KR20140056406A - Method of surface coating for phosphor - Google Patents

Method of surface coating for phosphor Download PDF

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KR20140056406A
KR20140056406A KR1020120118053A KR20120118053A KR20140056406A KR 20140056406 A KR20140056406 A KR 20140056406A KR 1020120118053 A KR1020120118053 A KR 1020120118053A KR 20120118053 A KR20120118053 A KR 20120118053A KR 20140056406 A KR20140056406 A KR 20140056406A
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phosphor
silicic acid
metal ion
alkali metal
active silicic
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KR101719839B1 (en
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김유혁
박승혁
윤호신
강병규
양승규
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단국대학교 천안캠퍼스 산학협력단
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/59Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing silicon
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y10STECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract

The present invention relates to a method for coating phosphor on a surface. The method includes a step of preparing an alkaline metal ion-activated silicate complex solution and a step of forming a silica coating layer by putting the alkaline metal ion-activated silicate complex solution in a phosphor dispersion solution. The method for coating phosphor on a surface according to the present invention simplifies a coating process and can provide a silica coated phosphor with improved thermal stability and luminescent properties.

Description

형광체 표면 코팅방법{Method of surface coating for phosphor}FIELD OF THE INVENTION [0001] The present invention relates to a method for coating a phosphor,

본 발명은 형광체 표면 코팅방법 및 이 방법으로 제조된 표면 코팅된 형광체에 관한 것이다.
The present invention relates to a phosphor surface coating method and a surface-coated phosphor prepared by this method.

일반적으로 형광체는 형광램프, 복사용 램프 등과 같은 광원용, 전계발광소자, 플라즈마 디스플레이 등과 같은 표시 소자에 이용되거나 검지용 기기 등에 이용되어 왔다. 이러한 형광체는 적용 분야에 적합한 열화특성, 휘도, 색순도, 잔광특성 등을 갖기 위해서 다양한 방법들이 시도되었다. 특히, 형광체는 사용 기간 동안 수분에 의한 화학적 안정성이 좋지 않고, 장치 내에서 발생하는 열 등에 의해서 초기 광특성이 저하되어 휘도 및 색좌표 등에서 심각한 변화를 초래하는 문제점이 있다. 이러한 문제점을 해결하기 위해서 형광체의 표면에 실리콘 화합물을 코팅하는 방법이 제시되었다. 기존의 실리콘 화합물 코팅층의 형성방법은 촉매로서 염기촉매 또는 아민 및 에탄올 내에서 TEOS(tetraethylorthosilicate)의 졸-겔 공정을 이용하여 형광체 표면에 실리콘 화합물을 코팅하는 것이다. 하지만, 이러한 코팅층 형성방법은 불균일한 코팅층의 발생이 빈번하고, 염기촉매나 실란 커플링제 등과 같은 첨가제를 사용하고 있어 반응 공정이 까다롭고, 대량 생산시 제조 공정에 어려움이 있으며, 코팅 공정 과정에서 불분완전하게 반응한 에틸 그룹과 같은 유기물질이 다량 함유될 가능성이 높아 형광체 오염이 발생하고, 발광특성에 악영향을 미칠 수 있다.
BACKGROUND ART [0002] Generally, phosphors have been used for a display device such as a light source such as a fluorescent lamp and a copying lamp, an electroluminescent device, a plasma display or the like, or a detecting device. Various methods have been attempted to obtain such a phosphor having deterioration characteristics, luminance, color purity, and afterglow characteristics suitable for application fields. Particularly, the phosphor has poor chemical stability due to moisture during the use period, and the initial light characteristic is deteriorated due to heat generated in the apparatus, resulting in a serious change in luminance and chromaticity coordinates. In order to solve such a problem, a method of coating a silicon compound on the surface of a phosphor has been proposed. A conventional method of forming a silicon compound coating layer is to coat a silicon compound on the surface of a phosphor by using a base catalyst or a sol-gel process of TEOS (tetraethylorthosilicate) in amine and ethanol. However, such a method of forming a coating layer has a disadvantage in that uneven coating layers occur frequently, additives such as a base catalyst and a silane coupling agent are used, so that the reaction process is difficult, and the production process is difficult in mass production. There is a high possibility that a large amount of an organic substance such as a completely reacted ethyl group is contained, so that phosphor contamination occurs and the luminescence characteristics may be adversely affected.

