WO2008062781A1 - Substance fluorescente et son procédé de fabrication, et dispositif électroluminescent - Google Patents
Substance fluorescente et son procédé de fabrication, et dispositif électroluminescent Download PDFInfo
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- WO2008062781A1 WO2008062781A1 PCT/JP2007/072443 JP2007072443W WO2008062781A1 WO 2008062781 A1 WO2008062781 A1 WO 2008062781A1 JP 2007072443 W JP2007072443 W JP 2007072443W WO 2008062781 A1 WO2008062781 A1 WO 2008062781A1
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- Prior art keywords
- phosphor
- light
- sialon
- light emitting
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- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
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- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/597—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon oxynitride, e.g. SIALONS
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
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- H01L33/50—Wavelength conversion elements
- H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
- H01L33/502—Wavelength conversion materials
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Definitions
- the present invention is useful for various light emitting devices such as white light emitting diodes (white LEDs) using blue light emitting diodes (blue LEDs) or ultraviolet light emitting diodes (ultraviolet LEDs).
- white LEDs white LEDs
- blue LEDs blue light emitting diodes
- ultraviolet light emitting diodes ultraviolet light emitting diodes
- Patent Document 1 discloses that a semiconductor light emitting element that emits blue to violet short-wavelength visible light and a phosphor are combined to emit light from the semiconductor light emitting element and light that has been wavelength-converted by the phosphor.
- a white LED that obtains white light by mixing the two colors is disclosed.
- phosphors are widely known in which silicates, phosphates, aluminates, and sulfides are used for the base material V, and transition metals or rare earth metals are used for the emission center! / RU
- sialon which is a solid solution of silicon nitride
- sialon has two types of crystal systems, ⁇ -type and / 3-type.
- ⁇ -sialons activated with specific rare earth elements are known to have useful fluorescence characteristics, and their application to white LEDs and the like is being studied (Patent Documents 2 to 4, Non-Patent Document 1). reference).
- / 3 type sialon is a solid solution of / 3 type silicon nitride, and Si position of / 3 type silicon nitride crystal Al is substituted and O is substituted at the N position. Since there are two formula atoms in the unit cell (unit cell), Si Al ON is used as a general formula.
- the composition z is 0 to 4.2.
- the solid solution range is very wide, and the molar ratio of (Si, A1) / (N, O) must be maintained at 3/4.
- the crystal structure of the / 3 type nitride nitride has P6 or P6 / m symmetry,
- ⁇ -sialon can be obtained by heating by adding silicon oxide and aluminum nitride, or aluminum oxide and aluminum nitride in addition to silicon nitride.
- Eu 2+ When Eu 2+ is included in the crystal structure of ⁇ -type sialon, it is excited by ultraviolet to blue light and becomes a phosphor that emits green light of 520 to 550 nm. It can be used as an ingredient and is known as Eu-activated / type 3 sialon.
- This Eu-activated / 3-type sialon has a very sharp emission spectrum among the phosphors activated by Eu 2+ , and is particularly a liquid crystal display panel that requires blue, green, and red narrow-band emission. This phosphor is suitable for the green light emitting component of the backlight light source.
- Patent Document 1 Japanese Patent No. 2927279
- Patent Document 2 Japanese Patent No. 3668770
- Patent Document 3 Japanese Patent No. 3726131
- Patent Document 4 Japanese Patent Laid-Open No. 2003-124527
- Patent Document 5 Japanese Unexamined Patent Application Publication No. 2005-255895
- Non-Patent Document lliU J. W. J. van Krebei, On new rare— earth doped M — Si— Al— O— N materials, TU Eindhoven, The Netherlands, ppl4 5-161 (1998)
- a conventional phosphor mainly composed of Eu-activated / 3-type sialon has a low luminous efficiency and is difficult to be put into practical use.
- the present invention has an object to provide a phosphor with Eu activation (type sialon as a main component) capable of realizing high luminous efficiency!
