JP5016187B2 - Nitride phosphor, method for producing nitride phosphor, light source and LED using the nitride phosphor - Google Patents

Nitride phosphor, method for producing nitride phosphor, light source and LED using the nitride phosphor Download PDF

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JP5016187B2
JP5016187B2 JP2004207271A JP2004207271A JP5016187B2 JP 5016187 B2 JP5016187 B2 JP 5016187B2 JP 2004207271 A JP2004207271 A JP 2004207271A JP 2004207271 A JP2004207271 A JP 2004207271A JP 5016187 B2 JP5016187 B2 JP 5016187B2
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phosphor
nitride phosphor
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nitride
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堅之 坂根
修次 山下
昌大 後藤
晶 永富
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Dowaエレクトロニクス株式会社
日亜化学工業株式会社
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    • 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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    • Y02BCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
    • Y02B20/00Energy efficient lighting technologies
    • Y02B20/16Gas discharge lamps, e.g. fluorescent lamps, high intensity discharge lamps [HID] or molecular radiators
    • Y02B20/18Low pressure and fluorescent lamps
    • Y02B20/181Fluorescent powders

Description

  The present invention relates to a phosphor used in display devices such as CRT, PDP, FED, EL, etc., and illumination devices such as fluorescent display tubes, fluorescent lamps, etc., and is excited by ultraviolet to green light, The present invention relates to a nitride phosphor for emitting visible light or white light, a method for producing the nitride phosphor, and a light source and an LED using the nitride phosphor.

  Currently, discharge fluorescent lamps and incandescent lamps used as lighting devices have various problems such as containing harmful substances such as mercury and short life. However, in recent years, LEDs that emit blue and ultraviolet light have been developed one after another, and the combination of ultraviolet to green light generated from the LED and a phosphor having an excitation band in the ultraviolet to green wavelength range has allowed white light to be emitted. Research and development to obtain a next-generation lighting device that emits light is actively conducted. This lighting device has a small amount of heat generation, and is composed of a semiconductor element (LED) and a phosphor, so it has a long life without fear of breaking like an incandescent light bulb. There are many advantages such as unnecessary, and it is an ideal lighting device.

  Here, in order to obtain white light by combining the above-described LED and phosphor, generally two methods are conceivable. One is a combination of an LED that emits blue light and a phosphor that receives the blue light emission and is excited to emit yellow light, and obtains white light emission by a combination of blue light emission and yellow light emission that are complementary to each other. .

  The other one is an LED that emits near ultraviolet or ultraviolet light, a phosphor that emits red (R) when excited by the near ultraviolet or ultraviolet light emission, a phosphor that emits green (G), and blue (B ) And a phosphor emitting another color, and white light emission is obtained by mixing light such as RGB. This method of obtaining white light emission by light such as RGB can obtain any light emission color other than white light depending on the combination or mixing ratio of phosphors that emit light such as RGB. Wide application range.

As a phosphor used for this application, if it is a red phosphor, for example, Y 2 O 2 S: Eu, La 2 O 2 S: Eu, 3.5MgO · 0.5MgF 2 · GeO 2 : Mn, If there is (La, Mn, Sm) 2 O 2 S · Ga 2 O 3 and it is a green phosphor, for example, there are ZnS: Cu, Al, SrAl 2 O 4 : Eu, BAM: Eu, Mn, yellow For example, YAG: Ce may be used as the phosphor, and BAM: Eu, Sr 5 (PO 4 ) 3 Cl: Eu, ZnS: Ag, (Sr, Ca, Ba, Mg) may be used as the blue phosphor. ) 10 (PO 4 ) 6 Cl: Eu. And, by combining these phosphors that emit RGB and the like with light emitting parts (light emitting elements) such as LEDs that emit near ultraviolet or ultraviolet light, light sources such as LEDs that emit white light or a desired single color, It is possible to obtain an illumination device including the light source.

  However, in the illumination that obtains white color by combining the blue LED and the yellow phosphor (YAG: Ce), the light emission on the long wavelength side in the visible light region is insufficient. As a result, it is not possible to obtain white light emission that is slightly reddish like a light bulb.

