KR20110112720A - Multi-coated phosphors and manufacturing method thereof - Google Patents

Multi-coated phosphors and manufacturing method thereof Download PDF

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KR20110112720A
KR20110112720A KR1020100032004A KR20100032004A KR20110112720A KR 20110112720 A KR20110112720 A KR 20110112720A KR 1020100032004 A KR1020100032004 A KR 1020100032004A KR 20100032004 A KR20100032004 A KR 20100032004A KR 20110112720 A KR20110112720 A KR 20110112720A
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oxide
colloidal
phosphor
coated
mixture
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KR101139542B1 (en
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손상호
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경북대학교 산학협력단
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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
    • 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

Abstract

The present invention relates to multi-coated phosphors and methods for their preparation.
The present invention provides a multi-coated phosphor characterized in that the surface is coated with two or more oxides selected from the group consisting of silicon oxide, yttrium oxide, aluminum oxide and zinc oxide.
In addition, the present invention is a colloidal silicon oxide (SiO 2 ), colloidal yttrium oxide (Y 2 O 3 ), colloidal aluminum oxide (Al 2 O 3 ), colloidal zinc oxide (ZnO) selected from two or more colloidal oxides Mixing the distilled water to prepare a colloidal oxide mixed solution; Preparing a colloidal oxide-phosphor mixture by mixing phosphors with the colloidal oxide mixture; And it provides a method for producing a multi-coated phosphor, characterized in that it comprises the step of raising the pH step by step with respect to the colloidal oxide-phosphor mixture mixture, followed by drying.
When the multi-coated phosphor of the present invention is used for a display material or an illumination, it has a high light transmittance with respect to ultraviolet rays incident from the outside and at the same time shows a high light transmittance with respect to the visible light emitted from the phosphor, thereby providing excellent luminous efficiency.

Description

Multi-Coated Phosphors and Manufacturing Method Thereof

The present invention relates to multi-coated phosphors and methods for their preparation.

More particularly, the present invention relates to a multi-coated phosphor having a high light transmittance with respect to ultraviolet rays incident from the outside and a high light transmittance even with visible light emitted from the phosphor at the same time, and a method of manufacturing the same.

In the field of display, there is a need for a highly efficient phosphor suitable for determining image display quality and reducing driving power. Phosphors are used not only for plasma display panels (PDPs), which are attracting attention as high-definition large-screen flat panel display devices, but also for CCFL, EEFL, and FFL (Fluorescent Flat Lamps), which are LCD backlight unit (BLU) lamps. Development is very important when you think about the whole display area.

The structure of a general phosphor used for a display depends on the type.

Although somewhat different, as shown in FIG. 1, the phosphor 1 alone is usually formed without surface coating.

Examples of the blue light-emitting fluorescent substance of the phosphor is BaMgAl 10 O 17 in a small amount of BaMgAl 10 O 17 added with Eu 2+ activator of the matrix: The number of the Eu 2 + there was a situation that requires the brightness improvement and improved degradation and life characteristics . Blue light emission emits light, while the active agents Eu 2 + ions present in the Ba 2 + place transition 5d-4f. Since 5d electrons are contained in the excited state, the light emission position changes slightly due to the change of crystal field, that is, the distortion of the structure or lattice point. Therefore, as Ba 2 + is substituted with Sr 2 + , the ion radius decreases and the size of the crystal field changes. That is, as the Sr 2 + / Ba 2 + molar ratio increases, the intensity of the crystal field increases and the emission spectrum shifts toward the longer wavelength. Further, when increasing the amount of Al + 3 is also the light emission spectrum is also moved to the long wavelength side. Therefore, slight changes in the matrix composition affect the color and brightness of the phosphor.

Referring to FIG. 2, when ultraviolet light (VU) is incident on the phosphor 1, electrons of the phosphor are excited, and the excited electrons fall back to the ground state, and the energy is reduced while the phosphor emits light in the visible region. ) In this case, the phosphor 1 emits light mainly in the specific region 2 of the distance d near the surface. Therefore, depending on the state of the surface of the phosphor, the light generated may or may not be emitted.

