group-containing monomer is more than 70% by weight based on the total solid content, the crosslinking density of the coating film is lowered, and the solvent resistance, adhesion, and hardness of the coating film are lowered. Poor, I am afraid I can't get enough features.
又,於熱硬化型樹脂組成物中,上述之2官能至3官能之含有環氧基之單體同時,視需要,亦可配合單官能之含有環氧基之單體、及/或、4官能以上之含有環氧基之樹脂、及/或、含有環氧基之單體以外之熱硬化性成分。Further, in the thermosetting resin composition, the above-mentioned bifunctional to trifunctional epoxy group-containing monomer may be blended with a monofunctional epoxy group-containing monomer, and/or 4, if necessary. A thermosetting component other than the functional group-containing epoxy group-containing resin and/or the epoxy group-containing monomer.
單官能之含有環氧基之單體可例示甲基縮水甘油醚、丁基縮水甘油醚、苯基縮水甘油醚、丁基苯基縮水甘油醚、2-乙基己基縮水甘油醚、癸基縮水甘油醚、硬脂基縮水甘油醚、烯丙基縮水甘油醚、聚丙二醇縮水甘油醚、丁氧基聚乙二醇單縮水甘油醚。The monofunctional epoxy group-containing monomer may, for example, be methyl glycidyl ether, butyl glycidyl ether, phenyl glycidyl ether, butylphenyl glycidyl ether, 2-ethylhexyl glycidyl ether or thiol glycated ether. Glycerol ether, stearyl glycidyl ether, allyl glycidyl ether, polypropylene glycol glycidyl ether, butoxy polyethylene glycol monoglycidyl ether.
又,含有環氧基之單體以外的熱硬化性成分可例示例如,蜜胺樹脂、脲樹脂、醇酸樹脂、酚樹脂、環戊二烯樹脂等。Further, examples of the thermosetting component other than the epoxy group-containing monomer include a melamine resin, a urea resin, an alkyd resin, a phenol resin, and a cyclopentadiene resin.
2官能至3官能之含有環氧基之單體同時,配合4官能以上之含有環氧基之樹脂為佳。熱硬化型樹脂組成物中所配合之含有環氧基成分全部為2官能至3官能之情形中,因為難因油墨乾燥而引起黏度上升,故噴墨噴頭的吐出性安定,但其反面,硬化油墨層所得之硬化層的膜強度和對於基板的密合性有時不夠充分。於是,將上述之2官能至3官能之含有環氧基之單體同時,適量配合4官能以上之含有環氧基之樹脂,則可對硬化層的圖型賦予充分的膜強度和密合性。The bifunctional to trifunctional epoxy group-containing monomer is preferably a tetrafunctional or higher epoxy group-containing resin. In the case where all of the epoxy group-containing components contained in the thermosetting resin composition are bifunctional to trifunctional, since the viscosity is hard to be increased due to drying of the ink, the discharge property of the ink jet head is stable, but the reverse side is hardened. The film strength of the hardened layer obtained by the ink layer and the adhesion to the substrate may not be sufficient. Therefore, when the above-mentioned bifunctional to trifunctional epoxy group-containing monomer is blended in an appropriate amount with a tetrafunctional or higher epoxy group-containing resin, sufficient film strength and adhesion can be imparted to the pattern of the hardened layer. .
4官能以上之含有環氧基之樹脂可使用例如,苯酚酚醛清漆環氧、甲酚酚醛清漆環氧等之酚醛清漆樹脂類、四縮水甘油基二胺基二苯基甲烷、四縮水甘油基間二甲苯二胺等之縮水甘油胺樹脂類、四苯基縮水甘油醚乙烷、三苯基縮水甘油醚甲烷等之縮水甘油醚樹脂類等。For the epoxy group-containing resin having four or more functional groups, for example, a novolac resin such as a phenol novolac epoxy resin, a cresol novolac epoxy resin, a tetraglycidyldiamine diphenylmethane or a tetraglycidyl group can be used. A glycidylamine resin such as xylene diamine or a glycidyl ether resin such as tetraphenyl glycidyl ether ethane or triphenyl glycidyl ether methane.
4官能以上之含有環氧基之樹脂,相對於熱硬化性透明樹脂組成物之固形成分全量,通常,配合1~30重量%之比例為佳。又,為了令2官能至3官能之含有環氧基所造成的吐出性安定化;和4官能以上之含有環氧基之樹脂所提高的強度及密合性平衡,乃相對於2官能至3官能性單體100重量份,令4官能以上之含有環氧基之樹脂的配合比例通常為1~50重量份,較佳令該配合比例之下限為2重量份以上,且/或,該配合比例之上限為35重量份以下。The epoxy group-containing resin having four or more functional groups is preferably added in an amount of from 1 to 30% by weight based on the total solid content of the thermosetting transparent resin composition. Further, in order to stabilize the discharge property due to the bifunctional to trifunctional epoxy group-containing epoxy group, and to improve the strength and adhesion balance of the tetrafunctional or higher epoxy group-containing resin, it is relative to the bifunctional to 3-functional group. 100 parts by weight of the functional monomer, the blending ratio of the epoxy group-containing resin having 4 or more functional groups is usually 1 to 50 parts by weight, preferably the lower limit of the blending ratio is 2 parts by weight or more, and/or the blending ratio The upper limit of the ratio is 35 parts by weight or less.
此處,4官能以上之含有環氧基之樹脂的配合比例,相對於前述2官能至3官能性單體100重量份未達1重量份之情形中,擔心油墨硬化後的硬度、耐溶劑性等之特性無法充分取得。又,4官能以上之含有環氧基之樹脂的前述配合比例為超過50重量份之情形中,擔心油墨的硬化速度變慢,步驟速度變慢。Here, in the case where the blending ratio of the epoxy group-containing resin having four or more functional groups is less than 1 part by weight based on 100 parts by weight of the above-mentioned bifunctional to trifunctional monomer, there is concern about hardness and solvent resistance after curing of the ink. The characteristics of etc. cannot be fully obtained. When the blending ratio of the epoxy group-containing resin having four or more functional groups is more than 50 parts by weight, there is concern that the curing rate of the ink is slow and the step speed is slow.
於本發明所用之熱硬化型樹脂組成物中,通常,配合硬化劑。硬化劑例如使用多價羧酸酐或多價羧酸。In the thermosetting resin composition used in the present invention, a curing agent is usually blended. The hardener is, for example, a polyvalent carboxylic anhydride or a polyvalent carboxylic acid.
多價羧酸酐的具體例可列舉例如酞酸酐、衣康酸酐、琥珀酸酐、檸康酸酐、十二碳烯基琥珀酸酐、丙三羧酸酐、順丁烯二酸酐、六氫酞酸酐、二甲基四氫酞酸酐、海明克酸酐、橋亞甲基四氫化鄰苯二甲酸酐等之脂肪族或脂環族二羧酸酐;1,2,3,4-丁烷四羧酸二酐、環戊烷四羧酸二酐等之脂肪族多價羧酸二酐;均苯四甲酸酐、偏苯三酸酐、二苯酮四羧酸酐等之芳香族多價羧酸酐;乙二醇雙(偏苯三酸鹽)、甘油三(偏苯三酸鹽)等之含有酯基之酸酐,特佳可列舉芳香族多價羧酸酐。又,市售之羧酸酐所構成的環氧樹脂硬化劑亦適於使用。Specific examples of the polyvalent carboxylic acid anhydride include phthalic anhydride, itaconic anhydride, succinic anhydride, citraconic anhydride, dodecenyl succinic anhydride, propylene tricarboxylic anhydride, maleic anhydride, hexahydrophthalic anhydride, and dimethyl An aliphatic or alicyclic dicarboxylic anhydride such as tetrahydrofurfuric anhydride, heiming anhydride, benzylidene tetrahydrophthalic anhydride; 1,2,3,4-butanetetracarboxylic dianhydride, An aliphatic polyvalent carboxylic acid dianhydride such as cyclopentane tetracarboxylic dianhydride; an aromatic polyvalent carboxylic acid anhydride such as pyromellitic anhydride, trimellitic anhydride or benzophenone tetracarboxylic anhydride; ethylene glycol bis(p-benzoate) An acid anhydride-containing acid anhydride such as an acid salt or a triglyceride (trimellitic acid salt) is particularly preferably an aromatic polyvalent carboxylic acid anhydride. Further, an epoxy resin curing agent composed of a commercially available carboxylic anhydride is also suitable for use.
