KR100315112B1 - Method for manufacturing pigment-coated phosphor - Google Patents
Method for manufacturing pigment-coated phosphor Download PDFInfo
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- KR100315112B1 KR100315112B1 KR1019990014260A KR19990014260A KR100315112B1 KR 100315112 B1 KR100315112 B1 KR 100315112B1 KR 1019990014260 A KR1019990014260 A KR 1019990014260A KR 19990014260 A KR19990014260 A KR 19990014260A KR 100315112 B1 KR100315112 B1 KR 100315112B1
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- pigment
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- 239000000049 pigment Substances 0.000 title claims abstract description 95
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims description 11
- 238000004519 manufacturing process Methods 0.000 title abstract description 8
- 239000006185 dispersion Substances 0.000 claims abstract description 46
- 239000011230 binding agent Substances 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 239000005018 casein Substances 0.000 claims description 15
- BECPQYXYKAMYBN-UHFFFAOYSA-N casein, tech. Chemical compound NCCCCC(C(O)=O)N=C(O)C(CC(O)=O)N=C(O)C(CCC(O)=N)N=C(O)C(CC(C)C)N=C(O)C(CCC(O)=O)N=C(O)C(CC(O)=O)N=C(O)C(CCC(O)=O)N=C(O)C(C(C)O)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=O)N=C(O)C(CCC(O)=O)N=C(O)C(COP(O)(O)=O)N=C(O)C(CCC(O)=N)N=C(O)C(N)CC1=CC=CC=C1 BECPQYXYKAMYBN-UHFFFAOYSA-N 0.000 claims description 15
- 235000021240 caseins Nutrition 0.000 claims description 15
- 108010010803 Gelatin Proteins 0.000 claims description 14
- 229920000159 gelatin Polymers 0.000 claims description 14
- 239000008273 gelatin Substances 0.000 claims description 14
- 235000019322 gelatine Nutrition 0.000 claims description 14
- 235000011852 gelatine desserts Nutrition 0.000 claims description 14
- 229920000084 Gum arabic Polymers 0.000 claims description 5
- 241000978776 Senegalia senegal Species 0.000 claims description 5
- 235000010489 acacia gum Nutrition 0.000 claims description 5
- 239000000205 acacia gum Substances 0.000 claims description 5
- 150000001449 anionic compounds Chemical class 0.000 claims description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 15
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 6
- 239000002253 acid Substances 0.000 description 6
- 239000003513 alkali Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 239000011324 bead Substances 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 239000002356 single layer Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 3
- 229910021529 ammonia Inorganic materials 0.000 description 3
- 238000000498 ball milling Methods 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
- C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/50—Wavelength conversion elements
- H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Power Engineering (AREA)
- Luminescent Compositions (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
본 발명은 (a) 안료, 제1 결합제 및 순수를 포함하는 안료 분산액을 제조한 다음 단일 피복량 분량의 안료를 포함하는 안료 분산액 (단일 피복량 안료 분산액)으로 수등분하는 단계; (b) 형광체, 제2 결합제 및 순수를 포함하는 형광체 분산액을 제조하는 단계; (c) 상기 형광체 분산액에 상기 수등분된 단일 피복량 안료 분산액중 하나를 첨가한 다음 pH를 등전점 범위로 조절하는 단계; (d) 상기 단계 (c)의 결과물에 다른 하나의 단일 피복량 안료 분산액 및 제2 결합제를 첨가한 다음 pH를 등전점 범위로 조절하는 단계; (e) 수등분된 단일 피복량 안료 분산액이 모두 첨가될 때까지 상기 단계 (d)를 반복하는 단계; 및 (f) 상기 단계 (e)의 결과물의 pH를 등전점 범위로 조절하고 감압 여과 및 건조하는 단계를 포함하는 안료 부착 형광체의 제조방법을 제공하는 것이다. 본 발명에 따른 안료 부착 형광체의 제조방법에 따르면 다량의 안료가 부착되더라도 안료 탈락율이 크게 감소되며, 다량의 안료가 부착되는만큼 반사율이 감소된다. 따라서, 본 발명에 따라 제조된 안료 부착 형광체를 채용하는 표시장치의 경우 콘트라스트 특성을 개선할 수 있다.The present invention comprises the steps of (a) preparing a pigment dispersion comprising the pigment, the first binder and the pure water and then dividing into a pigment dispersion (single dose pigment dispersion) comprising a single dose of pigment; (b) preparing a phosphor dispersion comprising the phosphor, the second binder and the pure water; (c) adding one of the equally divided single dose pigment dispersions to the phosphor dispersion and then adjusting the pH to an isoelectric point range; (d) adding another single dose pigment dispersion and a second binder to the result of step (c) and then adjusting the pH to an isoelectric point range; (e) repeating step (d) until all of the equally divided single dose pigment dispersions are added; And (f) adjusting the pH of the resultant product of step (e) to an isoelectric point range, and filtration and drying under reduced pressure. According to the method of manufacturing the pigment-attached phosphor according to the present invention, even if a large amount of pigment is attached, the pigment dropout rate is greatly reduced, and the reflectance is reduced as much of the pigment is attached. Accordingly, in the case of a display device employing a phosphor with a pigment manufactured according to the present invention, contrast characteristics can be improved.