Referring to FIG. 3, when the angle of the light emitted from the visible region generated by the phosphor is greater than a specific angle θ with respect to the central axis, the light is totally reflected and cannot come out.

Therefore, in order to improve the performance of the display, various methods for improving the lifetime and the light emitting characteristics of the phosphor have been studied. Such improvement methods include methods of synthesizing spherical phosphors, synthesizing nanophosphors, and surface modification of phosphors.

A surface coating method can be used as the phosphor surface modification method for improving the lifetime and luminescence properties of the phosphor, and in this case, a metal oxide coating method can be considered as a representative. However, even in this case, in the case of the phosphor coated with the metal oxide 3 on the phosphor 1, one layer is less likely to come out of the generated light. More specifically, the probability that light generated in the phosphor comes out depends on the surface state of the metal oxide layer 3. 4 shows the path of light generated near the surface of the phosphor according to the surface state of the single oxide layer. When the surface of the oxide layer 3 coated on the surface of the phosphor 1 is smooth as shown in FIG. 4 (a), when the surface of the oxide layer 3 is smooth, the light generated from the phosphor is totally reflected from the surface of the oxide layer to exit the oxide layer 3. it's difficult. As shown in (b) and (c) of FIG. 3, as the surface state of the oxide layer 3 becomes rougher on the surface of the phosphor 1, the total reflectance decreases and the scattering degree on the surface becomes larger. Thus, visible light generated in the phosphor It is more likely to be released out.

In order to solve the problem of such a smooth single oxide layer, the production of a rough surface oxide coating is required.

In order to solve the above problems, the present invention is directed to ultraviolet light incident from the outside.

The present invention provides a novel multi-coated phosphor having a high light transmittance and a rough surface having a high light transmittance even for visible light emitted from the phosphor and a method of manufacturing the same.

In order to solve the above problems, the present invention provides a multi-coated phosphor characterized in that the surface is coated with two or more oxides selected from the group consisting of silicon oxide, yttrium oxide, aluminum oxide and zinc oxide.

In addition, the present invention is a colloidal silicon oxide (SiO 2 ), colloidal yttrium oxide (Y 2 O 3 ), colloidal aluminum oxide (Al 2 O 3 ), colloidal zinc oxide (ZnO) selected from two or more colloidal oxides Mixing the distilled water to prepare a colloidal oxide mixed solution; Preparing a colloidal oxide-phosphor mixture by mixing phosphors with the colloidal oxide mixture; And it provides a method for producing a multi-coated phosphor, characterized in that it comprises the step of raising the pH step by step with respect to the colloidal oxide-phosphor mixture mixture, followed by drying.

When the multi-coated phosphor of the present invention is used for display materials or lighting, it has a high light transmittance against ultraviolet rays incident from the outside and at the same time shows a high light transmittance even for visible light emitted from the phosphor, thereby providing excellent light emission efficiency.

1 is a schematic diagram showing conventional uncoated phosphor particles used in flat panel displays.
2 is a schematic diagram showing that visible light is emitted after electrons of a phosphor are excited by incident ultraviolet (UV) light;
Figure 3 is a schematic diagram showing whether the transmission according to the angle of visible light emitted from the phosphor.
4 is a schematic diagram showing a path of visible light emitted from a phosphor coated with an oxide coating 3 according to a surface state.
Figure 5 is a schematic diagram showing an oxide double coated phosphor according to an embodiment of the present invention.
6 is a SEM (electron microscope) photograph (a) of a blue phosphor before oxide double coating according to Example 1 of the present invention, and a SEM photograph (b) of a blue phosphor after oxide double coating.
7 is a SEM photograph (a) of the red phosphor before the oxide double coating according to Example 3 of the present invention and a SEM photograph (b) of the red phosphor after the oxide double coating.
8 is a SEM photograph (a) of the green phosphor before the oxide double coating according to Example 4 of the present invention and a SEM photograph (b) of the green phosphor after the oxide double coating.