又,本發明所用之多價羧酸的具體可列舉琥珀酸、戊二酸、己二酸、丁烷四羧酸、順丁烯二酸、衣康酸等之脂肪族多價羧酸;六氫酞酸、1,2-環己烷二羧酸、1,2,4-環己烷三羧酸、環戊烷四羧酸等之脂肪族多價羧酸、及酞酸、異酞酸、對酞酸、均苯四甲酸、偏苯三酸、1,4,5,8-萘四羧酸、二苯酮四羧酸等之芳香族多價羧酸,較佳可列舉芳香族多價羧酸。Further, specific examples of the polyvalent carboxylic acid used in the present invention include aliphatic polyvalent carboxylic acids such as succinic acid, glutaric acid, adipic acid, butanetetracarboxylic acid, maleic acid, and itaconic acid; An aliphatic polyvalent carboxylic acid such as hydroquinone, 1,2-cyclohexanedicarboxylic acid, 1,2,4-cyclohexanetricarboxylic acid or cyclopentanetetracarboxylic acid, and citric acid or isophthalic acid The aromatic polyvalent carboxylic acid such as citric acid, pyromellitic acid, trimellitic acid, 1,4,5,8-naphthalenetetracarboxylic acid or benzophenonetetracarboxylic acid is preferably aromatic. Valence carboxylic acid.
此些多價羧酸酐及多價羧酸可單獨1種或混合使用2種以上。本發明所用之硬化劑的配合量為含有環氧基之成分(單體與樹脂)每100重量份,通常為1~100重量份之範圍,較佳為5~50重量份。硬化劑之配合量若未達1重量份,則硬化不足,無法形成強韌的塗膜。又,硬化劑的配合量若超過100重量份,則塗膜對於基板的密合性差,加上無法形成均勻且平滑的塗膜。These polyvalent carboxylic anhydrides and polyvalent carboxylic acids may be used alone or in combination of two or more. The amount of the curing agent used in the present invention is usually from 1 to 100 parts by weight, preferably from 5 to 50 parts by weight, per 100 parts by weight of the epoxy group-containing component (monomer and resin). If the amount of the hardener is less than 1 part by weight, the hardening is insufficient and a tough coating film cannot be formed. In addition, when the amount of the curing agent is more than 100 parts by weight, the adhesion of the coating film to the substrate is inferior, and a uniform and smooth coating film cannot be formed.
其他之添加劑可列舉例如,填充劑、黏合聚合物以外之高分子化合物、界面活性劑、密合促進劑、防凝集劑、有機酸、硬化劑等。界面活性劑可列舉例如,非離子系界面活性劑、陽離子系界面活性劑、陰離子系界面活性劑及兩性界面活性劑等。密合促進劑可列舉例如,乙烯基三甲氧基矽烷、乙烯基三乙氧基矽烷、乙烯基三(2-甲氧乙氧基)矽烷、N-(2-胺乙基)-3-胺丙基甲基二甲氧基矽烷、N-(2-胺乙基)-3-胺丙基三甲氧基矽烷、3-胺丙基三乙氧基矽烷、3-環氧丙氧基三甲氧基矽烷、3-環氧丙氧丙基甲基二甲氧基矽烷、2-(3,4-環氧環己基)乙基三甲氧基矽烷、3-氯丙基甲基二甲氧基矽烷、3-氯丙基三甲氧基矽烷、3-甲基丙烯氧丙基三甲氧基矽烷、3-氫硫丙基三甲氧基矽烷等。Examples of the other additives include a filler, a polymer compound other than the binder polymer, a surfactant, an adhesion promoter, an anti-agglomerating agent, an organic acid, a curing agent, and the like. Examples of the surfactant include a nonionic surfactant, a cationic surfactant, an anionic surfactant, and an amphoteric surfactant. Examples of the adhesion promoter include vinyl trimethoxy decane, vinyl triethoxy decane, vinyl tris(2-methoxyethoxy) decane, and N-(2-aminoethyl)-3-amine. Propylmethyldimethoxydecane, N-(2-aminoethyl)-3-aminopropyltrimethoxydecane, 3-aminopropyltriethoxydecane, 3-epoxypropoxytrimethoxy Baseline, 3-glycidoxypropylmethyldimethoxydecane, 2-(3,4-epoxycyclohexyl)ethyltrimethoxydecane, 3-chloropropylmethyldimethoxydecane , 3-chloropropyltrimethoxydecane, 3-methylpropoxypropyltrimethoxydecane, 3-hydrothiopropyltrimethoxydecane, and the like.
透明樹脂溶液之溶劑為與前述顏料分散液之溶劑同樣,根據噴墨裝置之印刷適性而選擇。較佳為使用沸點為200℃以上之溶劑。又,較佳為使用表面張力範圍為25~35mN/m溶劑。特佳為使用表面張力範圍為25~35mN/m,且沸點為200℃以上之溶劑。沸點若未達200℃,則於管嘴附近的乾燥性顯著變高,其結果有時導致管嘴堵塞等之不良情況發生。又,表面張力若超過35mN/m,則擔心對噴墨吐出時之點形狀的安定性造成顯著的不良影響,於著色層上塗佈時透明樹脂溶液無法濕潤據展至著色層全體的各個角落。The solvent of the transparent resin solution is selected in the same manner as the solvent of the above-mentioned pigment dispersion liquid, depending on the printing suitability of the ink jet apparatus. It is preferred to use a solvent having a boiling point of 200 ° C or higher. Further, it is preferred to use a solvent having a surface tension in the range of 25 to 35 mN/m. It is particularly preferred to use a solvent having a surface tension of 25 to 35 mN/m and a boiling point of 200 ° C or higher. When the boiling point is less than 200 ° C, the drying property in the vicinity of the nozzle is remarkably high, and as a result, problems such as clogging of the nozzle may occur. Further, when the surface tension exceeds 35 mN/m, there is a fear that the stability of the dot shape at the time of inkjet discharge is remarkably adversely affected, and the transparent resin solution cannot be wetted to the entire corner of the colored layer when applied on the colored layer. .
滿足此些條件的溶劑,具體而言,可使用二乙二醇乙醚、二乙二醇正丁醚、二乙二醇正丁醚醋酸酯、二乙二醇己醚、二丙二醇甲醚醋酸酯、二丙二醇正丙醚、二丙二醇正丁醚等。又,視需要可將二種以上之溶劑以配合前述條件般混合、調整供使用。其中最佳者為二丙二醇甲醚醋酸酯、二乙二醇正丁醚醋酸酯。A solvent satisfying such conditions, specifically, diethylene glycol diethyl ether, diethylene glycol n-butyl ether, diethylene glycol n-butyl ether acetate, diethylene glycol hexyl ether, dipropylene glycol methyl ether acetate, and the like Propylene glycol n-propyl ether, dipropylene glycol n-butyl ether and the like. Further, two or more kinds of solvents may be mixed and adjusted for use in accordance with the above conditions as needed. The most preferred ones are dipropylene glycol methyl ether acetate and diethylene glycol n-butyl ether acetate.