Description
본 발명은 안료 부착 형광체에 관한 것으로서, 보다 상세하게는 다단계 방식에 따라 다량의 안료를 부착시킬 수 있는 안료부착형광체의 제조방법에 관한 것이다.BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a pigment with phosphor, and more particularly, to a method for producing a pigment with phosphor capable of attaching a large amount of pigments in a multi-step manner.
형광체는 대부분 그 자체가 백색을 띠는 물질로서, 외부로부터의 빛을 반사하는 성질을 가지고 있다. 따라서 이러한 형광체를 그대로 표시소자의 칼라구현층으로 적용하는 경우에는 화상의 콘트라스트를 저하시키는 문제점이 있다. 이러한 문제점을 해결하기 위하여 형광체 표면에 안료를 부착하는 방법이 제안되었다.Phosphors are mostly white in themselves and have a property of reflecting light from the outside. Therefore, when such a phosphor is used as a color implementation layer of a display device as it is, there is a problem of reducing the contrast of an image. In order to solve this problem, a method of attaching a pigment to the surface of the phosphor has been proposed.
도 1은 통상적인 안료 부착 방법을 순차적으로 도시한 것이다. 도 1을 참조하여 통상의 안료 부착 형광체의 제조방법을 설명하면 다음과 같다:1 illustrates a conventional pigment deposition method sequentially. Referring to Figure 1 describes a conventional method for producing a phosphor with a pigment:
먼저, 안료(20)와 아라비아 고무(30)를 볼밀하면서 혼합하여 안료 분산액을 제조한다. (도 1a).First, the pigment 20 and the gum arabic 30 are mixed while ball milling to prepare a pigment dispersion. (FIG. 1A).
이어서, 상기 안료 분산액에 형광체(10)와, 젤라틴 또는 카제인으로부터 선택된 결합제(40)를 첨가한다 (도 1b).Subsequently, phosphor 10 and binder 40 selected from gelatin or casein are added to the pigment dispersion (FIG. 1B).
마지막으로, 적당한 산 또는 알칼리를 가하여 pH를 등전점으로 조절하고 글루타르알데하이드와 같은 경화제를 가하여 냉동경화시킨후, 상등액을 제거하고 얻어지는 침전물을 수세척, 감압 여과 및 건조하면 안료 부착 형광체가 수득된다 (도 1c 내지 1d).Finally, the pH is adjusted to an isoelectric point by the addition of a suitable acid or alkali and freeze-cured by the addition of a curing agent such as glutaraldehyde, and then the supernatant is removed and the resulting precipitate is washed with water, filtered under reduced pressure and dried to obtain a pigment-containing phosphor. 1C-1D).