- the phosphor having such a configuration is excellent as a green phosphor because it is excited in a wide wavelength range from ultraviolet to visible light and emits green light with a high efficiency within a range of 520 nm to 550 nm as a main wavelength. ing. Therefore, it can be suitably used for various light emitting elements, particularly white LEDs using UV LEDs or blue LEDs as a light source, alone or in combination with other phosphors.
- a light-emitting device comprising the above-described phosphor and a light-emitting light source.
- the light-emitting device having such a configuration uses the phosphor having a / 3 type sialon as a main component as described above, and therefore is thermally and chemically stable possessed by the / 3 type sialon. Reflecting this feature, it has a feature that it has a small decrease in brightness even when used at high temperatures and has a long life.
- the first step of generating Eu-type / 3-type sialon, and heat treatment in a nitrogen atmosphere at a temperature range of 1450 ° C to 1650 ° C for 1 hour or longer there is provided a phosphor manufacturing method including a second step of further reducing the crystal defect density.
- the first step of producing Eu-containing ⁇ -sialon heat treatment in a temperature range of 1200 ° C to 1550 ° C in vacuum, and further acid treatment
- a method for producing a phosphor including a second step of reducing the crystal defect density.
- the Eu-activated / 3-type sialon obtained by a conventionally known production method is simply subjected to a simple heat treatment or acid treatment, and the light emission as described above.
- a phosphor with excellent characteristics can be produced with good reproducibility.
- the phosphor of the present invention contains, as a main component, Eu-activated 0 type sialon capable of realizing high luminous efficiency. Phosphor.
- the method for producing a phosphor of the present invention can produce a phosphor excellent in light emission characteristics as described above with good reproducibility. Further, since the light emitting device of the present invention uses the phosphor that can realize the high light emission efficiency as described above, it is possible to realize high luminance of the light emitting device.
- FIG. 1 is a graph showing an excitation spectrum when the fluorescent intensity of the phosphor powder in Comparative Example 1 and Example 2 is measured at 535 nm and an emission spectrum by external excitation light having a wavelength of 455 nm.
- the phosphor based on the conventional Eu-activated / 3-type sialon has a low luminous efficiency, and a light emitting device such as a white LED using the phosphor cannot obtain sufficient luminance. Difficult to use in practical use.
- the phosphor according to the present embodiment is capable of realizing high luminance of a light emitting device such as a white LED using blue to ultraviolet light emitted from a blue LED or an ultraviolet LED as a light source. It was developed for the purpose of providing a phosphor comprising type 3 sialon.
- the main component of the phosphor of the present embodiment has a general formula: Si AI ON (where z is 0 to 4 ⁇
- the / 3 type sialon shown in 2) is contained in the host crystal and Eu 2+ is contained as the emission center. Since fluorescence is caused by electronic transition of ions that are the emission center, it is important to increase the light emission efficiency to minimize the light absorption of the host crystal itself.
- the present inventor For the purpose of investigating the influence of the host crystal itself in Eu-activated / 3-type sialon, the present inventor compared the light absorption characteristics of Eu-type / 3-type sialon with Eu-activated ⁇ -type. In Sialon, about 10 to 30% of incident light was absorbed over a wide wavelength range from ultraviolet to visible light, and it was found that this was the cause of a significant decrease in luminous efficiency.
- ESR electron spin resonance
- the present inventor examined Eu-activated ⁇ -type sialon! /, Using the ESR method, and the unpaired electrons present due to crystal defects are fluorescence based on excitation light and Eu 2+. It has been found that the luminous efficiency is reduced when light emission is absorbed and the force is not accompanied by light emission.
- the phosphor of this embodiment is a ⁇ -sialon represented by the general formula: Si AI ON.
- the main component is a crystal containing Eu 2+ as a luminescent center.
- Eu 2+ absorbs and emits light due to electron transition between 4f and 5d orbitals.
- the emission color depends on the state of the crystal field around Eu 2+ , and when / 3 type sialon is used as the host crystal, it emits green light with a main wavelength of 520 to 55 Onm.
- this phosphor it is important that the 4f electrons at the emission center are efficiently excited and emit light without changing to heat.Other than that, a region unrelated to light emission, for example, the host crystal itself emits light. In order to increase the luminous efficiency of the phosphor, it is important that the light absorption without accompanying light is minimized.