本發明之彩色濾光片之製造方法為包含於透明性絕緣基板上之間隔部的間隙,以噴墨方式選擇性塗佈顏料分散液之步驟(顏料分散液塗佈步驟)、和在前述顏料分散液塗佈步驟後,於前述間隔部的間隙以噴墨方式選擇性塗佈透明樹脂溶液,並於該間隙內混合顏料分散液和透明樹脂溶液之步驟(透明樹脂溶液塗佈步驟)、和令前述透明樹脂溶液塗佈步驟所形成之顏料分散液和透明樹脂溶液的混合液層硬化之步驟(硬化步驟)。The method for producing a color filter of the present invention is a step of selectively coating a pigment dispersion liquid by an inkjet method in a gap of a spacer portion on a transparent insulating substrate (pigment dispersion coating step), and a pigment in the foregoing After the dispersion coating step, a step of selectively coating the transparent resin solution by the inkjet method at the gap of the spacer portion, and mixing the pigment dispersion liquid and the transparent resin solution in the gap (transparent resin solution coating step), and The step of hardening the mixed layer of the pigment dispersion liquid and the transparent resin solution formed by the aforementioned transparent resin solution coating step (hardening step).
於本發明之顏料分散液塗佈步驟中,首先於彩色濾光片之透明性絕緣基板上形成間隔部(黑色矩陣)。In the pigment dispersion coating step of the present invention, a spacer (black matrix) is first formed on the transparent insulating substrate of the color filter.
本發明中彩色濾光片所用之透明性絕緣基板,可列舉例如玻璃、矽、聚碳酸酯、聚酯、芳香族聚醯胺、聚醯胺醯亞胺、聚醯亞胺等。又,於此等透明性絕緣基板上,視需要亦可適當施行以矽烷偶合劑等之藥品處理、電漿處理、離子電鍍、濺鍍、氣相反應法和真空蒸鍍處理等之前處理。The transparent insulating substrate used for the color filter of the present invention may, for example, be glass, ruthenium, polycarbonate, polyester, aromatic polyamide, polyamidimide or polyimine. Further, on the transparent insulating substrate, a pretreatment such as a drug treatment such as a decane coupling agent, a plasma treatment, an ion plating, a sputtering, a gas phase reaction method, or a vacuum vapor deposition treatment may be appropriately performed.
形成間隔部的材料為含有樹脂成分和黑色顏料(碳黑等)及/或混合R(紅)、G(綠)、B(藍)、Y(黃)、V(紫)等顏料之混色黑色顏料、和分解溶解此些成分用之溶劑的感光性樹脂。樹脂材料可為一般使用作為黑色感光性樹脂用之丙烯酸樹脂般之負型或正型亦可。間隔部的高度可為透明著色樹脂膜的膜厚程度,於使用作為高色度區域方式的彩色濾光片時,為1.5μm以上5.0μm以下,更佳為2.0μm以上4.0μm以下。間隔部的寬度為10μm以上30μm以下,則經由間隔部所區隔的光穿透區域一般為寬60μm至250μm的矩形和彎曲形。The material forming the spacer is a mixed color black containing a resin component and a black pigment (carbon black or the like) and/or a mixture of R (red), G (green), B (blue), Y (yellow), V (purple), and the like. A pigment and a photosensitive resin which decomposes a solvent for dissolving these components. The resin material may be a negative type or a positive type which is generally used as an acrylic resin for a black photosensitive resin. The height of the spacer may be a film thickness of the transparent colored resin film, and when it is used as a color filter of a high chroma region, it is 1.5 μm or more and 5.0 μm or less, and more preferably 2.0 μm or more and 4.0 μm or less. When the width of the spacer is 10 μm or more and 30 μm or less, the light-transmitting region partitioned via the spacer is generally rectangular and curved in a width of 60 μm to 250 μm.
使用此感光性樹脂於透明絕緣基板上形成間隔部上,則如以旋塗等全面形成具有1~3μm左右厚度之薄膜後,以光阻步驟(曝光及顯像)則可形成。When the photosensitive resin is used to form a spacer on the transparent insulating substrate, a film having a thickness of about 1 to 3 μm is formed by spin coating or the like, and then formed by a photoresist step (exposure and development).
其次,於如此所得之間隔部的間隙,即間隔部所圍住的部分(成為RGB畫素的部分),將配合R、G、B等所欲顏料之上述顏料分散液,以噴墨方式選擇性附著,於畫素部和遮光層等塗佈顏料分散液(著色液),形成著色液層。著色液層的厚度為根據R、G、B各層而有差異,大約為0.4~2.0μm之範圍。著色液層的厚度若為此範圍外,則有時發生間隔部與著色層的段差。Next, in the gap between the spacers thus obtained, that is, the portion surrounded by the spacer (the portion which becomes the RGB pixel), the pigment dispersion liquid of the desired pigment such as R, G, or B is selected by the ink jet method. Sexual adhesion, coating a pigment dispersion (coloring liquid) on a pixel portion and a light shielding layer to form a coloring liquid layer. The thickness of the coloring liquid layer varies depending on each of the layers of R, G, and B, and is approximately in the range of 0.4 to 2.0 μm. If the thickness of the coloring liquid layer is outside this range, a step difference between the spacer and the coloring layer may occur.
其次,令所形成的著色液層,視需要予以乾燥(預乾燥步驟)。經由進行此類預乾燥,顏料可於著色液層中以均勻分散的狀態下,僅將顏料分散液的溶劑成分減量。顏料分散液的乾燥(溶劑之減量)若不夠充分,則在塗佈透明樹脂溶液時,顏料分散液與透明樹脂溶液混合後的液量變大,恐混合液滲出間隔部並且混色。Next, the formed coloring liquid layer is dried as needed (pre-drying step). By performing such pre-drying, the pigment can be reduced only in the solvent dispersion of the pigment dispersion in a state where the pigment is uniformly dispersed in the coloring liquid layer. When the drying of the pigment dispersion liquid (the amount of reduction in the solvent) is insufficient, when the transparent resin solution is applied, the amount of the liquid after the pigment dispersion liquid and the transparent resin solution are mixed becomes large, and the mixed liquid leaks out of the partition portion and is mixed.
以40~160℃之溫度範圍進行乾燥為佳。乾燥溫度若過低,則顏料分散液的體積變化變小,塗佈透明樹脂溶液時恐混色。又,乾燥溫度若過高,則在塗佈透明樹脂溶液時,透明樹脂溶液無法於著色液層上均勻濕潤擴展,恐發生硬化膜表面粗糙。乾燥時間雖無特別限定,但以1~20分鐘為佳。It is preferred to carry out drying at a temperature ranging from 40 to 160 °C. When the drying temperature is too low, the volume change of the pigment dispersion liquid becomes small, and the color mixture is feared when the transparent resin solution is applied. Further, when the drying temperature is too high, when the transparent resin solution is applied, the transparent resin solution cannot be uniformly wetted and spread on the coloring liquid layer, and the surface of the cured film may be rough. Although the drying time is not particularly limited, it is preferably from 1 to 20 minutes.
於本發明之透明樹脂溶液塗佈步驟中,於前述間隔部的間隙將透明樹脂溶液以噴墨方式選擇性塗佈,於該間隙內將顏料分散液和透明樹脂溶液混合。即,於前述顏料分散液塗佈步驟所形成之著色液層上,塗佈透明樹脂溶液形成透明樹脂層,將兩層混合形成著色液層與透明樹脂層所構成的混合液層(著色樹脂層)。In the transparent resin solution coating step of the present invention, the transparent resin solution is selectively applied by the inkjet method in the gap of the spacer portion, and the pigment dispersion liquid and the transparent resin solution are mixed in the gap. That is, on the coloring liquid layer formed by the pigment dispersion coating step, a transparent resin solution is applied to form a transparent resin layer, and the two layers are mixed to form a mixed liquid layer composed of a colored liquid layer and a transparent resin layer (colored resin layer). ).