이러한 통상의 안료 부착 형광체의 제조방법에 있어서, 상기 아라비아 고무, 젤라틴, 카제인 등과 같은 수용성 고분자가 물에 용해되고 pH가 소정 범위 (예를 들면, 약 4 내지 5)로 조절되면 젤라틴 또는 카제인과 아라비아검은 콜로이드를 형성한다. 이렇게 형성된 콜로이드와, 안료와, 형광체사이의 반데르 바알스 힘에 의하여 형광체 표면에 안료가 부착되어 있게 된다.In such a conventional method for preparing a pigment-containing phosphor, gelatin or casein and arabian are dissolved when the water-soluble polymer such as gum arabic, gelatin, casein is dissolved in water and the pH is adjusted to a predetermined range (for example, about 4 to 5). Black colloids form. The pigment is attached to the surface of the phosphor by the van der Waals forces between the colloid, the pigment, and the phosphor thus formed.
그러나, 이러한 통상의 안료 부착 방법은 부착되는 안료의 양이 소량인 경우, 즉 단일층 이하의 안료량인 경우에만 사용가능하며, 반사율 감소를 위해 안료량을 단일층 도포 용량 이상으로 증가시키게 되면 안료간의 응집이 심해지면서 안료 탈락 현상이 과다하여 후속의 공정에서 막 불량을 일으키게 된다.However, this conventional pigment deposition method can be used only when the amount of pigment to be attached is small, that is, when the amount of pigment is less than a single layer, and if the pigment amount is increased above the single layer coating capacity to reduce the reflectance, As the aggregation of the liver becomes more severe, the pigment dropout phenomenon becomes excessive, resulting in film defects in subsequent processes.
본 발명이 이루고자 하는 기술적 과제는 전술한 바와 같은 문제점을 극복하여 과량의 안료를 여러번에 나누어 순차적으로 부착함으로써 안료 탈락 현상을 현저하게 개선한 안료 부착 형광체의 제조방법을 제공하는 것이다.SUMMARY OF THE INVENTION The present invention has been made in an effort to provide a method for producing a phosphor with a pigment, which significantly improves a pigment dropping phenomenon by overcoming the above-described problems by dividing an excess of pigment in a plurality of times in order.
도 1a 내지 1d는 통상의 안료 부착 형광체의 제조방법을 설명하기 위한 개략도이다.1A to 1D are schematic diagrams for explaining a conventional method for producing a pigment-containing phosphor.
도 2a 내지 2f는 본 발명에 따른 안료 부착 형광체의 제조방법을 설명하기 위한 개략도이다.2A to 2F are schematic diagrams for explaining a method for producing a pigment-containing phosphor according to the present invention.
도 3은 본 발명의 실시예에 따른 안료 부착 형광체 및 종래의 안료 부착 형광체의 반사율을 도시한 그래프이다.3 is a graph showing reflectances of the pigment with phosphor and the conventional pigment with phosphor according to the embodiment of the present invention.
*도면의 주요부분에 대한 부호의 설명** Description of the symbols for the main parts of the drawings *
10... 형광체 20... 안료10 ... Phosphor 20 ... Pigment
30... 아라비아 고무 40... 젤라틴 또는 카제인30 ... Arabian rubber 40 ... Gelatin or casein
본 발명의 기술적 과제는, (a) 안료, 제1 결합제 및 순수를 포함하는 안료 분산액을 제조하는 단계; (b) 형광체, 제2 결합제 및 순수를 포함하는 형광체 분산액을 제조하는 단계; (c) 상기 형광체 분산액에 안료 분산액을 첨가하여 혼합 분산액을 제조하는 단계; (d) 상기 단계 (c)의 결과물에 제2 결합제 및 안료 분산액을 첨가한 다음, pH를 조절하는 단계; (e) 상기 단계 (d)를 반복하는 단계; 및 (f) 상기 단계 (e)의 결과물의 pH를 조절하고 감압 여과 및 건조하는 단계를 포함하는 안료 부착 형광체의 제조방법에 의하여 이루어질 수 있다.Technical problem of the present invention, (a) preparing a pigment dispersion comprising the pigment, the first binder and the pure water; (b) preparing a phosphor dispersion comprising the phosphor, the second binder and the pure water; (c) adding a pigment dispersion to the phosphor dispersion to prepare a mixed dispersion; (d) adding a second binder and a pigment dispersion to the result of step (c), and then adjusting the pH; (e) repeating step (d); And (f) adjusting the pH of the resultant product of step (e), filtering under reduced pressure, and drying.