- the spin density is a value per unit mass obtained by dividing the number of spins measured by ESR by the sample mass used for the measurement.
- E when u 2+ enters the / 3-type sialon crystal, the defect density increases and the amount of unpaired electrons that cause a decrease in luminous efficiency tends to increase.
- the spin density exceeds 2.0 ⁇ 10 17 atoms / g, the light emission efficiency is remarkably lowered, which is not practically preferable.
- the lattice constant of the / 3 type sialon is mainly governed by the number of substitution of Si-N bonds to Al-O bonds, that is, the z value.
- the lattice constant a force of the 0-type sialon is in the range of 0.7608 nm or more and 0.7620 nm or less, and the lattice constant c force of 0.2908 nm or more and 0.2920 ⁇ m or less.
- the larger the crystal lattice size of ⁇ -type sialon the more Eu is contained. Soon, especially when the lattice constants a and c are within the above-mentioned range, the amount of Eu necessary for obtaining sufficient brightness should be contained. Preferred because it will be easier!
- the Eu content is preferably in the range of 0.1 mass% to 3 mass%. According to the study by the present inventors, if the Eu content is within the above range, the light emission luminance can be sufficiently obtained.
- the phosphor contains a / 3 type sialon crystal phase with a high purity and as much as possible, and preferably comprises a single phase of the / 3 type sialon crystal phase.
- the properties will not deteriorate! /, If included, it may be included! / ,.
- the free silicon has a very adverse effect, and ⁇ -sialon and the nitride nitride used as its raw material are thermodynamically unstable at high temperatures and decomposed. It is necessary to keep in mind that it is easy to produce silicon. Therefore, during production, decomposition is usually suppressed by increasing the nitrogen partial pressure in the production atmosphere.
- the diffraction line intensity of the (111) plane of silicon is 1% of the diffraction line intensity of the (101) plane of 0-type sialon. The following is preferable.
- the phosphor of the present embodiment has a particle size distribution measured by a laser diffraction scattering method, and the 50% diameter (D50) in the integrated volume fraction is 6 111 or more, and the 10% diameter (D10 ) Force m or more is preferred. Particles of several meters or less are close to the wavelength of visible light due to the effects of crystal defects, etc., and the phosphor itself has a low emission intensity. This is because when an LED is assembled using a phosphor, it is possible to suppress strong light scattering within the layer containing the phosphor, and the light emission efficiency (light extraction efficiency) of the LED is improved.
- the phosphor of the present embodiment preferably has a D50 force of 0 Hm or less! /. Adjusting D50 to 3 O ⁇ m or less is preferable because it facilitates uniform mixing into the resin that seals the LED and reduces the causes of LED chromaticity variation and uneven color on the irradiated surface.
- ⁇ -sialon can be obtained by heating and reacting a mixed powder composed of silicon nitride, aluminum nitride, aluminum oxide, or silicon oxide in a high-temperature nitrogen atmosphere.
- a mixed powder composed of silicon nitride, aluminum nitride, aluminum oxide, or silicon oxide in a high-temperature nitrogen atmosphere.
- some of the components form a liquid phase, and the substance moves through it to form a ⁇ sialon solid solution.
- the synthesized type 0 sialon forms secondary particles with a complex shape in which a plurality of primary particles (single crystal particles) are sintered. Therefore, pulverization and classification are required to bring the phosphor into the above particle size range.
- the specific surface area of the phosphor powder is preferably 0.5 m 2 / g or less. If the particle size is the same as compared to particles formed by sintering a large number of small primary particles, particles composed of single crystal particles or particles formed from a small number of relatively large primary particles emit light. High efficiency! In addition, the smoother the phosphor particle surface is, the more light scattering on the particle surface is suppressed and the efficiency of capturing excitation light into the particles is increased. When assembling an LED, the interface between the phosphor particles and the sealing resin This is because of the high adhesion. The primary particle size and the particle surface smoothness have a large correlation with the specific surface area. From such a viewpoint, the specific surface area is preferably in the above range.