於乾燥之顏料分散液(著色液層)上若塗佈黏度低的透明樹脂溶液,則顏料於透明樹脂溶液中以再分散之狀態,如此令顏料分散液與透明樹脂溶液混合、或者著色液層與透明樹脂層融合。因此,於上述顏料分散液塗佈步驟中,所形成的著色液層即使為經由預乾燥步驟被完全乾燥之狀態,亦可與顏料和透明樹脂溶液充分混合。When a transparent resin solution having a low viscosity is applied to the dried pigment dispersion (coloring liquid layer), the pigment is redispersed in the transparent resin solution, so that the pigment dispersion liquid is mixed with the transparent resin solution or the coloring liquid layer Fusion with a transparent resin layer. Therefore, in the above-described pigment dispersion coating step, the formed coloring liquid layer can be sufficiently mixed with the pigment and the transparent resin solution even in a state of being completely dried through the pre-drying step.
透明樹脂溶液之塗佈量為根據RGB各層而有差異,RGB各色之著色樹脂層的膜厚差為0.1μm以下般適當調整塗佈量。透明樹脂溶液之塗佈量為令顏料分散液與透明樹脂溶液乾燥後之固形成分比率(混合液層硬化後之顏料與透明樹脂之固形成分的比率)為顏料:透明樹脂=1:0.4~1般調整為佳。The coating amount of the transparent resin solution is different depending on the RGB layers, and the coating amount is appropriately adjusted as the film thickness difference of the colored resin layers of the respective RGB colors is 0.1 μm or less. The coating amount of the transparent resin solution is a ratio of solid content of the pigment dispersion liquid and the transparent resin solution after drying (the ratio of the solid content of the pigment after the mixture layer is hardened to the transparent resin) is pigment: transparent resin = 1: 0.4 to 1 The general adjustment is better.
又,前述混合液層(著色樹脂層)期望形成與前述間隔部相同膜厚,如此必須調整透明樹脂溶液的塗佈量。透明樹脂溶液的塗佈量若對於顏料分散液為小量,則恐無法濕潤擴展至著色樹脂層全體的各個角落。又,透明樹脂溶液之塗佈量若對於顏料分散液為大量,則著色樹脂層的膜厚變大,無法形成間隔部與著色樹脂層之間無段差的著色樹脂層。Moreover, it is desirable that the mixed liquid layer (colored resin layer) has the same film thickness as the above-mentioned spacer, and it is necessary to adjust the coating amount of the transparent resin solution. When the coating amount of the transparent resin solution is small for the pigment dispersion liquid, it may not be wetted and spread to the respective corners of the entire colored resin layer. In addition, when the coating amount of the transparent resin solution is large for the pigment dispersion liquid, the thickness of the colored resin layer becomes large, and the colored resin layer having no difference between the spacer portion and the colored resin layer cannot be formed.
著色樹脂層的厚度大約為1.0~2.5μm之範圍內。著色樹脂層的厚度若超過此範圍,則於間隔部與著色層之間產生段差,發生濾光片全體的平坦性變差之缺點。The thickness of the colored resin layer is approximately in the range of 1.0 to 2.5 μm. When the thickness of the colored resin layer exceeds this range, a step is generated between the spacer and the coloring layer, and the flatness of the entire filter is deteriorated.
令著色樹脂層乾燥的步驟(預烘烤步驟)為於80~200℃之溫度範圍下進行為佳。The step of drying the colored resin layer (prebaking step) is preferably carried out at a temperature of from 80 to 200 °C.
乾燥溫度若過低,則著色樹脂層的體積變化變小,著色樹脂層的膜厚變大,恐無法形成間隔部與著色樹脂層之間無段差的著色樹脂層。又,乾燥溫度若過高,則著色樹脂層的體積變化變大,著色樹脂層的膜厚變小,恐無法形成間隔部與著色樹脂層之間無段差的著色樹脂層。When the drying temperature is too low, the volume change of the colored resin layer becomes small, and the film thickness of the colored resin layer becomes large, so that the colored resin layer having no difference between the spacer and the colored resin layer cannot be formed. In addition, when the drying temperature is too high, the volume change of the colored resin layer becomes large, and the film thickness of the colored resin layer becomes small, so that the colored resin layer having no difference between the spacer and the colored resin layer cannot be formed.
於本發明中,令前述透明樹脂溶液塗佈步驟所形成的顏料分散液與透明樹脂溶液的混合液層硬化(硬化步驟)。In the present invention, the mixed liquid layer of the pigment dispersion liquid and the transparent resin solution formed by the transparent resin solution coating step is hardened (hardening step).
使用光硬化型樹脂組成物作為透明樹脂時,以照射光線進行硬化。所使用之光以紫外光或可見光為佳,其中,以波長200~500nm之光為佳。此些光源例如可使用低壓水銀燈、高壓水銀燈、超高壓水銀燈、金屬鹵素燈、化學燈、黑光燈、水銀-氙燈、準分子雷射燈、短電弧燈、氦-鎘雷射、氬雷射、Nd-YAG雷射之THG和FHG光雷射等公知慣用的光源。光硬化條件為受到所用光源之種類、光聚合啟始劑之種類和份量影響,無法一概決定,但一般以100~3000mJ/m2 之範圍為佳。光硬化後,以200~250℃施以10~30分鐘的後硬化(後烘烤)處理。When a photocurable resin composition is used as the transparent resin, it is cured by irradiation with light. The light to be used is preferably ultraviolet light or visible light, and light having a wavelength of 200 to 500 nm is preferred. Such light sources may, for example, use low pressure mercury lamps, high pressure mercury lamps, ultra high pressure mercury lamps, metal halide lamps, chemical lamps, black lamps, mercury-xenon lamps, excimer laser lamps, short arc lamps, neo-cadmium lasers, argon lasers, Known conventional light sources such as Nd-YAG laser THG and FHG light lasers. The photohardening condition is not affected by the kind of the light source used and the type and amount of the photopolymerization initiator, but is generally determined to be in the range of 100 to 3000 mJ/m 2 . After photohardening, post-hardening (post-baking) treatment is carried out at 200 to 250 ° C for 10 to 30 minutes.
使用熱硬化型樹脂組成物作為透明樹脂時,以加熱進行硬化。加熱硬化條件為以加熱溫度為200~250℃左右、加熱時間為20~60分鐘左右。When a thermosetting resin composition is used as the transparent resin, it is cured by heating. The heat curing conditions are such that the heating temperature is about 200 to 250 ° C and the heating time is about 20 to 60 minutes.
於本發明之彩色濾光片的製造方法中,令上述混合液層(著色樹脂層)硬化後,視需要亦可於其上形成保護層。保護層通常可使用光硬化型、熱硬化型、或熱-光併用硬化型之樹脂組成物層、或蒸鍍或濺鍍所形成的無機化合物層。In the method for producing a color filter of the present invention, after the mixed liquid layer (colored resin layer) is cured, a protective layer may be formed thereon as needed. As the protective layer, a photocurable type, a thermosetting type, or a thermo-optic curing type resin composition layer or an inorganic compound layer formed by vapor deposition or sputtering can be usually used.
其次,於此保護層上形成ITO(氧化銦錫)膜作為電極。更且,於其上以公知方法形成配向膜(聚醯亞胺膜),製造彩色濾光片。Next, an ITO (Indium Tin Oxide) film was formed as an electrode on this protective layer. Further, an alignment film (polyimine film) is formed thereon by a known method to produce a color filter.