  In addition, in illumination that obtains white color by combining near-ultraviolet / ultraviolet LEDs and phosphors that emit RGB, etc., the red phosphor of the three color phosphors has lower excitation efficiency on the longer wavelength side than the other phosphors. Since the luminous efficiency is reduced, the mixing ratio of the red phosphors must be increased, and the phosphors for improving the luminance are insufficient, and a high luminance white color cannot be obtained.

  Therefore, recently, an oxynitride glass phosphor that has good excitation on the long wavelength side and a broad emission half-width emission peak (see, for example, Patent Document 1), and a phosphor based on sialon (for example, a patent) References 2, 3, and 4) and phosphors containing nitrogen such as silicon nitride (for example, see Patent Documents 5 and 6) have been proposed. Since these phosphors containing nitrogen have a higher covalent bond ratio than oxide-based phosphors and the like, they have a good excitation band even in light with a wavelength of 400 nm or more and emit white light. It is attracting attention as a fluorescent material for use.

Japanese Patent Laid-Open No. 2001-214162 JP2003-336059 Japanese Patent Laid-Open No. 2003-124527 Japanese Patent Application No. 2004-067837 Special table 2003-515655 JP 2003-277746 A

Light sources such as LEDs that emit visible light and white light by combining the light emitting element that emits ultraviolet to green light and a phosphor having an excitation band in the ultraviolet to green wavelength range generated from the light emitting element. However, in order to improve the light emission characteristics of visible light or white light, improvement in light emission efficiency and stability of the light emitting element and the phosphor are required. However, in the phosphor according to the conventional technique, the light emission efficiency is not always stable for each production batch, and the light emission efficiency sometimes varies. Here, the present inventors have investigated the cause of the variation, and thought that the luminous efficiency of the phosphor could be further improved if the countermeasure can be taken.
Therefore, the present inventors prepared various phosphor samples and pursued the cause of the variation, and came up with the cause of carbon and / or oxygen contained as impurities in the phosphor.
Here, the present inventors have further studied the origin of carbon and / or oxygen contained as the impurities. As a result, the element is not only derived from the originally anticipated atmosphere, but also diffuses into the nitride phosphor from the firing vessel and becomes an impurity in the sintering process when producing the nitride phosphor. I came up with that.

An object of the present invention has been made in consideration of the above-described circumstances, and a nitride phosphor having improved luminous efficiency by suppressing carbon and / or oxygen contained as impurities in the nitride phosphor. Is to provide.
Another object of the present invention is to provide a method for producing a nitride phosphor capable of improving the luminous efficiency of the phosphor by suppressing carbon and / or oxygen contained as the impurity in the nitride phosphor. There is to do.
Still another object of the present invention is to provide a light source and an LED using a nitride phosphor with improved luminous efficiency.

The first structure is represented by the general formula MAlSiN 3 : Eu, and M is one or more elements selected from the group consisting of Mg, Ca, Sr, Ba, and Zn, where Al has a valence of II, Al is aluminum, Si is silicon, N is nitrogen, Eu is an activator, is in powder form, has a carbon content of less than 0.08% by weight, and an oxygen content of less than 3.0% by weight. This is a nitride phosphor.

The second configuration, the average particle size of the powder of the nitride phosphor is 20μm or less, a nitride phosphor according to the first configuration, characterized in that at 0.1μm or more.

A third configuration is a method for manufacturing a nitride phosphor according to any one of the first and second configurations, in which a raw material for the nitride phosphor is filled in a firing container made of a boron nitride material. A nitride phosphor manufacturing method is characterized in that a nitride phosphor is manufactured by firing in an active atmosphere.

A fourth configuration includes the nitride phosphor according to any one of the first and second configurations and a light emitting unit that emits light of a predetermined wavelength, and a part of the light of the predetermined wavelength is an excitation source. And the nitride phosphor emits light at a wavelength different from the predetermined wavelength.

A fifth configuration is the light source according to the fourth configuration, wherein the predetermined wavelength is a wavelength of 250 to 550 nm.