- the first step is a step of generating a / 3-type sialon containing Eu.
- Conventionally known production methods can be applied to this, and specific examples include the following method. That is, various raw materials are obtained so that a mixed composition containing Si, Al, N, 0, Eu, which are constituent elements of ⁇ -sialon containing Eu, is contained as a main component, and other components contain inevitable impurities. And the resulting mixed composition is heated in a nitrogen atmosphere to contain Eu (this is a method of synthesizing sialon.
- the heating temperature described above varies depending on the desired composition of Eu-containing type 0 sialon, and thus cannot be generally specified, but is generally in the temperature range of 1820 ° C or higher and 2200 ° C or lower. A stable green phosphor can be obtained. If the heating temperature is 1820 ° C or higher, Eu can enter the ⁇ -type sialon crystal, and a phosphor having sufficient luminance can be obtained. In addition, if the heating temperature is 2200 ° C or less, it is not necessary to apply a very high nitrogen pressure to suppress the decomposition of the / 3-type sialon, so there is no need for special equipment. Is preferable.
- a raw material a known material can be used.
- 2 2 3 can use Eu compounds selected from Eu metals, oxides, carbonates, nitrides or oxynitrides. Using these ingredients, they are blended so that a predetermined / 3 type sialon composition is obtained after the reaction.
- a dry mixing method a method of removing the solvent after wet mixing in an inert solvent that does not substantially react with each component of the raw material, and the like can be employed.
- a V-type mixer a rocking mixer, a ball mill, a vibrating minole or the like is preferably used.
- the surface in contact with the raw material is filled in a container such as a crucible made of boron nitride, and heated in a nitrogen atmosphere. Promote solid solution reaction to obtain / 3 type sialon.
- the filling of the raw material mixed powder into the container is preferably a force S that is as bulky as possible from the viewpoint of suppressing sintering between particles during the solid solution reaction.
- the composite is granular or massive.
- This is pulverized, pulverized, and / or classified into a powder of a predetermined size.
- it is preferable to perform the final adjustment of the grain size in the crystal defect removal process described later, which is necessary to achieve the predetermined D50 and D10. In this case, it should be processed so that D50 is about 30 m or less.
- Specific examples of the treatment include a method of subjecting the synthesized product to sieve classification with an opening of about 45 am, and passing the sieved powder to the next process, or the synthesized product to a ball mill, a vibration mill, or a jet mill.
- pulverizing to a predetermined particle size using general grinders, such as these, is mentioned. In the latter method, excessive pulverization not only generates fine particles that easily scatter light, but also generates crystal defects on the particle surface, leading to a decrease in luminous efficiency.
- the powder obtained by the pulverization process without using the pulverization process and by the pulverization process in which the D50 by the jet mill pulverizer is about 6 am or more is finally high luminescence. Showed efficiency.
- the phosphor powder synthesized in the first step is heat-treated in a nitrogen atmosphere at a temperature range of 1450 ° C to 1650 ° C. .
- a temperature of 1450 ° C or higher the effect of reducing crystal defects is increased, where the diffusion of the material easily occurs, and the processing at 1650 ° C or lower causes the sintering between particles to progress, resulting in coarse secondary particles, An increase in the crystal defect concentration can be prevented, which is preferable.
- the heat treatment time is preferably maintained in the above temperature range for at least 1 hour. By making it longer than 1 hour, a sufficient crystal defect reduction effect can be obtained.
- the concentration of crystal defects can be effectively reduced by making the pressure of the nitrogen atmosphere as close to atmospheric pressure as possible, and it is preferably 1 atm or more and 3 atm or less.
- the second step of reducing crystal defects it is preferable! /
- the following method is also useful. That is, the phosphor containing Eu // 3-type sialon obtained in the first step is heat-treated at 1200 ° C. or higher and 1550 ° C. or lower in vacuum, and further acid-treated.
- ⁇ -sialon is thermodynamically unstable at high temperature and low pressure, and Si, N, A1N and
- the temperature and vacuum degree of the heat treatment can be adjusted to selectively decompose only the portion having a high crystal defect concentration, which is considered to reduce the crystal defect density.