상기 문제점을 해결하기 위한 본 발명의 목적은, 활성규산을 이용하여 형광체의 실리카 표면 코팅공정을 보다 단순화시키고, 균일한 실리카 코팅층을 형성시킬 수 있는 형광체 표면 코팅방법을 제공하는 것이다.
SUMMARY OF THE INVENTION An object of the present invention is to provide a phosphor surface coating method which can simplify the process of coating the surface of a phosphor with a silica using active silicic acid and form a uniform silica coating layer.

상기 목적을 달성하기 위한 본 발명의 양상은, 알칼리금속 이온-활성규산 복합체(Polysilicic acid) 용액을 제조하는 단계 및 형광체 분산액에 상기 알칼리금속 이온-활성규산 복합체를 투입하여 실리카 코팅층을 형성시키는 단계를 포함하는 형광체 표면 코팅방법에 관한 것이다.
According to an aspect of the present invention, there is provided a method for producing a phosphorous-based phosphor comprising the steps of preparing an alkali metal ion-active silicic acid solution and injecting the alkali metal ion-active silicate complex into a phosphor dispersion to form a silica coating layer To a method for coating a phosphor surface.

상기 알칼리금속 이온-활성규산 복합체(Polysilicic Acid) 용액은 활성규산에 NaOH 및 KOH 수용액을 투입하여 형성될 수 있다. 또한, 상기 알칼리금속 이온-활성규산 복합체(Polysilicic Acid) 용액의 pH는 9 내지 13일 수 있다.
The alkali metal ion-active silicic acid solution may be formed by adding an aqueous solution of NaOH and KOH to active silicic acid. In addition, the pH of the alkali metal ion-active silicic acid solution may be 9 to 13.

상기 실리카 코팅층을 형성하는 단계에서 상기 알칼리금속 이온-활성규산 복합체 용액은 상기 형광체 대 활성규산(SiO2)의 중량비 1:0.1 내지 1:5(w/w)로 투입될 수 있다.
In the step of forming the silica coating layer, the alkali metal ion-active silicic acid complex solution may be added in a weight ratio of 1: 0.1 to 1: 5 (w / w) of the phosphor to the active silicate (SiO 2 ).

상기 형광체 분산액에서 형광체의 농도는 0.1 내지 20중량%일 수 있다. 또한, 상기 형광체 분산액은 물, 및 케톤류, 에테르류, 지방족탄화수소류, 지환식탄화수소류, 방향족 탄화수소류, 에스테르류, 셀로솔브류, 셀로솔브아세테이트류, 설폭시드류 및 알코올류 유기용매로 이루어진 군에서 선택된 1종 이상을 포함할 수 있다.
The concentration of the phosphor in the phosphor dispersion may be 0.1 to 20 wt%. In addition, the phosphor dispersion may be prepared by dissolving a mixture of water and an organic solvent consisting of ketones, ethers, aliphatic hydrocarbons, alicyclic hydrocarbons, aromatic hydrocarbons, esters, cellosolves, cellosolve acetates, sulfoxides and alcohols And the like.