A sixth configuration includes the nitride phosphor according to any one of the first and second configurations, and a light emitting unit that emits light of a predetermined wavelength, and a part of the light of the predetermined wavelength is an excitation source. And the nitride phosphor emits light at a wavelength different from the predetermined wavelength.

A seventh configuration is the LED according to the sixth configuration, wherein the predetermined wavelength is a wavelength of 250 to 550 nm.

The nitride phosphor according to the first or second configuration is a nitride phosphor having a carbon content of less than 0.08% by weight and a nitride phosphor having an oxygen content of less than 3.0% by weight. Therefore, since the impurity contents of carbon and oxygen that do not contribute to light emission are small, it is possible to suppress a decrease in the light emission intensity of the nitride phosphor, and to improve the light emission efficiency of the nitride phosphor.

Further, the general formula is represented by M-Al-Si-N: Z, where M is one or more elements having a valence of II, Al is aluminum, Si is silicon, N is nitrogen, and Z is an activator. Since it has an excitation band in a wide range of light from ultraviolet to green (wavelength range 250 to 550 nm) from a light emitting part that emits ultraviolet to green light, the luminous efficiency can be further improved. .

Since the nitride phosphor according to the first or second configuration is in a powder form, it is possible to easily apply or fill the nitride phosphor. Furthermore, since the average particle size of the nitride phosphor powder is 20 μm or less and 0.1 μm or more, the luminous efficiency can be improved.

According to the method for producing a nitride phosphor according to the third configuration, the nitride phosphor is filled in a firing vessel made of boron nitride and fired in an inert atmosphere to produce the nitride phosphor. As a result, a nitride phosphor having a low carbon and oxygen impurity content can be produced. Thus, since the nitride phosphor with few impurities that do not contribute to light emission can be manufactured, a decrease in emission intensity can be suppressed, and the light emission efficiency of the nitride phosphor can be improved.

In the light source according to the fourth or fifth configuration, the nitride phosphor emits light having an excitation band in light of a predetermined wide wavelength range (250 to 550 nm) emitted from the light emitting unit. By combining the phosphor and the light emitting portion, a light source with high luminous efficiency that emits visible light or white light can be obtained.

In the LED according to the sixth or seventh configuration, the nitride phosphor emits light having an excitation band in light of a predetermined wide wavelength range (250 to 550 nm) emitted from the light emitting unit. By combining the phosphor and the light emitting portion, an LED having high luminous efficiency that emits visible light or white light can be obtained.

The best mode for carrying out the present invention will be described below with reference to the drawings.
The nitride phosphor according to the present invention is a nitride phosphor represented by the general formula M-Al-Si-N: Z, wherein M is one or more elements having a valence of II, Al A nitride phosphor, which is aluminum, Si is silicon, N is nitrogen, and Z is an activator, will be described as an example. In the nitride phosphor, the carbon content as an impurity is less than 0.08% by weight and the oxygen content as an impurity is less than 3.0% by weight. Both the impurity carbon content of less than 0.08% by weight and the impurity oxygen content of less than 3.0% by weight are preferably satisfied, but either one may be satisfied.

  Nitride phosphors with an impurity carbon content of less than 0.08% by weight and nitride phosphors with an impurity oxygen content of less than 3.0% by weight contain carbon and oxygen impurities that do not contribute to light emission in any case. Since the amount is small, when the emission intensity is expressed in relative intensity, a decrease in the emission intensity of about 25 to 30% can be suppressed, and thus the emission efficiency can be improved.

  The nitride phosphor is represented by a general formula M-Al-Si-N: Z, where M is one or more elements having a valence of II, Al is aluminum, Si is silicon, N is nitrogen, Since Z is an element that acts as an activator, it has an excitation band in a wide range of light from ultraviolet to green (wavelength range 250 to 550 nm) from the light emitting part that emits ultraviolet to green light, so that the luminous efficiency is improved. Further improvement can be achieved.