本發明之液晶顯示裝置,其特徵為具備根據上述本發明之彩色濾光片之製造方法所製造的彩色濾光片,和玻璃基板等之對向基板,和被夾於前述彩色濾光片與前述對向基板之間的液晶組成物。A liquid crystal display device of the present invention is characterized by comprising a color filter manufactured by the method for producing a color filter of the present invention, an opposite substrate such as a glass substrate, and a color filter sandwiched between the color filter and the color filter. a liquid crystal composition between the opposite counter substrates.
液晶顯示裝置為將彩色濾光片側的基板與對向基板合併,於其間封入液晶則可形成。於對向基板的內側,TFT與畫素電極為以矩狀形成。又,於對向基板側亦形成配向膜,令液晶分子於一定方向上排列。於穿透型之情形中以透明素材形成基板及畫素電極,並於各基板的外側接黏偏光板。於反射型之情形中,將基板或畫素電極,以具備反射機能的素材形成或者於基板設置反射層,並於透明基板的外側設置偏光板,將來自彩色濾光片側所的光線予以反射進行顯示。The liquid crystal display device can be formed by combining a substrate on the color filter side and a counter substrate, and enclosing liquid crystal therebetween. On the inner side of the counter substrate, the TFT and the pixel electrode are formed in a rectangular shape. Further, an alignment film is formed on the opposite substrate side so that the liquid crystal molecules are aligned in a certain direction. In the case of the penetrating type, the substrate and the pixel electrode are formed of a transparent material, and the polarizing plate is bonded to the outside of each of the substrates. In the case of the reflective type, the substrate or the pixel electrode is formed of a material having a reflection function or a reflective layer is provided on the substrate, and a polarizing plate is disposed outside the transparent substrate to reflect the light from the side of the color filter. Display.
本發明之液晶顯示裝置若為使用本發明之彩色濾光片所構成,則關於其他構材可適當使用先前之技術。When the liquid crystal display device of the present invention is configured by using the color filter of the present invention, the prior art can be suitably used for other members.
另外,本發明並非被限定於上述實施形態。上述實施形態為例示,具有與本發明申請專利範圍所記載之技術性思想實質上相同之構成,且達成同樣之作用效果者,則無論何者均被包含於本發明的技術範圍。Further, the present invention is not limited to the above embodiment. The above-described embodiments are exemplified, and have substantially the same configuration as the technical idea described in the patent application scope of the present invention, and the same effects are achieved, and any of them are included in the technical scope of the present invention.
以下,列舉實施例具體說明本發明,但本發明並非僅被限定於此些實施例。另外,以下實施例中之各物性的評價方法為如下。又,下列實施例中所謂「份」為表示「重量份」。Hereinafter, the present invention will be specifically described by way of examples, but the present invention is not limited to the examples. In addition, the evaluation method of each physical property in the following examples is as follows. In addition, in the following examples, "parts" means "parts by weight".
將Red顏料、顏料分散劑、及有機溶劑以下述之比例混合,並加入直徑0.3mm之氧化鋯珠粒500份,使用塗料振盪器分散4小時,取得顏料分散液(R)。The Red pigment, the pigment dispersant, and the organic solvent were mixed in the following ratio, and 500 parts of zirconia beads having a diameter of 0.3 mm were added, and dispersed using a paint shaker for 4 hours to obtain a pigment dispersion liquid (R).
Red顏料(C.I.顏料紅254):10份Red pigment (C.I. Pigment Red 254): 10 parts
顏料分散劑(AVECIA公司製:Solsperse 24000):10份Pigment dispersant (made by AVECIA: Solsperse 24000): 10 parts
DPMA(二丙二醇甲醚醋酸酯;沸點=209℃、表面張力=27mN/m):80份DPMA (dipropylene glycol methyl ether acetate; boiling point = 209 ° C, surface tension = 27 mN / m): 80 parts
於上述(1)中除了使用Green顏料(C.I.顏料綠36)10份、Yellow顏料(C.I.顏料黃150)10份代替Red顏料(C.I.顏料紅254)10份以外,同製造例1處理調製顏料分散液(G1)和顏料分散液(Y)。將顏料分散液(G1)53份與顏料分散液(Y)47份混合調製綠色顏料分散液(G2)。In the above (1), in addition to using 10 parts of Green Pigment (CI Pigment Green 36) and 10 parts of Yellow Pigment (CI Pigment Yellow 150) instead of 10 parts of Red Pigment (CI Pigment Red 254), the preparation of the pigment dispersion was treated as in Production Example 1. Liquid (G1) and pigment dispersion (Y). 53 parts of the pigment dispersion (G1) and 47 parts of the pigment dispersion (Y) were mixed to prepare a green pigment dispersion (G2).
於上述(1)中除了使用Blue顏料(C.I.顏料藍15:6)10份代替Red顏料10份以外,同製造例1處理調製顏料分散液(B)。In the above (1), the pigment dispersion liquid (B) was prepared in the same manner as in Production Example 1, except that 10 parts of Blue pigment (C.I. Pigment Blue 15:6) was used instead of 10 parts of the Red pigment.
於製造例1中除了使用BCA(二乙二醇丁醚醋酸酯;沸點=247℃、表面張力=30mN/m)代替DPMA以外,以製造例1(1)~(3)同樣之方法分別調製紅色、綠色、及藍色顏料分散液。In Production Example 1, except that BCA (diethylene glycol butyl ether acetate; boiling point = 247 ° C, surface tension = 30 mN/m) was used instead of DPMA, it was separately prepared in the same manner as in Production Example 1 (1) to (3). Red, green, and blue pigment dispersions.
將聚酯丙烯酸系低聚物15份、二季戊四醇六丙烯酸酯(以下,簡述為DPHA)15份、1,6-己二醇二丙烯酸酯20份、二丙二醇甲醚醋酸酯45.5份、及Ciba specialty Chemicals公司製光聚合啟始劑「Irgacure 369」0.5份混合後,使用孔徑1.0μm之濾紙過濾,取得透明樹脂溶液。15 parts of a polyester acrylic oligomer, 15 parts of dipentaerythritol hexaacrylate (hereinafter referred to as DPHA), 20 parts of 1,6-hexanediol diacrylate, 45.5 parts of dipropylene glycol methyl ether acetate, and 0.5 parts of the photopolymerization initiator "Irgacure 369" manufactured by Ciba Specialty Chemicals Co., Ltd. was mixed, and then filtered using a filter paper having a pore size of 1.0 μm to obtain a transparent resin solution.
將黏合劑(甲基丙烯酸酯水甘油酯-苯乙烯共聚物)10份、酚醛清漆型環氧樹脂(油化Shell公司製、商品名「Epicoat 154」:10份、新戊二醇二縮水甘油醚20重量份、硬化劑(偏苯三酸)5重量份、二丙二醇甲醚醋酸酯55份混合後,使用孔徑 1.0μm 之濾紙過濾,取得熱硬化型透明樹脂溶液。10 parts of a binder (methacrylate glycerol-styrene copolymer), a novolac type epoxy resin (manufactured by Oily Shell Co., Ltd., trade name "Epicoat 154": 10 parts, neopentyl glycol diglycidyl 20 parts by weight of an ether, 5 parts by weight of a curing agent (trimellitic acid), and 55 parts of dipropylene glycol methyl ether acetate were mixed, and then filtered using a filter paper having a pore size of 1.0 μm to obtain a thermosetting transparent resin solution.