- an appropriate heat treatment temperature varies depending on the degree of vacuum, a temperature range of 1200 ° C to 1550 ° C is preferable. Above 1200 ° C, the decomposition of / 3 type sialon proceeds and the density of crystal defects decreases. Rapid decomposition of type 0 sialon can be suppressed at temperatures below 1550 ° C.
- the phosphor containing Eu / 3 type sialon obtained in the first step is 1300 ° C or more in an inert atmosphere mainly containing a gas other than nitrogen having a nitrogen partial pressure of lOkPa or less.
- Heat treatment is performed at 00 ° C or lower, followed by acid treatment.
- the Si amount after heating is in the range of 1 wt% to 30 wt% in order to reduce the crystal defect density.
- a known technique such as dissolution removal with acid or alkali can be employed.
- the dissolution treatment with a mixture of hydrofluoric acid and nitric acid can quickly remove Si, and can be a by-product during the synthesis of / 3 sialon. /! Preferable because A1N polytype can be removed! /.
- the heat treatment in the first step and the heat treatment in the second step may be performed continuously at the time of cooling after heating in the first step described above, but after adjusting to a predetermined particle size, It is more effective to perform heat treatment. This is because crystal defects formed during crushing and crushing can be removed in addition to crystal defects formed during firing. In the heat treatment in the second step, the sintering between the particles does not proceed at all, the particle size is almost the same as that before the heat treatment, and it is not necessary to adjust the particle size again after the heat treatment.
- the phosphor mainly composed of 13-type sialon according to the present embodiment is used in a light emitting device including a light emitting source and a phosphor, and excites ultraviolet light or visible light having a wavelength of 350 nm to 500 nm.
- a light emitting device including a light emitting source and a phosphor
- it By irradiating as a source, it has emission characteristics with a peak in the wavelength range of 520 nm or more and 550 nm or less, so it can be combined with an ultraviolet LED or blue LED and, if necessary, a red phosphor and / or a blue phosphor. Therefore, white light can be easily obtained.
- the / 3 type sialon has a small decrease in luminance at high temperatures, so that a light emitting device using the / 3 type sialon does not deteriorate even when exposed to high temperatures where the luminance decrease and chromaticity shift are small, and further improves heat resistance. Since it is excellent and has excellent long-term stability in an oxidizing atmosphere and moisture environment, the light-emitting device is characterized by high brightness and long life, reflecting these factors.
- the light-emitting device of the present embodiment is configured using at least one light-emitting light source and a phosphor mainly composed of the 13-type sialon of the present embodiment.
- the light-emitting device of this embodiment includes an LED, a phosphor lamp, and the like.
- known light-emitting devices described in Japanese Patent Laid-Open Nos. 5-152609, 7-99345, and 2927279 are known. By the method, an LED can be manufactured using the phosphor of this embodiment.
- an ultraviolet LED or a blue LED that emits light having a wavelength of 350 nm or more and 500 nm or less, particularly preferably a blue LED that emits light having a wavelength of 440 nm or more and 480 nm or less.
- nitride semiconductors such as GaN and InGaN, and by adjusting the composition, they can be light emitting light sources that emit light of a predetermined wavelength.
- a light emitting device in addition to the method of using the phosphor of the present embodiment alone, By using in combination with a phosphor having other light emission characteristics, a light emitting device that emits a desired color can be configured.
- a blue LED is used as an excitation source
- white light emission in a wide range of color temperatures is possible when the phosphor of this embodiment is combined with a yellow phosphor having an emission peak in the region of 575 nm to 590 nm.
- Examples of such a phosphor include ⁇ -sialon in which Eu is dissolved.
- color rendering and color reproducibility can be improved by combining with a red phosphor having an emission wavelength peak of 600 nm or more and 700 nm or less, such as CaAlSiN: Eu.
- a white light source that is rich in color rendering properties suitable for various indoor and outdoor lighting, has color reproducibility suitable for a backlight light source of a liquid crystal display device, etc., and has excellent high-temperature characteristics.
- the phosphor of the present embodiment is represented by the general formula: Si AI ON, and contains a Eu // 3 type support.