  More specifically, when the nitride phosphor is represented by a composition formula MmAlaSibNn: Z, a nitride phosphor having a relationship of n = 2 / 3m + a + 4 / 3b is preferable. When n, m, a, and b satisfy the relationship, the host structure of the nitride phosphor described above has a chemically stable structure, and an impurity phase that does not contribute to light emission is less likely to occur in the host structure. Because. Furthermore, stability is improved when m = a = b = 1. However, a slight compositional deviation from the composition formula of the matrix structure is allowed.

  M is preferably at least one element selected from Be, Mg, Ca, Sr, Ba, Zn, Cd, and Hg, and further selected from Mg, Ca, Sr, Ba, and Zn. Preferably, the element is at least one element.

  Z is preferably at least one element selected from rare earth elements or transition metal elements, and is particularly preferably at least one element selected from Eu, Mn, Sm, and Ce. . Among these, when Eu is used, the nitride phosphor exhibits strong light emission from orange to red, and thus has high luminous efficiency, and is more preferable as an activator of the nitride phosphor for a light source (LED) that emits white light.

  The nitride phosphor according to the present invention (hereinafter sometimes simply referred to as “phosphor”) is a powdery material in consideration of ease of application or filling. The average particle diameter of the phosphor powder is preferably 20 μm or less. This is because light emission is considered to occur mainly on the particle surface in the phosphor powder, and if the average particle size is 20 μm or less, a surface area per unit weight of the powder can be secured and a decrease in luminance can be avoided. . Furthermore, the density of the powder can be increased even when the powder is formed into a paste and applied to a light-emitting element or the like, and a decrease in luminance can be avoided also from this viewpoint. Further, according to the study by the present inventors, although the detailed reason is unknown, it has been found that the average particle size is preferably larger than 0.1 μm from the viewpoint of the luminous efficiency of the phosphor powder. From the above, the average particle diameter of the phosphor powder according to the present invention is preferably 0.1 μm or more and 20 μm or less.

In the method for producing a phosphor according to the present invention, a phosphor material is filled in a firing container made of boron nitride and fired in an inert atmosphere to produce the phosphor. This phosphor manufacturing method will be described by taking, as an example, the manufacture of CaAlSiN 3 : Eu (provided that Eu / (Ca + Eu) molar ratio = 0.015) as the phosphor.

First, Ca 3 N 2 (2N), AlN (3N), and Si 3 N 4 (3N) are prepared as raw materials of Ca, Al, and Si, respectively. Eu 2 O 3 (3N) is prepared as the Eu raw material.

  These raw materials are weighed and mixed so that the molar ratio of each element is Ca: Al: Si: Eu = 0.985: 1: 1: 0.015. ((Ca + Eu): Al: Si: = 1: 1: 1) The mixing may be performed by a normal mixing method using a mortar or the like, but operated in a glove box under an inert atmosphere such as nitrogen. It is convenient to do.

  The reason for operating the mixing in a glove box under an inert atmosphere is that if this operation is performed in the atmosphere, the ratio of the oxygen concentration contained in the matrix constituent elements collapses due to oxidation and decomposition of the above raw materials, resulting in a decrease in light emission characteristics. This is because there is a possibility of deviating from the target composition of the phosphor. Furthermore, since the nitride of each raw material element is easily affected by moisture, it is preferable to use an inert gas from which moisture has been sufficiently removed. When a nitride raw material is used as each raw material element, dry mixing is preferable as a mixing method in order to avoid decomposition of the raw material, and a normal dry mixing method using a ball mill, a mortar, or the like may be used.

  The mixed raw material is filled in a boron nitride crucible as a firing container and is heated to 1500 ° C. in an inert atmosphere such as nitrogen at 15 ° C./min. The temperature is increased at a temperature increase rate of 1,5 ° C. and held at 1500 ° C. for 3 hours for firing. The firing temperature may be 1000 ° C. or higher, preferably 1400 ° C. or higher. The holding time can be shortened because the firing proceeds more rapidly as the firing temperature is higher. Even if the firing temperature is low, the desired light emission characteristics can be obtained by holding for a long time. As the firing time is longer, the particle growth proceeds and the particle shape becomes larger. Therefore, an arbitrary firing time may be set according to the target particle size.