본 발명에 의한 형광체 표면 코팅방법은 코팅공정에서 촉매 또는 실란 커플링제 등과 같은 첨가물의 추가 없이 보다 단순화된 공정으로 형광체에 실리카 표면 처리가 가능하다. 또한, 본 발명에 의한 형광체 표면 코팅방법은 형광체 표면에 균일한 실리카 코팅층을 형성할 수 있고, 우수한 형광체 분말의 유동성 및 열적안정성 또는 화학적안정성 등을 부여하여 발광특성의 저하를 방지할 수 있다.
The phosphor surface coating method according to the present invention enables a silica surface treatment on a phosphor by a simpler process without adding additives such as a catalyst or a silane coupling agent in a coating process. In addition, the phosphor surface coating method according to the present invention can form a uniform silica coating layer on the surface of the phosphor, and can impart a fluidity, thermal stability, chemical stability, and the like of an excellent phosphor powder to prevent deterioration in luminescence properties.

도 1은 본 발명의 실시예 1에서 제조된 실리카 표면 코팅된 형광체의 TEM 이미지 및 EDS 측정결과를 나타낸 것이다.1 shows TEM images and EDS measurement results of the silica surface-coated phosphors prepared in Example 1 of the present invention.

이하, 본 발명에 관하여 보다 상세하게 설명한다.
Hereinafter, the present invention will be described in more detail.

본 발명은 형광체 표면 코팅방법을 제공하는 것이다.The present invention provides a method for coating a phosphor surface.

상기 형광체 표면 코팅방법은 활성규산으로 형광체의 표면에 균일한 실리카 코팅층을 형성하고, 형광체에 물리적 및 화학적 안정성을 제공하여 발광특성 저하를 방지할 수 있다.
The phosphor surface coating method can form a uniform silica coating layer on the surface of the phosphor with active silicic acid and provide physical and chemical stability to the phosphor to prevent a decrease in luminescence property.

상기 형광체 표면 코팅방법은 알칼리금속 이온-활성규산 복합체(Polysilicic Acid) 용액을 제조하는 단계 및 실리카 코팅층을 형성하는 단계를 포함한다.The phosphor surface coating method includes a step of preparing a solution of an alkali metal ion-active silicic acid (Polysilicic Acid) and a step of forming a silica coating layer.

상기 알칼리금속 이온-활성규산 복합체(Polysilicic Acid) 용액을 제조하는 단계는 활성규산을 제조하고, 알칼리성 수용액을 첨가하여 활성규산을 안정화시킨다. 상기 활성규산은 형광체 표면에 소수성을 부여하고, 유기그룹을 포함하지 않아 코팅 공정 중에 실리콘 화합물에서 발생하는 유기물에 의한 표면 오염 또는 이러한 오염에 따른 광학특성의 저하를 방지할 수 있다.The step of preparing the alkali metal ion-active silicic acid solution is to prepare active silicic acid and stabilize active silicic acid by adding an alkaline aqueous solution. The active silicic acid imparts hydrophobicity to the surface of the phosphor and does not contain an organic group, thereby preventing surface contamination due to organic substances generated in the silicon compound during the coating process or deterioration of optical properties due to such contamination.

보다 구체적으로, 물유리를 증류수에 혼합한 이후에 양이온 교환 수지에 통과시켜 활성규산을 제조한다. 다음으로, 상기 활성규산에 알칼리금속 수용액을 투입하고 활성규산의 pH를 9 내지 13으로 조정하여 알칼리금속 이온으로 안정화된 활성규산 복합체를 제조한다. More specifically, water glass is mixed with distilled water and then passed through a cation exchange resin to produce active silicic acid. Next, an alkali metal aqueous solution is added to the active silicic acid and the pH of activated silicic acid is adjusted to 9 to 13 to prepare an activated silicate complex stabilized with alkali metal ions.

상기 알칼리금속 수용액은 NaOH 또는 KOH 수용액일 수 있으며, 바람직하게는 NaOH 수용액일 수 있다.The alkali metal aqueous solution may be NaOH or KOH aqueous solution, preferably NaOH aqueous solution.