The present invention adopts a method of surface modification as a method for improving the efficiency and lifetime of phosphors used in flat panel displays and the like, and provides a multi-coated phosphor by applying a method of surface coating with two or more kinds of oxides.

One embodiment of the present invention is a surface coating with two or more oxides selected from the group consisting of silicon oxide (SiO 2 ), yttrium oxide (Y 2 O 3 ), aluminum oxide (Al 2 O 3 ) and zinc oxide (ZnO). It is a multi-coated phosphor characterized in that.

When the two or more oxides are multi-coated on the phosphor, that is, when two or more oxides are simultaneously coated, the colloidal state is simultaneously decreased due to the difference in physical properties in the colloidal state, that is, due to the zeta potential difference between the colloidal oxides. Collapses and causes coating to proceed irregularly. 5 and As shown in the SEM photograph of FIG. 6B, a multi-coated phosphor having an oxide layer in the form of a rough surface is formed, and thus serves to increase light transmittance.

Accordingly, when the multi-coated phosphor of the present invention is applied to a display or the like, visible light generated near the surface of the phosphor is not emitted to the inside of the phosphor but is more likely to be emitted to the outside, thereby exhibiting a brightness enhancement effect.

In addition, BaMgAl 10 O 17 , a blue phosphor used for lamps and the like, when two or more oxides are multi-coated on a phosphor, that is, two or more oxides are simultaneously coated to form a phosphor having an oxide layer having a rough surface. : Eu 2 + phosphor is also serves to prevent developer reacts with Hg discharge gas to the luminous life of the phosphor is significantly reduced.

The surface roughness of two or more oxide-coated phosphors according to the present invention

It is possible to check the surface by taking a SEM photograph and to increase the light transmittance due to the increase in surface roughness.

The present invention also provides a method for producing a multi-coated phosphor.

The method for producing a multi-coated phosphor of the present invention is selected from colloidal silicon oxide (SiO 2 ), colloidal yttrium oxide (Y 2 O 3 ), colloidal aluminum oxide (Al 2 O 3 ), colloidal zinc oxide (ZnO) Mixing two or more colloidal oxides in distilled water to prepare a colloidal oxide mixed solution; Preparing a colloidal oxide-phosphor mixture by mixing phosphors with the colloidal oxide mixture; And a step of raising the pH with respect to the colloidal oxide-phosphor mixture and stirring and drying the mixture.

Unlike the conventional oxide coating process using a sol-gel method, the method for preparing a multi-coated phosphor of the present invention is the silicon oxide (SiO 2 ), yttrium oxide (Y 2 O 3 ), aluminum oxide (Al 2 O 3 ), In order to coat the oxides such as zinc oxide (ZnO) on the phosphor efficiently, the pH is adjusted so that two or more oxides can be coated at the same time in a simple process.

In the present invention, a colloidal oxide is used as a precursor to apply a suitable pH to the material to multi-coat the phosphor. More specifically, the manufacturing method of the multi-coated phosphor of the present invention The modified sol-gel process involves the following steps.

First, at least two colloidal oxides selected from colloidal silicon oxide (SiO 2 ), colloidal yttrium oxide (Y 2 O 3 ), colloidal aluminum oxide (Al 2 O 3 ), and colloidal zinc oxide (ZnO) are used. Concentration of 0.1 to 1.0% by weight It is mixed with distilled water to prepare a colloidal oxide mixed solution. If the concentration of the colloidal oxide mixture is out of the above range, the coating becomes too thick or too thin to achieve the desired phosphor efficiency.

When preparing the colloidal oxide mixture is added to the pH adjuster to maintain a pH of 4 ~ 6 It is preferable to prevent collapse of the colloidal mixture. If the colloidal state is disintegrated in advance, there is a problem in that the oxide is all settled down and subsequent coating of the phosphor is difficult. At this time, the pH adjusting agent may be used, such as NaOH and HCl aqueous solution, but is not limited thereto.

Next, by mixing at a ratio of 1 ~ 10g phosphor per 100ml of the colloidal oxide mixture A colloidal oxide-phosphor mixture is prepared. Colloidal Mixing the oxide mixture and the phosphor at the above ratios is advantageous in terms of drying and coating rate control.