  Here, the present inventors, as a firing container (for example, a crucible) for firing a phosphor material, are fired from a carbon firing container when fired using, for example, a carbon firing container. It has been conceived that carbon may be mixed as an impurity in the phosphor and the emission intensity of the phosphor may be reduced. According to the study by the present inventors, it has been found that when the amount of carbon contained in the phosphor becomes 0.08% by weight or more, the emission intensity of the phosphor starts to decrease. In addition, when the present inventors baked using an alumina firing container, oxygen diffuses as an impurity in the phosphor fired from the alumina firing container, and the emission intensity of the phosphor decreases. I thought that there was a risk of doing. According to the study by the present inventors, it has been found that when the amount of oxygen contained in the phosphor becomes 3.0% by weight or more, the emission intensity of the phosphor starts to decrease.

  The inventors of the present invention can produce a phosphor with a low content of impurity carbon and low content of impurity oxygen that does not contribute to light emission by firing the phosphor using a firing container made of boron nitride. Thus, it has been conceived that a decrease in emission intensity can be suppressed and the luminous efficiency of the luminous body can be improved.

Therefore, a boron nitride firing container is used as the firing container, and after firing is completed, the temperature is cooled from 1500 ° C. to 200 ° C. in 1 hour, and further cooled to room temperature, and then predetermined using pulverizing means such as a mortar and ball mill. (preferably 20Myuemu~1myuemu) was ground to an average particle size of the composition formula Ca 0.985 SiAlN 3: preparing a phosphor of Eu 0.015.

  Even when the set value of Eu / (Ca + Eu) molar ratio fluctuates, a phosphor having a predetermined composition can be manufactured by a similar manufacturing method by adjusting the blending amount of each raw material to a predetermined composition formula. it can. All of the obtained phosphors had a carbon content of less than 0.08% by weight and an oxygen content of less than 3.0% by weight.

The phosphor according to the present invention in a powder form is combined with a light emitting part (particularly, a light emitting part that emits light in any of the light emission wavelength ranges of 250 to 550 nm) by a known method, so that the light emitting part emits light. Since light having an excitation band is emitted in light in a wide wavelength range, a light source with high emission efficiency that emits visible light or white light can be obtained. In particular, an LED that emits visible light or white light can be obtained by combining an LED that emits light in the emission wavelength range of 250 to 550 nm as a light emitting unit with a known method.
Therefore, this light source (LED) can be used as various light sources for display devices such as CRT and PDP and illumination devices such as fluorescent lamps.

Hereinafter, based on an Example, this invention is demonstrated more concretely.
Example 1
Commercially available Ca 3 N 2 (2N), AlN (3N), Si 3 N 4 (3N), and Eu 2 O 3 (3N) were prepared, and the molar ratio of each element was Ca: Al: Si: Eu = 0. Each raw material was weighed so that it would become 985: 1: 1: 0.015, and it mixed using the mortar in the glove box of nitrogen atmosphere. The mixed raw material is filled in a crucible made of boron nitride, and 15 ° C./min. Was heated at 1500 ° C. for 3 hours and fired, and then cooled from 1500 ° C. to 200 ° C. for 1 hour to obtain a phosphor of composition formula Ca 0.985 SiAlN 3 : Eu 0.015. It was.
When the obtained phosphor powder was irradiated with monochromatic light of 460 nm, red light emission having an emission peak at 656 nm was shown as shown in FIG. The impurity carbon concentration and impurity oxygen concentration obtained by chemical analysis were 0.043 wt% and 2.09 wt%, respectively.

(Comparative Example 1)
A phosphor was produced under the same conditions as in Example 1 except that the container used for firing was changed from a boron nitride crucible to a carbon crucible. When the obtained phosphor powder was irradiated with monochromatic light of 460 nm, it showed red light emission having an emission peak at 650 nm. FIG. 1 shows the relative emission intensity of the phosphor produced in this comparative example, and the impurity carbon concentration and impurity oxygen concentration obtained by chemical analysis.
As shown in FIGS. 1 and 2, the phosphor produced using a carbon crucible for the firing container has a light emission intensity of about 1% compared to the phosphor of Example 1 produced using a boron nitride crucible. The result decreased by 26%. Since the phosphor produced using a carbon crucible has an impurity carbon content increased to 0.080% by weight, it is considered that the impurity carbon reduces the emission intensity.