於厚度 0.7mm 之 10 公分×10 公分玻璃基板(旭硝子(股)製)上,使用黑色矩陣用硬化性樹脂組成物,根據光微影法形成線寬20μm、膜厚1.6μm的黑色矩陣圖型。A black matrix pattern having a line width of 20 μm and a film thickness of 1.6 μm was formed by a photolithography method using a curable resin composition for a black matrix on a 10 cm × 10 cm glass substrate (manufactured by Asahi Glass Co., Ltd.) having a thickness of 0.7 mm. .
於上述基板之經黑色矩陣區隔的藍色畫素形成部,將製造例1所得之藍色顏料分散液經由噴墨方式,正確且均勻附著。The blue pigment dispersion liquid obtained in Production Example 1 was accurately and uniformly adhered to the blue pigment dispersion portion obtained in the black matrix of the substrate.
其次,於相同基板之綠色畫素形成部,將製造例1之綠色顏料分散液經由噴墨方式,正確且均勻附著。其次,於相同基板之紅色畫素形成部,將製造例1之紅色顏料分散液經由噴墨方式,正確且均勻附著。塗佈顏料分散液後,於100℃之熱板上進行10分鐘預乾燥。Next, the green pigment dispersion liquid of Production Example 1 was accurately and uniformly adhered to the green pigment dispersion portion of the same substrate by an inkjet method. Next, the red pigment dispersion liquid of Production Example 1 was accurately and uniformly adhered to the red pixel dispersion portion of the same substrate by an inkjet method. After the pigment dispersion was applied, it was pre-dried on a hot plate at 100 ° C for 10 minutes.
其後,於黑色矩陣所區隔之各色畫素形成部的顏料分散液上,將製造例3的透明樹脂溶液,以混合液層硬化後之固形成分比率為顏料:透明樹脂=1:0.8般調整,並且經由噴墨方式正確且均勻附著。其後,於180℃之熱板上進行20分鐘預烘烤,並以高壓水銀燈進行 200mJ/cm2 之曝光令其光硬化後,再以230℃施行20分鐘硬化。Thereafter, on the pigment dispersion liquid of each color pixel forming portion in which the black matrix is partitioned, the solid resin solution of the production example 3 was cured in a mixed liquid layer, and the solid content ratio was pigment: transparent resin = 1:0.8 Adjusted and adhered correctly and evenly via the inkjet method. Thereafter, it was prebaked on a hot plate at 180 ° C for 20 minutes, and exposed to light at 200 mJ/cm 2 with a high pressure mercury lamp, and then hardened at 230 ° C for 20 minutes.
將形成RGB畫素圖型的基板,於IPA(異丙醇)中浸漬5分鐘,其次以IPA蒸氣進行乾燥洗淨後,以基板設定溫度200℃,於 6×10-3 Torr真空下以 120nm之厚度成膜出ITO(氧化銦錫)電極。將此進行ITO成膜的基板再於IPA中浸漬5分鐘,並以IPA進行蒸洗淨後,將聚醯亞胺旋塗,進行180℃、60分鐘之煅燒,形成配向膜,取得彩色濾光片。The substrate of the RGB pixel pattern was formed, immersed in IPA (isopropyl alcohol) for 5 minutes, and then dried by IPA vapor, and then set at a substrate temperature of 200 ° C under a vacuum of 6 × 10 -3 Torr at 120 nm. The thickness is formed into an ITO (indium tin oxide) electrode. The substrate on which the ITO film was formed was further immersed in IPA for 5 minutes, and then washed with IPA, and then spin-coated with polyimine, and calcined at 180 ° C for 60 minutes to form an alignment film to obtain color filter. sheet.
於實施例1中,除了以混合液層之硬化後的固形成分比率為顏料:透明樹脂=1:0.4般塗佈透明樹脂溶液以外,以實施例1同樣之方法製作彩色濾光片。In the first embodiment, a color filter was produced in the same manner as in Example 1 except that the solid content ratio after curing of the mixed liquid layer was a pigment: transparent resin = 1:0.4.
於實施例2之彩色濾光片製作步驟中,除了令塗佈顏料分散液後之預乾燥為於60℃之熱板上10分鐘,塗佈透明樹脂溶液後之預烘烤為於150℃之熱板上20分鐘以外,以實施例2同樣之方法製作彩色濾光片。In the color filter manufacturing step of the second embodiment, the pre-baking after coating the pigment dispersion liquid is performed on a hot plate at 60 ° C for 10 minutes, and the pre-baking after coating the transparent resin solution is at 150 ° C. A color filter was produced in the same manner as in Example 2 except for 20 minutes on a hot plate.
除了使用製造例4之熱硬化型透明樹脂溶液,代替實施例2中使用製造例3之光硬化型透明樹脂溶液,且硬化條件為以230℃加熱30分鐘以外,以實施例2同樣之方法製作彩色濾光片。The same procedure as in Example 2 was carried out except that the thermosetting transparent resin solution of Production Example 4 was used instead of the photocurable transparent resin solution of Production Example 3 in Example 2, and the curing conditions were at 230 ° C for 30 minutes. Color filter.
除了使用製造例2之顏料分散液,代替實施例2中使用製造例1之顏料分散液、及混合液層硬化後之固形成分比率為顏料:透明樹脂=1:1.2般塗佈透明樹脂溶液以外,以實施例2同樣之方法製作彩色濾光片。In addition to the use of the pigment dispersion liquid of Production Example 2, instead of the pigment dispersion liquid of Production Example 1 used in Example 2 and the solid content ratio after curing of the mixed liquid layer, the pigment: transparent resin = 1:1.2 was coated with a transparent resin solution. A color filter was produced in the same manner as in Example 2.
於實施例5中,除了混合液層硬化後之固形成分比率為顏料:透明樹脂=1:0.2般塗佈透明樹脂溶液以外,以同樣之方法製作彩色濾光片。In Example 5, a color filter was produced in the same manner except that the solid solution ratio after curing of the mixed liquid layer was a pigment: transparent resin = 1:0.2, and a transparent resin solution was applied.
除了未進行實施例5中塗佈顏料分散液後之預乾燥、透明樹脂溶液塗佈後之預烘烤以220℃之熱板進行20分鐘、及混合液層硬化後之固形成分比率為顏料:透明樹脂=1:0.8般塗佈透明樹脂溶液以外,以實施例5同樣之方法製作彩色濾光片。Pre-baking after coating the pigment dispersion in Example 5, pre-baking after coating of the transparent resin solution, hot plate at 220 ° C for 20 minutes, and solid solution ratio after hardening of the mixed layer were pigments: A color filter was produced in the same manner as in Example 5 except that a transparent resin solution was applied as a transparent resin = 0.8.
除了使用製造例4之熱硬化型透明樹脂溶液,代替實施例7中使用製造例3之光硬化型透明樹脂溶液,及硬化條件為以230℃加熱30分鐘以外,以實施例7同樣之方法製作彩色濾光片。The same procedure as in Example 7 was carried out except that the thermosetting transparent resin solution of Production Example 4 was used instead of the photocurable transparent resin solution of Production Example 3 in Example 7, and the curing conditions were at 230 ° C for 30 minutes. Color filter.
將Red顏料、顏料分散劑、及有機溶劑以下述之比例混合,並加入直徑0.3mm之氧化鋯珠粒500份,使用塗料振盪器分散4小時,取得顏料分散液(R)。將所得之顏料分散液(R)50份、聚酯丙烯酸系低聚物10份、DPHA 10份、1,6-己二醇二丙烯酸酯20份、DPMA 9.5份、及Ciba Specialty Chemicals公司製光聚合啟始劑「Irgacure 369」0.5份混合後,使用孔徑1.0μm之濾紙過濾,取得彩色濾光片用紅色噴墨油墨。The Red pigment, the pigment dispersant, and the organic solvent were mixed in the following ratio, and 500 parts of zirconia beads having a diameter of 0.3 mm were added, and dispersed using a paint shaker for 4 hours to obtain a pigment dispersion liquid (R). 50 parts of the obtained pigment dispersion (R), 10 parts of polyester acrylic oligomer, 10 parts of DPHA, 20 parts of 1,6-hexanediol diacrylate, 9.5 parts of DPMA, and light by Ciba Specialty Chemicals Co., Ltd. After mixing 0.5 parts of the polymerization initiator "Irgacure 369", it was filtered using a filter paper having a pore size of 1.0 μm to obtain a red inkjet ink for a color filter.