상기 물유리는 본 발명의 기술분야에서 알려진 것이라면 제한 없이 사용될 수 있으나, SiO2가 28 내지 40 중량%이고, Na2O가 5 내지 15중량%로 포함되는 것이 바람직하다. 또한, 상기 활성규산의 제조공정에서 물유리는 증류수에 희석하여 사용되고, 상기 물유리 대 증류수의 부피비는 1:2 내지 1:5(v/v)일 수 있다. 상기 부피비가 상기 범위 내에 포함되면 형광체 표면에 균일한 코팅층을 형성하여 열적안정성 등을 개선시킬 수 있다. The water glass may be used without limitation as long as it is known in the technical field of the present invention, but it is preferable that SiO 2 is 28 to 40% by weight and Na 2 O is 5 to 15% by weight. In addition, water glass may be diluted with distilled water in the process of producing active silicate, and the volume ratio of water glass to distilled water may be 1: 2 to 1: 5 (v / v). When the volume ratio is within the above range, a uniform coating layer may be formed on the surface of the phosphor to improve the thermal stability and the like.

상기 실리카 코팅층을 형성하는 단계는 형광체 분산액에 상기 알칼리금속 이온-활성규산 복합체(Polysilicic Acid) 용액을 적하하여 형광체 표면에 실리카 코팅층을 형성시킨다. In the step of forming the silica coating layer, the alkali metal ion-active silicic acid solution is dropped into the phosphor dispersion to form a silica coating layer on the phosphor surface.

상기 알칼리금속 이온-활성규산 복합체(Polysilicic Acid) 용액은 형광체 대 활성규산(활성규산의 SiO2의 중량)의 중량비 1:0.01 내지 1:1(w/w)로 혼합되며, 바람직하게는 1:0.15 내지 1:0.5일 수 있다.The alkali metal ion-active silicic acid solution is mixed at a weight ratio of phosphor to active silicate (weight of SiO 2 of active silicic acid) of 1: 0.01 to 1: 1 (w / w), preferably 1: 0.15 to 1: 0.5.

상기 중량비가 0.01 미만이면 형광체 표면에 충분한 실리카 코팅층이 형성되지 않아 형광체에 소수성 부여가 어려워지고, 1을 초과하면 형광체 표면에 불균일한 실리카 코팅층이 형성되거나 실리카에 의한 형광체의 뭉침 등이 발생하여 발광특성이 저하될 수 있어 바람직하지 않다.
If the weight ratio is less than 0.01, a sufficient silica coating layer is not formed on the surface of the phosphor, which makes it difficult to impart hydrophobicity to the phosphor. If the weight ratio is more than 1, a non-uniform silica coating layer is formed on the phosphor surface, Is undesirably deteriorated.

상기 형광체 분산액에서 형광체의 농도는 0.1 내지 20중량%일 수 있다. 상기 농도가 0.1 중량% 미만이면 형광체 코팅 공정의 생산성이 낮아지고, 20중량%를 초과하면 형광체들 간에 충분한 분산이 이루어지지 않아 균일한 코팅층 형성이 어렵고, 형광체의 분산을 위해서 분산제, 계면활성제 등과 같은 첨가제의 투입이 요구되어 바람직하지 않다.
The concentration of the phosphor in the phosphor dispersion may be 0.1 to 20 wt%. If the concentration is less than 0.1 wt%, the productivity of the phosphor coating process is lowered. If the concentration is more than 20 wt%, sufficient dispersion is not achieved between the phosphors, which makes it difficult to form a uniform coating layer. In order to disperse the phosphor, The addition of the additive is required.