Next, the pH was added to the colloidal oxide-phosphor mixture, the pH was adjusted to 6-8, and the first stirring was performed for 0.5 to 1.5 hours. Then, the pH was added to adjust the pH to 10 or more and 0.5 to 1.5. Stir further for time. At this time, the pH adjusting agent may be used, such as NaOH aqueous solution, but is not limited thereto.

It is preferable to carry out stirring for 0.5 to 1.5 hours, respectively, so that the oxide of the colloidal state is coated on the phosphor.

The colloidal oxides are well coated with the phosphor near the pH value at which the zeta potential is zero. Each colloidal oxide has a different pH range for coating due to the difference in zeta potential. do. For example, colloidal silicon oxide (SiO 2 ) and colloidal zinc oxide (ZnO) in the case of colloidal yttrium oxide (Y 2 O 3 ) and colloidal aluminum oxide (Al 2 O 3 ) at pH 6-8 At pH above 10, the surface of the phosphor is well coated.

Therefore, when the pH is gradually increased, specific oxides are first coated, and other oxides are intercalated to form a multi-coated phosphor having an overall rough surface.

Finally, after stirring is complete, the mixture is dried at about 80 to 100 ° C. for 10 to 14 hours to finally obtain a multi-coated phosphor having a rough surface.

Commercially available examples of the colloidal oxide include colloidal silica (SiO 2 ) and LUDOX AM manufactured by Grace Corporation, and examples of colloidal alumina (Al 2 O 3 ) include Nyacol Nano Technologies. For example, the product (trade name: Nyacol® AL20) may be used. For example, colloidal yttria (Y 2 O 3 ) may be used as an example of the product Nyacol Nano Technologies (trade name: Nyacol®Y 2 O 3 ). Examples of zinc oxide (ZnO) this month include, but are not limited to, the product of Nyacol Nano Technologies (trade name: Nyacol® DP5370).

In the fluorescent substance, if a phosphor used for the display and can be used without particular limitation, as an example of the blue light-emitting fluorescent substance representatively BaMgAl 10 O 17 in the matrix a BaMgAl 10 O added Eu 2 + a small amount of activator in 17: Eu 2 + Can be mentioned.

The modified sol-gel method applied in the present invention is subjected to multiple coatings in a single process, the process itself is very simple, efficient and less expensive than the conventional method is economical.

Hereinafter, the present invention will be described in more detail with reference to Examples, but the scope of the present invention is not limited to the range illustrated by the following Examples.

[Example 1]

Colloidal silicon oxide (SiO 2) Grace Co. in US LUDOX AM, colloidal aluminum oxide (Al 2 O 3) as the Nyacol Nano Technologies社product (trade name: Nyacol®AL20) an oxide of the total solution (SiO 2, Al 2 O 3 ) was mixed in distilled water so that the weight ratio of about 0.86% by weight to prepare a mixed solution, at which time 5ml HCl aqueous solution was added as a pH regulator per 100ml of the mixed solution A colloidal oxide mixed solution was prepared while maintaining a pH of 5.

80 ml of Kasei Co., Ltd. Phosphor (brand name: KX-501A) 5g was mixed to prepare a colloidal oxide-phosphor mixture.

10 mL NaOH aqueous solution was added to the colloidal oxide-phosphor mixture as a pH adjusting agent. After the pH was adjusted to 7 and stirred for 1 hour, 10 mL of an aqueous NaOH solution was added to the pH adjuster to adjust the pH to 10 or more and stirred for 1 hour.

Next, the resultant was dried at 90 ° C. for 12 hours to finally obtain a multi-coated phosphor.

The obtained phosphor was photographed by SEM and shown in FIG. 6 (b).

In order to measure visible light transmittance and luminance with respect to the obtained phosphor, a phosphor paste was prepared to form a thick film. The phosphor paste is mixed with a solvent (binder) in a 9: 1 weight ratio at 100 ℃ and stirred until the bubble disappears to prepare a phosphor vehicle (vehicle), the double-coated phosphor obtained in Example 1 It was prepared by mixing 1: 2 weight ratio to the phosphor vehicle.