Red顏料(C.I.顏料紅254):20份Red pigment (C.I. Pigment Red 254): 20 parts
顏料分散劑(AVECIA公司製:Solsperse 24000):15份Pigment dispersant (made by AVECIA: Solsperse 24000): 15 parts
DPMA(二丙二醇甲醚醋酸酯):65份DPMA (dipropylene glycol methyl ether acetate): 65 parts
除了使用Green顏料(C.I.顏料綠36)20份、Yellow顏料(C.I.顏料黃150)20份,代替上述製造例5(1)之噴墨油墨調製中使用之Red顏料(C.I.顏料紅254)20份以外,同樣處理調製綠色顏料分散液和黃色顏料分散液。將綠色顏料分散液53份與黃色顏料分散液47份混合,調製綠色顏料分散液(G)。使用所得之綠色顏料分散液(G),以上述(1)之紅色噴墨油墨同樣之方法,調製綠色噴墨油墨。In addition to 20 parts of Green Pigment (CI Pigment Green 36) and 20 parts of Yellow Pigment (CI Pigment Yellow 150), 20 parts of Red Pigment (CI Pigment Red 254) used in the preparation of the inkjet ink of the above Production Example 5 (1) was used. In addition, the green pigment dispersion and the yellow pigment dispersion were also treated in the same manner. 53 parts of the green pigment dispersion liquid and 47 parts of the yellow pigment dispersion liquid were mixed to prepare a green pigment dispersion liquid (G). Using the obtained green pigment dispersion (G), a green inkjet ink was prepared in the same manner as in the above red inkjet ink of (1).
除了使用Blue顏料(C.I.顏料藍15:6)10份,代替上述製造例5(1)之Red顏料(C.I.顏料紅254)20份以外,同樣處理調製藍色顏料分散液。使用所得之藍色顏料分散液,以上述(1)之紅色噴墨油墨同樣之方法,調製藍色噴墨油墨。A blue pigment dispersion liquid was prepared in the same manner except that 10 parts of Blue pigment (C.I. Pigment Blue 15:6) was used instead of 20 parts of the Red pigment (C.I. Pigment Red 254) of the above Production Example 5 (1). Using the obtained blue pigment dispersion liquid, a blue inkjet ink was prepared in the same manner as in the above red inkjet ink of (1).
將Red顏料、顏料分散劑、及有機溶劑以下述之比例混合,並加入直徑0.3mm之氧化鋯珠粒500份,使用塗料振盪器分散4小時,取得顏料分散液。將所得之顏料分散液50份、聚酯丙烯酸系低聚物10份、DPHA 10份、1,6-己二醇二丙烯酸酯20份、DPMA 9.5份、及Ciba Specialty Chemicals公司製光聚合啟始劑「Irgacure 369」0.5份混合後,使用孔徑1.0μm之濾紙過濾,取得彩色濾光片用紅色噴墨油墨。The Red pigment, the pigment dispersant, and the organic solvent were mixed in the following ratio, and 500 parts of zirconia beads having a diameter of 0.3 mm were added, and dispersed using a paint shaker for 4 hours to obtain a pigment dispersion liquid. 50 parts of the obtained pigment dispersion, 10 parts of polyester acrylic oligomer, 10 parts of DPHA, 20 parts of 1,6-hexanediol diacrylate, 9.5 parts of DPMA, and photopolymerization by Cib a Specialty Chemicals Co., Ltd. After 0.5 parts of the initiator "Irgacure 369" was mixed, it was filtered using a filter paper having a pore size of 1.0 μm to obtain a red inkjet ink for a color filter.
Red顏料(C.I.顏料紅254):15份Red pigment (C.I. Pigment Red 254): 15 parts
顏料分散劑(AVECIA公司製:Solsperse 24000):15份Pigment dispersant (made by AVECIA: Solsperse 24000): 15 parts
DPMA(二丙二醇甲醚醋酸酯):70份DPMA (dipropylene glycol methyl ether acetate): 70 parts
除了使用Green顏料(C.I.顏料綠36)15份、Yellow顏料(C.I.顏料黃150)15份,代替上述製造例6(1)之Red顏料(C.I.顏料紅254)15份以外,同樣處理調製顏料分散液(G1)和顏料分散液(Y)。將顏料分散液(G1)53份與顏料分散液(Y)47份混合,調製綠色顏料分散液(G2)。使用所得之綠色顏料分散液(G2),以上述紅色噴墨油墨同樣之方法,調製綠色噴墨油墨。In addition to using 15 parts of Green Pigment (CI Pigment Green 36) and 15 parts of Yellow Pigment (CI Pigment Yellow 150), instead of 15 parts of Red Pigment (CI Pigment Red 254) of the above Production Example 6 (1), the same treatment was used to prepare the pigment dispersion. Liquid (G1) and pigment dispersion (Y). 53 parts of the pigment dispersion liquid (G1) and 47 parts of the pigment dispersion liquid (Y) were mixed to prepare a green pigment dispersion liquid (G2). Using the obtained green pigment dispersion (G2), a green inkjet ink was prepared in the same manner as the above red inkjet ink.
除了使用Blue顏料(C.I.顏料藍15:6)15份,代替上述製造例6(1)之Red顏料(C.I.顏料紅254)15份以外,同樣處理調製顏料分散液(B)。使用所得之顏料分散液(B),以上述紅色噴墨油墨同樣之方法,調製藍色噴墨油墨。The pigment dispersion liquid (B) was prepared in the same manner except that 15 parts of Blue pigment (C.I. Pigment Blue 15:6) was used instead of 15 parts of the Red pigment (C.I. Pigment Red 254) of the above Production Example 6 (1). Using the obtained pigment dispersion liquid (B), a blue inkjet ink was prepared in the same manner as the above red inkjet ink.
於實施例1同樣基板之經黑色矩陣區隔的藍色畫素形成部,將製造例5之藍色噴墨油墨經由噴墨方式,正確且均勻附著。其次,於相同基板之綠色畫素形成部,將製造例5之綠色噴墨油墨經由噴墨方式,正確且均勻附著。其次,於相同基板之紅色畫素形成部,將製造例5之紅色噴墨油墨經由噴墨方式,正確且均勻附著。其後,於180℃熱板上進行20分鐘預烘烤,並使用高壓水銀燈進行200mJ/cm2 之曝光令其光硬化後,再以230℃施行20分鐘硬化。In the blue pixel forming portion partitioned by the black matrix of the same substrate of Example 1, the blue inkjet ink of Production Example 5 was adhered accurately and uniformly via the inkjet method. Next, the green inkjet ink of Production Example 5 was adhered accurately and uniformly to the green pixel forming portion of the same substrate via the inkjet method. Next, the red inkjet ink of Production Example 5 was accurately and uniformly attached via the inkjet method to the red pixel forming portion of the same substrate. Thereafter, it was prebaked on a hot plate at 180 ° C for 20 minutes, and exposed to light at 200 mJ/cm 2 using a high-pressure mercury lamp, and then hardened at 230 ° C for 20 minutes.