(Comparative Example 2)
A phosphor was produced under the same conditions as in Example 1 except that the container used for firing was changed from a boron nitride crucible to an alumina crucible. When the obtained phosphor powder was irradiated with monochromatic light of 460 nm, it showed red light emission having an emission peak at 652 nm. FIG. 1 shows the relative emission intensity of the phosphor produced in this comparative example, and the impurity carbon concentration and impurity oxygen concentration obtained by chemical analysis.
As shown in FIGS. 1 and 2, the phosphor produced using the alumina crucible for the firing container has a light emission intensity of about 1% compared to the phosphor of Example 1 produced using the boron nitride crucible. The result decreased by 20%. Since the phosphor produced using the crucible made of alumina has an impurity oxygen amount increased to 3.02% by weight, the impurity oxygen is considered to decrease the emission intensity.

  As mentioned above, although this invention was demonstrated based on the said embodiment, this invention is not limited to this.

6 is a chart showing the material of the firing container (crucible) used when manufacturing the phosphor according to the present invention, and the characteristics and impurity concentration of the manufactured phosphor. And the material of the firing vessel for preparing by firing a CaAlSiN 3 as the phosphor according to the present invention (crucible) is a graph showing the relationship between the emission intensity of the phosphor.

Claims (7)

  1. One or more elements selected from the group consisting of Mg, Ca, Sr, Ba, and Zn, in which M is a valence of II, M is represented by the general formula MAlSiN 3 : Eu, Al is aluminum, Si is silicon, N is Nitrogen, Eu is an activator element, is in powder form, has a carbon content of less than 0.08% by weight, and an oxygen content of less than 3.0% by weight. Phosphor.
  2. 2. The nitride phosphor according to claim 1 , wherein an average particle size of the powdered nitride phosphor is 20 μm or less and 0.1 μm or more.
  3. A method for producing a nitride phosphor according to claim 1 or 2 ,
    A nitride phosphor is produced by filling a nitride phosphor material into a firing vessel made of boron nitride and firing in an inert atmosphere to produce a nitride phosphor.
  4. 3. The nitride phosphor according to claim 1 , and a light emitting unit that emits light of a predetermined wavelength, wherein a part of the light of the predetermined wavelength is used as an excitation source, and the nitride phosphor is A light source that emits light at a wavelength different from the predetermined wavelength.
  5. The light source according to claim 4 , wherein the predetermined wavelength is a wavelength of 250 to 550 nm.
  6. 3. The nitride phosphor according to claim 1 , and a light emitting unit that emits light of a predetermined wavelength, wherein a part of the light of the predetermined wavelength is used as an excitation source, and the nitride phosphor is An LED that emits light at a wavelength different from the predetermined wavelength.
  7. The LED according to claim 6 , wherein the predetermined wavelength is a wavelength of 250 to 550 nm.
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JP2004207271A JP5016187B2 (en) 2004-07-14 2004-07-14 Nitride phosphor, method for producing nitride phosphor, light source and LED using the nitride phosphor
TW94105848A TWI262609B (en) 2004-02-27 2005-02-25 Phosphor and manufacturing method thereof, and light source, LED using said phosphor
KR20050016250A KR100702757B1 (en) 2004-02-27 2005-02-26 Phosphor and manufacturing method thereof, and light source, led using said phosphor
CN 200510052522 CN100340631C (en) 2004-02-27 2005-02-28 Phosphor and manufacturing method thereof, and led light source using said phosphor
DE200560014296 DE602005014296D1 (en) 2004-02-27 2005-02-28 Phosphor and its preparation and LED light source using this phosphor
EP05004375A EP1568753B1 (en) 2004-02-27 2005-02-28 Phosphor and manufacturing method thereof, and LED light source using said phosphor

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