상기 형광체는 본 기술 분야에서 알려진 형광체라면 제한 없이 사용될 수 있으며, 예를 들면, Sr5(PO4)3Cl:Eu계 형광체, BaMgAl10O17:Eu계 형광체, ZnO:Zn계 형광체, Zn2SiO4:Mn계 형광체, Zn2GeO4:Mn계 형광체, YVO4:Eu계 형광체, Y2O2S:Eu계 형광체, MgO-GeO2:Mn계 형광체, ZnS:Cu계 형광체, Y2O3:Eu계 형광체, (YGd)2O3:Eu계 형광체, LaOCl:Eu계 형광체, SrO2(Al2O3)nEu계 형광체, GaOF:Eu계 형광체, CaS:Bi계 형광체, La2O2S:Eu계 형광체, Li2Mg(MoO4):Eu,Sm계 형광체, (Ba, Sr)2SiO4:Eu계 형광체, ZnS:Cu,Al계 형광체, SrGa2S4:Eu계 형광체, Sr5(PO4)3Cl:Eu계 형광체, (SrMg)5PO4Cl:Eu계 형광체, BaMg2Al16O27:Eu계 형광체, (Y,Gd)BO3:Eu, Y(V,P)O4:Eu, (Y,Gd)2O3:Eu계 형광체, CaMgSi2O6:Eu계 형광체, CaWO4:Pb계 형광체, Y2SiO5:Eu계 형광체로 이루어진 군에서 선택된 1종 이상일 수 있으며, 이에 제한하는 것은 아니다.
For example, the phosphor may be a Sr 5 (PO 4 ) 3 Cl: Eu based phosphor, a BaMgAl 10 O 17 : Eu based phosphor, a ZnO: Zn based phosphor, a Zn 2 SiO 4: Mn-based fluorescent material, Zn 2 GeO 4: Mn-based fluorescent material, YVO 4: Eu-base phosphor, Y 2 O 2 S: Eu-based phosphors, MgO-GeO 2: Mn-based phosphor, ZnS: Cu-based fluorescent material, Y 2 O 3: Eu-based fluorescent material, (YGd) 2 O 3: Eu -based phosphors, LaOCl: Eu-based phosphors, SrO 2 (Al 2 O 3 ) n Eu -based phosphors, GaOF: Eu-base phosphor, CaS: Bi-based fluorescent material, La 2 O 2 S: Eu-based phosphors, Li 2 Mg (MoO 4) : Eu, Sm -based phosphor, (Ba, Sr) 2 SiO 4: Eu -based phosphors, ZnS : Cu, Al-base phosphor, SrGa 2 S 4: Eu-based phosphors, Sr 5 (PO 4) 3 Cl: Eu -based fluorescent material, (SrMg) 5 PO 4 Cl : Eu -base phosphor, BaMg 2 Al 16 O 27: Eu -based (Y, Gd) BO 3 : Eu, Y (V, P) O 4 : Eu, (Y, Gd) 2 O 3 : Eu phosphor, CaMgSi 2 O 6 : Eu phosphor, CaWO 4 : Pb A phosphor, and a Y 2 SiO 5 : Eu-based phosphor, but the present invention is not limited thereto.

상기 형광체 분산액에서 용매는 형광체를 분산시킬 수 있는 것이라면 제한 없이 사용될 수 있으며, 보다 구체적으로, 물, 케톤류(아세톤, 메틸에틸케톤, 메틸이소부틸케톤, 시클로헥사논 등), 에테르류(디옥산, 테트라히드로퓨란 등), 지방족탄화수소류(헥산 등), 지환식탄화수소류(시클로헥산 등), 방향족 탄화수소류(톨루엔, 크실렌 등), 에스테르류(아세트산메틸, 아세트산에틸, 아세트산부틸 등), 알콜류(에탄올, 이소프로판올, 부탄올, 시클로헥사놀 등), 셀로솔브류(메틸셀로솔브, 에틸셀로솔브 등), 셀로솔브아세테이트류, 설폭시드류(디메틸설폭시드 등) 유기용매 등으로 이루어진 군에서 선택된 1종 이상일 수 있으며, 바람직하게는 물 또는/및 에테르류 유기용매일 수 있다.
The solvent in the phosphor dispersion may be any one that can disperse the fluorescent material without limitation, and more specifically, water, ketones (acetone, methyl ethyl ketone, methyl isobutyl ketone, cyclohexanone and the like), ethers (dioxane, (Methyl acetate, ethyl acetate, butyl acetate, etc.), alcohols (such as benzene, toluene, and the like), aliphatic hydrocarbons such as hexane, alicyclic hydrocarbons such as cyclohexane, aromatic hydrocarbons such as toluene and xylene, Selected from the group consisting of ethanol, isopropanol, butanol, cyclohexanol, etc.), cellosolve (methylcellosolve, ethylcellosolve etc.), cellosolve acetates, sulfoxides (dimethylsulfoxide etc.) And may be one or more kinds, preferably water, and / or ethers.