As the binder, ethyl cellulose (Ethylcelluose (powder)) was used, and as a solvent, butyl carbitol acetate (Dimethyl Glycol Monobutyl Ether Acetate, liquid) and butyl carbitol (Diethylene Glycol Monobutyl Ether) were used. , liquid)) was used in a 8: 1 weight ratio.

Phosphor paste was prepared using the double-coated phosphor obtained in Example 1 to form a thick film, and the visible light transmittance of the phosphor was measured, and also applied to a PDP device to measure the luminance, and the results are shown in Table 1.

Permeability was evaluated by the method of comparing measured from coming out by irradiating the light from the same light sources (Light Source) to the fluorescent material value, specifically, a blue phosphor: For (BaMgAl 10 O 17 Eu 2 + ) thick film (厚幕) The blue light emitted from the fluorescent film was irradiated indirectly by a method of collecting the light emitted from an integrating sphere and measuring it again.

In the case of luminance, a device was fabricated, and the average value was calculated after measuring five times with CS-100A of Minolta.

PDP device using uncoated phosphor PDP device using phosphor according to Example 1 Transmittance (%) 86 (average) 95 (average) Luminance 1000 cd / m 2 (average) 1150cd / m 2 (average value)

Example 2

A phosphor paste was prepared in the same manner using the double-coated phosphor obtained in Example 1 to form a thick film, and the visible light transmittance was measured, and also applied to the LCD backlight to measure the brightness, the results are shown in Table 2. In case of LCD backlight, it is manufactured by using FFL (Surface Light Source Lamp) which has the same structure as PDP. Table 2 shows the measured value when it is manufactured by blue surface light source lamp. The driving conditions were measured at a frequency of 20 kHz and a duty ratio of 20% at 2.5kV RMS .

With uncoated phosphor
Blue LCD backlight Using the phosphor according to Example 2
Blue LCD backlight Transmittance (%) 85 (average) 95 (average) Luminance 1100 cd / m 2 (average) 1250 cd / m 2 (average)

Example 3

The first embodiment of the blue phosphor, instead of Japan Kasei社prepared in the same content in red carried out in the same manner as in Example 1, but applied to ((Y, Gd) BO 3 :: Eu 3 +) phosphor (KX-504A trade name) To obtain a double-coated red phosphor, and the obtained phosphor was photographed by SEM and shown in FIG. 7 (b).

The obtained phosphor was evaluated for application to the LCD backlight in the same manner as in Example 2 and the results are shown in Table 3.

With uncoated phosphor
Red LCD backlight Using the phosphor according to Example 3
Red LCD backlight Transmittance (%) 84 (average) 94 (average) Luminance 2200 cd / m 2 (average) 2450 cd / m 2 (average)

Example 4

Except for applying the blue phosphor of Example 1 to the green (ZnSiO 4 : Mn 2 + ) phosphor (trade name: P1-G1S) manufactured by Kasei Co., Ltd. in the same content as in Example 1, double-coated green Phosphors were obtained, and the obtained phosphors were photographed by SEM and shown in FIG. 8 (b).

The obtained phosphor was evaluated for application to the LCD backlight in the same manner as in Example 2 and the results are shown in Table 4.

With uncoated phosphor
Green LCD backlight Using the phosphor according to Example 4
Green LCD backlight Transmittance (%) 82 (average) 96 (average) Luminance 5300 cd / m 2 (average) 6050 cd / m 2 (average)

Example 5

In order to prepare a white 3-wavelength multi-coated phosphor powder, the green, red, and blue double coated phosphors obtained in Examples 1, 3, and 4 were prepared using 41.3 wt% Red, 27.3 wt% Green, and 31.3 wt% Blue, respectively. Mix in proportions. The mixed double-coated phosphor was fabricated and applied to FFL (Surface Light Source Lamp) in the same manner as in Example 2. In the case of white light transmittance of the three wavelengths it is difficult to measure the transmittance by the above method, only the luminance value was measured and compared and the results are shown in Table 5.