본 발명에 따른 안료 부착 형광체의 제조방법에 있어서, 제1 결합제는 폴리카르복실계 음이온성 화합물 또는 아라비아 고무이며 그 함량은 안료의 총중량에 대하여 0.04∼4.0중량%인 것이 바람직하고, 제2 결합제는 젤라틴 또는 카제인이며 그 함량은 형광체의 총중량에 대하여 0.1∼3중량%인 것이 바람직하다.In the method for producing a pigment with phosphor according to the present invention, the first binder is a polycarboxylic anionic compound or gum arabic, and its content is preferably 0.04 to 4.0% by weight based on the total weight of the pigment, and the second binder is It is preferable that it is gelatin or casein and the content is 0.1 to 3 weight% with respect to the total weight of a fluorescent substance.
상기 단계 (d)에서 pH는 산 또는 알칼리의 첨가에 의해 제어될 수 있으며, 제2 결합제가 젤라틴인 경우에는 3.0∼4.0으로, 카제인인 경우에는 6.0∼8.0으로 조절된다.In step (d) the pH can be controlled by the addition of an acid or an alkali and is adjusted to 3.0 to 4.0 if the second binder is gelatin and 6.0 to 8.0 for casein.
또한, 상기 단계 (f)에서 pH는 5.0∼6.0범위로 조절되는 것이 바람직하다.In addition, the pH in step (f) is preferably adjusted to 5.0 to 6.0 range.
이하, 도 2a 내지 도 2f를 참조하여 본 발명에 따른 안료 부착 형광체의 제조방법을 보다 상세하게 설명하기로 한다:Hereinafter, a method of preparing a pigment-containing phosphor according to the present invention will be described in more detail with reference to FIGS. 2A to 2F:
먼저, 안료(20), 폴리카르복실계 음이온성 화합물 또는 아라비아 고무로부터 선택된 결합제(30'), 및 글라스 비드, 알루미나 볼 등과 같은 볼밀 매체 (미도시)를 순수와 함께 교반하에 혼합하여 안료 분산액을 제조한다 (도 2a).First, the pigment 20, a binder 30 'selected from a polycarboxylic anionic compound or gum arabic, and a ball mill medium (not shown) such as glass beads, alumina balls, etc. are mixed with pure water under stirring to prepare a pigment dispersion. To manufacture (FIG. 2A).
이어서, 형광체(10), 볼밀매체(미도시) 및 젤라틴 또는 카제인으로부터 선택된 결합제(40)를 순수와 함께 교반하에 혼합하거나, 미리 볼밀링된 형광체를 순수, 및 젤라틴 또는 카제인으로부터 선택된 결합제와 혼합한 다음 산을 가하여 pH를 소정 범위로 조절하여 형광체 분산액을 제조한다. 여기서, 결합제로서 젤라틴이 사용되는 경우에는 염산 또는 초산과 같은 산을 가하여 pH를 3.0∼4.0 범위로, 카제인이 사용되는 경우에는 암모니아와 같은 알칼리를 가하여 pH를 6.0∼8.0 범위로 조절하는 것이 바람직하다 (도 2b).Subsequently, the binder 10 selected from the phosphor 10, the ball mill medium (not shown) and the gelatin or casein is mixed with pure water under stirring, or the preball milled phosphor is mixed with the pure water and the binder selected from gelatin or casein. The acid is then added to adjust the pH to a predetermined range to prepare a phosphor dispersion. Here, when gelatin is used as a binder, it is preferable to adjust the pH to a range of 3.0 to 4.0 by adding an acid such as hydrochloric acid or acetic acid, and when using casein, an alkali such as ammonia to adjust the pH to a range of 6.0 to 8.0. (FIG. 2B).
이렇게 제조된 형광체 분산액에 안료 분산액을 첨가하여 혼합 분산액을 제조하고, 이 혼합 분산액에 적당한 산 또는 알칼리를 가하여 pH를 3.0∼8.0으로 조절한다. 이때, 안료 분산액중 안료의 함량은 단층피복량이다 (도 2c).A pigment dispersion is added to the phosphor dispersion thus prepared to prepare a mixed dispersion, and an appropriate acid or alkali is added to the mixed dispersion to adjust the pH to 3.0 to 8.0. At this time, the pigment content in the pigment dispersion is a monolayer coating amount (Fig. 2c).