본 발명은 상기 코팅방법으로 제조된 실리카로 표면 코팅된 형광체 및 이를 포함하는 발광소자를 제공한다. 상기 발광소자는 본 기술 분야에서 알려진 것이며, 본 발명에서는 특별히 언급하지 않는다.
The present invention provides a phosphor surface-coated with silica prepared by the coating method and a light emitting device including the same. The light emitting device is known in the art, and is not specifically referred to in the present invention.

이하, 실시예 및 비교예를 통하여 본 발명을 보다 상세히 설명한다. 이는 본 발명의 설명을 위한 것일 뿐, 이로 인해 본 발명의 범위가 제한되지 않는다.
Hereinafter, the present invention will be described in more detail with reference to examples and comparative examples. This is for the purpose of illustrating the present invention, and thus the scope of the present invention is not limited thereto.

제조예Manufacturing example 1:  One: NaOHNaOH 에 안정화된 활성규산의 제조(Preparation of stabilized activated silicic acid ( polysilicicpolysilicic acidacid ))

물유리(Sodium silicate, SiO2 30%, Na2O 10%, pH=12-13) 100ml과 탈이온수 300ml를 혼합하여 7% SiO2 물유리 수용액을 제조하였다. 상기 물유리 수용액을 양이온 교환수지 컬럼에 통과시켜 pH=2-3의 활성규산 수용액을 얻었다. 상기 활성규산 수용액에 NaOH(14 ml, 1 M)를 첨가하여 pH 9-10로 맞추어 NaOH에 안정화된 활성규산을 제조하였다.
Sodium silicate, SiO 2 30%, Na 2 O 10%, pH = 12-13) and 300 ml of deionized water were mixed to prepare a solution of 7% SiO 2 Aqueous solution of water glass was prepared. The water glass aqueous solution was passed through a cation exchange resin column to obtain an active silicic acid aqueous solution of pH = 2-3. To the activated silicate aqueous solution was added NaOH (14 ml, 1 M) to adjust the pH to 9 to 10 to prepare active silicic acid stabilized in NaOH.

제조예Manufacturing example 1:  One: KOHKOH 에 안정화된 활성규산의 제조(Preparation of stabilized activated silicic acid ( polysilicicpolysilicic acidacid ))

물유리(Sodium silicate, SiO2 30%, Na2O 10%, pH=12-13) 100ml과 탈이온수 300ml를 혼합하여 7% SiO2 물유리 수용액을 제조하였다. 상기 물유리 수용액을 양이온 교환수지 컬럼(제품명, 제조사)에 통과시켜 pH=2-3의 활성규산 수용액을 얻었다. 상기 활성규산 수용액에 KOH(1 M)를 첨가하여 pH 9-10로 맞추어 NaOH에 안정화된 활성규산을 제조하였다.
Sodium silicate, SiO 2 30%, Na 2 O 10%, pH = 12-13) and 300 ml of deionized water were mixed to prepare a solution of 7% SiO 2 Aqueous solution of water glass was prepared. The water glass aqueous solution was passed through a cation exchange resin column (product name, manufacturer) to obtain an active silicic acid aqueous solution having pH = 2-3. KOH (1 M) was added to the activated silicate aqueous solution to adjust the pH to 9 to 10 to prepare stabilized active silicic acid in NaOH.