With uncoated phosphor
White LCD backlight Using the phosphor according to Example 5
White LCD backlight Luminance 8500 cd / m 2 (average) 9150cd / m 2 (average value)

Referring to Tables 1 to 5, as a result, the visible light transmittance of the phosphor in both the PDP device and the LCD backlight adopting the coarse multi-coated phosphor obtained by using the two or more oxides of the present invention is improved, and as a result, the luminance is improved. It can be seen that an improved effect can be obtained.

Since the multi-coated phosphor according to the present invention is nano-coated with an oxide, when the existing phosphor is used for a display device, the problem of decrease in luminance and lifespan due to deterioration due to long-term vacuum ultraviolet exposure is improved. In addition, it is possible to increase the luminous efficiency by minimizing the probability that the generated visible light is not emitted due to total reflection on the surface of the phosphor.

In addition, since the oxide multiple coating layer of the present invention is manufactured using a modified sol-gel method, the manufacturing cost can be lowered.

Simple modifications or changes of the present invention can be easily carried out by those skilled in the art, and all such modifications or changes can be seen to be included in the scope of the present invention.

1: phosphor
2: light emission area
3: oxide layer

Claims (9)

A multi-coated phosphor characterized in that two or more oxides selected from the group consisting of silicon oxide, yttrium oxide, aluminum oxide and zinc oxide are surface coated simultaneously. The multi-coated phosphor according to claim 1, wherein silicon oxide and aluminum oxide are surface coated at the same time. Two or more colloidal oxides selected from colloidal silicon oxide (SiO 2 ), colloidal yttrium oxide (Y 2 O 3 ), colloidal aluminum oxide (Al 2 O 3 ), and colloidal zinc oxide (ZnO) are mixed with distilled water. Preparing a colloidal oxide mixed solution;
Preparing a colloidal oxide-phosphor mixture by mixing phosphors with the colloidal oxide mixture; And
Method for producing a multi-coated phosphor, characterized in that it comprises the step of raising the pH step by step with respect to the colloidal oxide-phosphor mixture mixture, followed by drying. The method of claim 3, wherein the pH of the colloidal oxide-phosphor mixture is adjusted to 6 to 8, and then stirred for 0.5 to 1.5 hours, and then the pH is adjusted to 10 or more and stirred for 0.5 to 1.5 hours. Method for producing a multi-coated phosphor. The method of claim 3, wherein the drying is performed at 80 ° C. or higher and 100 ° C. or lower for 10 to 14 hours. The method of claim 3, wherein the colloidal oxide mixture is prepared while maintaining the pH at 4-6. The method of claim 3, 1 to 10g of the phosphor relative to 100ml of the colloidal oxide mixture solution Method for producing a multi-coated phosphor, characterized in that for mixing to prepare a colloidal oxide-phosphor mixture. 4. The colloidal oxide of claim 3, wherein the colloidal oxide is Concentration of 0.1 to 1.0% by weight Method of producing a multi-coated phosphor, characterized in that to prepare a colloidal oxide mixture by mixing in distilled water. The method of claim 3, wherein the phosphor mediator is prepared by mixing colloidal silicon oxide (SiO 2 ) and colloidal aluminum oxide (Al 2 O 3 ) in a solvent at the same time.
KR1020100032004A 2010-04-07 2010-04-07 Multi-coated Phosphors and Manufacturing Method thereof KR101139542B1 (en)

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Publication number Priority date Publication date Assignee Title
KR20140056406A (en) * 2012-10-23 2014-05-12 단국대학교 천안캠퍼스 산학협력단 Method of surface coating for phosphor

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KR100315113B1 (en) 1999-06-26 2001-11-24 김순택 Method for treating surface of phosphors for PDP and surface-treated phosphors for PDP manufactured using the same

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20140056406A (en) * 2012-10-23 2014-05-12 단국대학교 천안캠퍼스 산학협력단 Method of surface coating for phosphor

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