다음으로, 상기 혼합 분산액에 다시 단층피복량의 안료를 포함하는 안료 분산액과, 젤라틴 또는 카제인으로부터 선택된 결합제를 첨가하고, 첨가되는 결합제의 종류에 따라 적당한 산 또는 알칼리를 가하여 pH를 3.0∼8.0으로 조절하는 단계를 목적하는 양만큼의 안료가 형광체에 부착될 때까지 소정 횟수만큼 반복한다 (도 2d).Next, to the mixed dispersion, a pigment dispersion containing a single layer coating amount of pigment and a binder selected from gelatin or casein are added, and an appropriate acid or alkali is added according to the type of binder added to adjust the pH to 3.0 to 8.0. The step of repeating is repeated a predetermined number of times until the desired amount of pigment is attached to the phosphor (FIG. 2D).
마지막으로, 상기 결과물을 경화시킨후 순수로 세정하여 pH를 5.0∼6.0으로 조절한 다음, 감압여과하고 건조하여 다량의 안료가 다층으로 부착된 안료 부착 형광체를 수득한다 (도 2e 내지 2f).Finally, the resultant is cured and washed with pure water to adjust the pH to 5.0 to 6.0, and then filtered under reduced pressure and dried to obtain a pigment with phosphor attached with a large amount of pigments (FIGS. 2E to 2F).
이렇게 형성된 안료 부착 형광체는 동일량의 안료를 부착시킨 기존의 안료 부착 형광체에 비하여 반사율이 10% 이상 저하됨으로써 이를 채용하는 스크린막의 콘트라스트 특성을 개선하는 반면, 안료 탈락 현상은 약 1/50 수준으로 감소되었다.Thus formed pigment-attached phosphors have a 10% or more reduction in reflectance compared to conventional pigment-attached phosphors with the same amount of pigment, thereby improving the contrast characteristics of the screen film employing the same, while the pigment dropout is reduced to about 1/50. It became.
이하, 실시예 및 비교예를 들어 본 발명을 보다 상세하게 설명할 것이나, 본 발명이 이로써 한정되지는 않는다.Hereinafter, although an Example and a comparative example are given and this invention is demonstrated in detail, this invention is not limited to this.
먼저, 하기 실시예 및 비교예에서 얻어지는 안료 부착 형광체에 대하여 하기와 같이 안료 탈락율 및 반사율을 측정하였다.First, the pigment dropping rate and reflectance were measured about the fluorescent substance with pigment obtained by the following example and the comparative example as follows.
1) 안료 탈락율 측정1) Pigment dropout rate measurement
1999년 4월 15일자로 출원되어 계류중인 한국특허출원번호 제99-13319호에 개시된 방법에 따라서 안료 탈락율을 측정한다.The pigment dropout rate is measured according to the method disclosed in the pending Korean Patent Application No. 99-13319, filed April 15, 1999.
2) 반사율 측정2) reflectance measurement
형광체 5g을 칭량하여 침강법을 이용하여 막을 만든다. 상기 형성된 막의 확산반사를 이용, 반사율을 측정한다.5 g of the phosphor is weighed to form a film by sedimentation. The reflectance is measured using the diffuse reflection of the formed film.
실시예 1Example 1
25g의 CoO·Al2O3, 100g의 순수, 350g의 글라스 비이드를 500㎖ 들이 용기에 넣고 여기에 0.1g의 오로탄 (Orotan, Rohm & Haas 제품)을 첨가한후 3일 동안 60rpm에서 볼밀하여 안료 분산액을 제조하였다.Into a 500 ml container containing 25 g of CoO · Al 2 O 3 , 100 g of pure water, 350 g of glass beads, add 0.1 g of Orotan (from Orotan, Rohm & Haas) and ball mill at 60 rpm for 3 days. To prepare a pigment dispersion.