실시예Example 1:  One: BAMBAM 형광체:활성규산(1:0.15) Phosphor: activated silicic acid (1: 0.15)

증류수 20ml에 BAM 형광체 2.5g을 혼합하여 형광체 분산액을 제조하였다. 상기 형광체 분산액에 NaOH에 안정화된 활성규산 5ml을 적하하고 혼합하여 실리카 표면 코팅된 BAM 형광체를 제조하였다.
And 20 g of distilled water and 2.5 g of BAM phosphor were mixed to prepare a phosphor dispersion. 5 ml of activated silicate stabilized with NaOH was added dropwise to the phosphor dispersion and mixed to prepare a silica surface-coated BAM phosphor.

물성특성Physical Properties

(1) TEM 이미지 및 EDS(1) TEM images and EDS

상기 실시예 및 비교예의 실리카 표면 코팅된 형광체의 TEM 이미지를 측정하여 도 1 및 3에 제시하였으며, 상기 TEM 이미지로 코팅의 균일정도를 확인하였다. 또한, 실시예 1의 TEM 이미지에서 표시 부분에 대한 EDS를 측정하여 도 1에 제시하였다.The TEM images of the phosphors coated on the surface of the silica of the examples and comparative examples were measured and shown in FIGS. 1 and 3, and the uniformity of the coating was confirmed by the TEM image. In addition, the EDS for the display portion in the TEM image of Example 1 was measured and presented in FIG.

Claims (7)