將形成RGB畫素圖型的基板,於IPA中浸漬5分鐘,其次以IPA蒸氣進行乾燥洗淨後,以基板設定溫度200℃,於6×10-3 Torr真空下以120nm之厚度成膜出ITO(氧化銦錫)電極。將此進行ITO成膜的基板再於IPA中浸漬5分鐘,並以IPA蒸氣洗淨後,將聚醯亞胺旋塗,進行180℃、60分鐘之煅燒,形成配向膜,取得彩色濾光片。RGB pixel pattern forming substrate, for 5 minutes, followed by IPA vapor in drying after cleaning in IPA, to set the substrate temperature 200 ℃, at 6 × 10 -3 Torr vacuum deposition to a thickness of 120nm ITO (indium tin oxide) electrode. The substrate on which the ITO film was formed was further immersed in IPA for 5 minutes, washed with IPA vapor, and then spin-coated with polyimine, and calcined at 180 ° C for 60 minutes to form an alignment film to obtain a color filter. .
除了使用製造例6之噴墨油墨,代替比較例1製造中使用製造例5之噴墨油墨以外,以比較例1同樣之方法製作彩色濾光片。A color filter was produced in the same manner as in Comparative Example 1, except that the inkjet ink of Production Example 6 was used instead of the inkjet ink of Production Example 5 used in the production of Comparative Example 1.
關於上述製造例1~6所得之顏料分散液、透明樹脂溶液、及噴墨油墨(顏料油墨),以下列方法評價黏度及吐出安定性。又,關於上述實施例1~8、比較例1~2所製作之彩色濾光片,以下列方法評價有無脫白、有無混色、膜厚、及色度。With respect to the pigment dispersion liquid, the transparent resin solution, and the inkjet ink (pigment ink) obtained in the above Production Examples 1 to 6, the viscosity and the discharge stability were evaluated by the following methods. Further, with respect to the color filters produced in the above Examples 1 to 8 and Comparative Examples 1 and 2, the presence or absence of whitening, presence or absence of color mixing, film thickness, and chromaticity were evaluated by the following methods.
於23℃下,使用迴轉振動型黏度計(VM-1G、山一電機公司製)測定。The measurement was carried out at 23 ° C using a rotary vibration type viscometer (VM-1G, manufactured by Yamaichi Electric Co., Ltd.).
將前述實施例和比較例所得之顏料分散液、透明樹脂溶液、及噴墨油墨,於照片印畫用紙上以液滴大小為15pL般噴射1次後,待機5分鐘並再噴射2次,反覆待機5分鐘後再噴射3次。將此反覆過程經過4次印刷之油墨,以肉眼分析評價管嘴的堵塞。○為表示相比於初期狀態無變化,△為表示部分未被印刷,×為表示完全未被抑制。The pigment dispersion liquid, the transparent resin solution, and the inkjet ink obtained in the above Examples and Comparative Examples were sprayed once on a photoprinting paper with a droplet size of 15 pL, and then stood for 5 minutes and then sprayed twice, repeatedly. Spray 5 times after 5 minutes of standby. This repetitive process was subjected to four printing inks, and the clogging of the nozzle was evaluated by visual analysis. ○ indicates that there is no change from the initial state, Δ indicates that the portion is not printed, and × indicates that the portion is not completely suppressed.
關於上述實施例1~8及比較例1~2各步驟所製作之彩色濾光片,以目視計數每100000處之缺點處數(脫白、混色),並評價。With respect to the color filters prepared in the respective steps of the above Examples 1 to 8 and Comparative Examples 1 and 2, the number of defects per 100,000 (whitening, color mixing) was visually counted and evaluated.
以雷射顯微鏡(olympus公司製)觀察所製作之彩色濾光片,並進行膜厚測定。The color filter produced was observed with a laser microscope (manufactured by Olympus Co., Ltd.), and the film thickness was measured.
使用顯微分光側光裝置(濱松Hotonix公司製,商品名「PMA-11」)測定所製作之彩色濾光片之各著色層的色度。The chromaticity of each colored layer of the produced color filter was measured using a microscopic spectroscopic side light device (manufactured by Hamamatsu Hotonix Co., Ltd., trade name "PMA-11").
前述製造例1~6所得之顏料分散液、透明樹脂溶液(透明樹脂組成物)、噴墨油墨(顏料油墨)之顏料濃度、黏度、及噴墨吐出安定性之評價結果示於表1。相比於顏料油墨,可知顏料分散液和透明樹脂溶液為以較低黏度且以噴墨吐出亦良好。Table 1 shows the evaluation results of the pigment dispersion liquid, the transparent resin solution (transparent resin composition), the inkjet ink (pigment ink) pigment concentration, the viscosity, and the ink jet discharge stability obtained in the above Production Examples 1 to 6. Compared with the pigment ink, it is understood that the pigment dispersion liquid and the transparent resin solution have a low viscosity and are excellent in inkjet discharge.
關於上述實施例1~8、比較例1~2所製作之彩色濾光片,評價有無脫白、有無混色、膜厚、及色度之結果示於表2。於比較例1所製作之彩色濾光片察見因油墨管嘴缺乏所造成的脫白,於比較例2所製作之彩色濾光片察見因油墨滲出所造成的混色,相對地,實施例1~8所製作之彩色濾光片可知無混色、脫白。The color filters prepared in the above Examples 1 to 8 and Comparative Examples 1 and 2 were evaluated in Table 2 for the results of whether or not the whitening, the presence or absence of color mixing, the film thickness, and the chromaticity were evaluated. The color filter produced in Comparative Example 1 was observed to have whitening due to lack of ink nozzles, and the color filter produced in Comparative Example 2 was observed to have color mixture due to ink bleeding. The color filters produced in 1 to 8 are known to have no color mixing and whitening.
上述表2中,「乾燥溫度(A)」表示塗佈顏料分散液後之預乾燥步驟中的乾燥溫度,「乾燥溫度(B)」為表示塗佈透明樹脂溶液後之預烘烤步驟中的乾燥溫度(熱處理溫度)。In the above Table 2, the "drying temperature (A)" indicates the drying temperature in the pre-drying step after the application of the pigment dispersion liquid, and the "drying temperature (B)" indicates the pre-baking step after the application of the transparent resin solution. Drying temperature (heat treatment temperature).
又,「固形成分比率」為表示顏料分散液與透明樹脂溶液乾燥後的固形成分比率(令混合液層硬化後之顏料與透明樹脂之固形成分比率=顏料:透明樹脂)。「溶劑之沸點」為表示顏料分散液之分散溶劑的沸點。In addition, the "solid content ratio" is a solid content ratio after drying of the pigment dispersion liquid and the transparent resin solution (solid content ratio of the pigment and the transparent resin after the mixed liquid layer is cured = pigment: transparent resin). The "boiling point of the solvent" is the boiling point of the dispersion solvent of the pigment dispersion liquid.
若根據本發明,則可使用由噴頭吐出時之直進性及安定性優良的噴墨油墨,製造具有高色純度、色再現性的彩色濾光片,故可廉價製造性能更加優良之信賴性高的彩色濾光片。特別,可製造穿透濃度大且均勻、無脫色之畫素部為精密地形成,且亮度提高的彩色濾光片。因此,經由使用如本發明方法所得之優良性能的彩色濾光片,則可以良好產率提供彩色顯示特性優良的液晶顯示元件,並且可製造高品質之液晶顯示裝置。According to the present invention, it is possible to produce a color filter having high color purity and color reproducibility by using an inkjet ink which is excellent in straightness and stability when discharged from a head, and therefore has high reliability and high reliability. Color filter. In particular, it is possible to manufacture a color filter in which a pixel portion having a large penetration density and uniformity and no discoloration is precisely formed and brightness is improved. Therefore, by using the color filter excellent in performance obtained by the method of the present invention, a liquid crystal display element excellent in color display characteristics can be provided in a good yield, and a high quality liquid crystal display device can be manufactured.
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