이어서, 청색 발광 형광체인 ZnS:Ag, Cl 200g을 미리 볼밀하고, 여기에 400g의 순수 및 20g의 1% 젤라틴 수용액을 첨가하여 교반한후 20% 초산을 가하여 pH를 3.2로 조절하여 형광체 분산액을 제조하였다.Subsequently, ball-milling ZnS: Ag and Cl 200g, which are blue light-emitting phosphors, was preliminarily added thereto, followed by stirring with 400 g of pure water and 20 g of 1% gelatin aqueous solution, followed by 20% acetic acid to adjust pH to 3.2 to prepare a phosphor dispersion. It was.
상기 수득된 형광체 분산액에 20g의 안료분산액을 투입하고 충분히 혼합하고 20% 초산을 첨가하여 pH가 3.8이 되도록 조절하였다.20 g of a pigment dispersion was added to the obtained phosphor dispersion, mixed sufficiently, and 20% acetic acid was added to adjust the pH to 3.8.
이어서, 상기 혼합 분산액에 60g의 1% 젤라틴 수용액과 20g의 안료분산액을 재투입하고 충분히 교반한 다음, 20% 초산을 첨가하여 pH를 3.2로 조절한 다음, 글루타르알데하이드를 첨가하여 5℃에서 1시간 동안 냉동경화시키고 순수로 세정하여 pH를 5.6으로 조절한다. 세정후 수분리를 실시하고 110℃에서 48시간 동안 건조시켜서 안료가 다층으로 부착된 안료 부착 형광체를 생성물로서 수득하였다.Subsequently, 60 g of a 1% gelatin aqueous solution and 20 g of a pigment dispersion were added to the mixed dispersion and stirred sufficiently, and then the pH was adjusted to 3.2 by addition of 20% acetic acid, followed by addition of glutaraldehyde to 1 at 5 ° C. Freeze hardening for hours and washing with pure water to adjust the pH to 5.6. After washing, water separation was carried out and dried at 110 ° C. for 48 hours to obtain a pigment with phosphor attached as a multilayer product as a product.
얻어진 안료 부착 형광체에 대한 안료 탈락율을 측정하여 하기 표 1에 나타내었으며, 반사율을 측정하여 도 3의 a로서 나타내었다.The pigment dropping rate of the obtained pigment-containing phosphor was measured and shown in Table 1 below. The reflectance was measured and shown as a in FIG. 3.
실시예 2Example 2
25g의 CoO·Al2O3, 100g의 순수, 350g의 글라스 비이드를 500㎖ 들이 용기에 넣고 여기에 0.1g의 오로탄 (Orotan, Rohm & Haas 제품)을 첨가한후 3일 동안 60rpm에서 볼밀하여 안료 분산액을 제조하였다.Into a 500 ml container containing 25 g of CoO · Al 2 O 3 , 100 g of pure water, 350 g of glass beads, add 0.1 g of Orotan (from Orotan, Rohm & Haas) and ball mill at 60 rpm for 3 days. To prepare a pigment dispersion.
이어서, 청색 발광 형광체인 ZnS:Ag, Cl 200g을 미리 볼밀하고, 여기에 400g의 순수 및 20g의 1% 카제인 수용액을 첨가하여 교반한후 10% 암모니아를 가하여 pH를 6.0으로 조절하여 형광체 분산액을 제조하였다.Subsequently, 200 g of ZnS: Ag and Cl, which are blue light emitting phosphors, were preliminarily milled, and 400 g of pure water and 20 g of 1% casein solution were added thereto, followed by stirring. It was.
상기 수득된 형광체 분산액에 20g의 안료분산액을 투입하고 충분히 혼합한 다음 10% 암모니아를 첨가하여 pH가 6.0이 되도록 조절하였다.20 g of the pigment dispersion was added to the obtained phosphor dispersion, mixed well, and then adjusted to pH 6.0 by adding 10% ammonia.
이어서, 상기 혼합 분산액에 60g의 1% 카제인 수용액과 20g의 안료분산액을 재투입하고 충분히 교반한 다음, 10% 암모니아를 첨가하여 pH를 7.0으로 조절한 다음, 글루타르알데하이드를 첨가하여 5℃에서 1시간 동안 냉동경화시키고 순수로 세정하여 pH를 5.6으로 조절한다. 세정후 수분리를 실시하고 110℃에서 48시간 동안 건조시켜서 안료가 다층으로 부착된 안료 부착 형광체를 생성물로서 수득하였다.Subsequently, 60 g of a 1% casein aqueous solution and 20 g of a pigment dispersion were added to the mixed dispersion and sufficiently stirred, and then the pH was adjusted to 7.0 by adding 10% ammonia, followed by addition of glutaraldehyde to 1 at 5 ° C. Freeze hardening for hours and washing with pure water to adjust the pH to 5.6. After washing, water separation was carried out and dried at 110 ° C. for 48 hours to obtain a pigment with phosphor attached as a multilayer product as a product.