알칼리금속 이온-활성규산 복합체(Polysilicic Acid) 용액을 제조하는 단계; 및 형광체 분산액에 상기 알칼리금속 이온-활성규산 복합체 용액을 투입하여 실리카 코팅층을 형성하는 단계를 포함하는 것을 특징으로 하는 형광체 표면 코팅방법.
Preparing a solution of an alkali metal ion-active silicic acid complex (Polysilicic Acid); And injecting the alkali metal ion-activated silicate complex solution into the phosphor dispersion to form a silica coating layer.
제1항에 있어서,
상기 알칼리금속 이온-활성규산 복합체(Polysilicic Acid) 용액은 활성규산에 NaOH 및 KOH 수용액을 투입하여 형성되는 것을 특징으로 하는 형광체 표면 코팅방법.
The method according to claim 1,
Wherein the alkali metal ion-active silicic acid solution is formed by adding an aqueous solution of NaOH and KOH to active silicic acid.
제1항에 있어서,
상기 알칼리금속 이온-활성규산 복합체(Polysilicic Acid) 용액의 pH는 9 내지 13인 것을 특징으로 하는 형광체 표면 코팅방법.
The method according to claim 1,
Wherein the pH of the alkali metal ion-active silicic acid solution is from 9 to 13.
제1항에 있어서,
상기 실리카 코팅층을 형성하는 단계에서 상기 알칼리금속 이온-활성규산 복합체 용액은 상기 형광체 대 활성규산(SiO2)의 중량비 1:0.1 내지 1:5(w/w)로 투입되는 것을 특징으로 하는 형광체 표면 코팅방법.
The method according to claim 1,
The alkali metal ion in the step of forming the silica coating layer-activated silicate complex solution weight ratio of 1 of the phosphor for the active silicic acid (SiO 2): the phosphor surface characterized in that the input to 5 (w / w): 0.1 to 1 Coating method.
제1항에 있어서,
상기 형광체 분산액에서 형광체의 농도는 0.1 내지 20중량%인 것을 특징으로 하는 형광체 표면 코팅방법.
The method according to claim 1,
Wherein the concentration of the phosphor in the phosphor dispersion is 0.1 to 20 wt%.
제1항에 있어서,
상기 형광체 분산액은 물, 및 케톤류, 에테르류, 지방족탄화수소류, 지환식탄화수소류, 방향족 탄화수소류, 에스테르류, 셀로솔브류(메틸셀로솔브, 에틸셀로솔브 등), 셀로솔브아세테이트류, 설폭시드류 및 알코올류 유기용매로 이루어진 군에서 선택된 1종 이상을 포함하는 것을 특징으로 하는 형광체 표면 코팅방법.
The method according to claim 1,
The phosphor dispersion may be prepared by dissolving the above-mentioned phosphor dispersions in water or an organic solvent such as water and an organic solvent such as ketones, ethers, aliphatic hydrocarbons, alicyclic hydrocarbons, aromatic hydrocarbons, esters, cellosolve (methylcellosolve, ethylcellosolve, Wherein the phosphor is at least one selected from the group consisting of an organic solvent, an organic solvent, and an organic solvent.
제1항에 있어서,
상기 형광체는 Sr5(PO4)3Cl:Eu계 형광체, BaMgAl10O17:Eu계 형광체, ZnO:Zn계 형광체, Zn2SiO4:Mn계 형광체, Zn2GeO4:Mn계 형광체, YVO4:Eu계 형광체, Y2O2S:Eu계 형광체, MgO-GeO2:Mn계 형광체, ZnS:Cu계 형광체, Y2O3:Eu계 형광체, (YGd)2O3:Eu계 형광체, LaOCl:Eu계 형광체, SrO2(Al2O3)nEu2+계 형광체, GaOF:Eu계 형광체, CaS:Bi계 형광체, La2O2S:Eu계 형광체, Li2Mg(MoO4):Eu,Sm계 형광체, (Ba, Sr)2SiO4:Eu계 형광체, ZnS:Cu,Al계 형광체, SrGa2S4:Eu계 형광체, Sr5(PO4)3Cl:Eu계 형광체, (SrMg)5PO4Cl:Eu계 형광체, BaMg2Al16O27:Eu계 형광체, (Y,Gd)BO3:Eu, Y(V,P)O4:Eu, (Y,Gd)2O3:Eu계 형광체, CaMgSi2O6:Eu계 형광체, CaWO4:Pb계 형광체 및 Y2SiO5:Eu계 형광체로 이루어진 군에서 선택된 1종 이상인 것을 특징으로 하는 형광체 표면 코팅방법.
The method according to claim 1,
Wherein the phosphor is at least one selected from the group consisting of Sr 5 (PO 4 ) 3 Cl: Eu phosphor, BaMgAl 10 O 17 : Eu-based phosphor, ZnO: Zn-based phosphor, Zn 2 SiO 4 : Mn-based phosphor, Zn 2 GeO 4 : Mn- 4: Eu-base phosphor, Y 2 O 2 S: Eu-based phosphors, MgO-GeO 2: Mn-based phosphor, ZnS: Cu-based fluorescent material, Y 2 O 3: Eu-based fluorescent material, (YGd) 2 O 3: Eu -base phosphor , LaOCl: Eu-based phosphors, SrO 2 (Al 2 O 3 ) n Eu 2+ based phosphor, GaOF: Eu-base phosphor, CaS: Bi-based fluorescent material, La 2 O 2 S: Eu-based phosphors, Li 2 Mg (MoO 4) : Eu, Sm -based phosphor, (Ba, Sr) 2 SiO 4: Eu -based phosphors, ZnS : Cu, Al-base phosphor, SrGa 2 S 4: Eu-based phosphors, Sr 5 (PO 4) 3 Cl: Eu -based fluorescent material, (SrMg) 5 PO 4 Cl : Eu -base phosphor, BaMg 2 Al 16 O 27: Eu -based (Y, Gd) BO 3 : Eu, Y (V, P) O 4 : Eu, (Y, Gd) 2 O 3 : Eu phosphor, CaMgSi 2 O 6 : Eu phosphor, CaWO 4 : Pb Phosphor and a Y 2 SiO 5 : Eu-based phosphor.
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CN113024244A (en) * 2021-03-24 2021-06-25 山东大学 Orthophosphate thermal barrier coating material with high thermal expansion coefficient and preparation method thereof
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