얻어진 안료 부착 형광체에 대하여 안료 탈락율을 측정하여 하기 표 1에 나타내었으며, 반사율을 측정하여 도 3의 b로서 나타내었다.The pigment dropping rate of the obtained pigment-containing phosphor was measured and shown in Table 1 below. The reflectance was measured and shown as b in FIG. 3.
비교예 1Comparative Example 1
25g의 CoO·Al2O3(?), 100g의 순수, 350g의 글라스 비이드를 500㎖ 들이 용기에 넣고 여기에 0.1g의 오로탄 (Orotan, Rohm & Haas 제품)을 첨가한후 3일 동안 60rpm에서 볼밀하여 안료 분산액을 제조하였다.Place 25 g of CoO · Al 2 O 3 (?), 100 g of pure water, 350 g of glass beads in a 500 ml container, and add 0.1 g of Orotan (Orotan, Rohm & Haas) for 3 days. Ball milling was carried out at 60 rpm to prepare a pigment dispersion.
제조된 안료 분산액 40g을 200g의 ZnS:Ag, Cl 및 60g의 1% 카제인 수용액과 혼합한 다음, 20% 초산을 가하여 pH를 3.8로 조절하였다.40 g of the pigment dispersion prepared were mixed with 200 g of ZnS: Ag, Cl and 60 g of a 1% casein aqueous solution, and then 20% acetic acid was added to adjust the pH to 3.8.
이어서, 글루타르알데하이드를 가하여 1시간 동안 냉동경화시킨후, 수세척하고 여과 및 건조시켜서 안료 부착 형광체를 수득하였다.Subsequently, glutaraldehyde was added and freeze-cured for 1 hour, followed by washing with water, filtration and drying to obtain a pigment attached phosphor.
얻어진 안료 부착 형광체에 대하여 안료 탈락율을 측정하여 하기 표 1에 나타내었으며, 반사율을 측정하여 도 3의 c로서 나타내었다.The pigment dropping rate of the obtained pigment-containing phosphor was measured and shown in Table 1 below, and the reflectance was measured and shown as c in FIG. 3.
상기 표 1로부터 알 수 있듯이, 본 발명에 따라 제조된 안료 부착 형광체는 안료 탈락율이 상당히 낮은 것을 알 수 있다.As can be seen from Table 1, the pigment-attached phosphor prepared according to the present invention can be seen that the pigment dropout rate is very low.
또한, 도 3으로부터 알 수 있듯이, 본 발명에 따른 안료 부착 형광체 (도 3의 a 및 b)는 통상의 안료 부착 형광체 (도 3의 c)에 비하여 반사율이 낮기 때문에 콘트라스트 특성이 개선되는 효과를 얻을 수 있다.In addition, as can be seen from Figure 3, the pigment-containing phosphors (a and b of Figure 3) according to the present invention has an effect of improving the contrast characteristics because the reflectance is lower than that of the conventional pigmented phosphor (c of Figure 3) Can be.
본 발명에 따른 안료 부착 형광체의 제조방법에 따르면 다량의 안료가 부착되더라도 안료 탈락율이 크게 감소되며, 다량의 안료가 부착되는만큼 반사율이 감소된다. 따라서, 본 발명에 따라 제조된 안료 부착 형광체를 채용하는 표시장치의 경우 콘트라스트 특성이 개선될 수 있다.According to the method of manufacturing the pigment-attached phosphor according to the present invention, even if a large amount of pigment is attached, the pigment dropout rate is greatly reduced, and the reflectance is reduced as much of the pigment is attached. Therefore, in the case of a display device employing a phosphor with a pigment prepared according to the present invention, the contrast characteristic can be improved.
Claims (6)
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