- the phosphor having such a configuration is excellent as a green phosphor because it is excited in a wide wavelength range from ultraviolet to visible light and emits green light with a high efficiency within a range of 520 nm to 550 nm as a main wavelength. ing. Therefore, it can be suitably used for various light emitting elements, particularly white LEDs using UV LEDs or blue LEDs as a light source, alone or in combination with other phosphors.
- the lattice constant a of the main component ⁇ -sialon is preferably 0.776 08 or more and 0.7620 or less, lattice constant c force SO. 2908 or more and 0.2920 or more.
- the Eu content is 0.1 mass% or more and 3 mass% or less.
- the diffraction line intensity of the (111) plane of silicon was 1% of the diffraction line intensity of the (101) plane of 13-type sialon.
- the diffraction line intensities other than silicon and ⁇ -sialon are preferably 10% or less with respect to the diffraction line intensity of the (101) plane of ⁇ -sialon.
- silicon absorbs light of a wide wavelength range from ultraviolet to visible light and converts it into heat, if it is present even in a very small amount in the phosphor, fluorescence emission is significantly inhibited.
- the diffraction line intensity of the (111) plane of silicon is within the above range, the luminance of fluorescence emission is improved.
- the diffraction line intensity other than silicon and / 3 type sialon is within the above-mentioned range, it means that there are few impurities other than silicon, and the luminance of fluorescent light emission is similarly improved.
- the above-mentioned phosphor has a particle size distribution measured by a laser diffraction scattering method, and the 50% diameter (D50) in the integrated fraction is 6 111 or more and 30 111 or less and 10% diameter (D10 It is preferable that the force is m or more and the specific surface area is 0.5 m 2 / g or less.
- the light emitting device of this embodiment includes the above-described phosphor and a light emitting light source.
- the light-emitting device having such a configuration uses the phosphor having a / 3 type sialon as a main component as described above, the / 3 type sialon has both thermal and chemical stability. Reflecting this feature, it has a feature that it has a small decrease in brightness even when used at high temperatures and has a long life.
- the above-described light-emitting device preferably includes ultraviolet light or visible light as the above-described light-emitting light source, which may include another phosphor having an emission wavelength peak of 600 nm to 700 nm. You can use a light source that can emit light!
- a blue LED capable of emitting visible light having a wavelength of 440 nm to 480 nm or ultraviolet light having a wavelength of 350 nm to 410 nm.
- UV light that can emit light is used as the light source, or the light from such a light source is combined with phosphors mainly composed of / 3-type sialon and red or blue phosphors as necessary. Therefore, white light can be easily provided. Therefore, such a light emitting device is, for example, a backlight of a display device such as a liquid crystal device or various indoor / outdoor illuminations. It can be applied to various uses such as devices.
- the phosphor manufacturing method of the present embodiment includes a first step of generating Eu-type / 3-type sialon and a temperature range of 1450 ° C to 1650 ° C in a nitrogen atmosphere. A second step of reducing the crystal defect density by heat-treating for more than a time.
- the phosphor production method of the present embodiment includes a first step of producing Eu-containing / 3-type sialon, and heat treatment in a temperature range of 1200 ° C to 1550 ° C in vacuum. Further, a second step of reducing the crystal defect density by acid treatment may be included.
- the phosphor manufacturing method of the present embodiment includes a first step of generating Eu-type / 3-type sialon and a gas other than nitrogen having a nitrogen partial pressure of lOkPa or less as a main component.
- the light emission as described above can be achieved by simply performing a simple heat treatment or acid treatment on Eu-activated / 3-type sialon obtained by a conventionally known production method.
- a phosphor with excellent characteristics can be produced with good reproducibility.
- ⁇ -type nitride nitride powder manufactured by Ube Industries, Ltd. (“SN-E10” grade, oxygen content 1.2 mass%, / 3-phase content 4.5 mass%) 95.5 mass%, aluminum nitride powder manufactured by Tokuyama (“F” grade, oxygen content 0.9% by mass) 3.3% by mass, aluminum oxide powder manufactured by Daimei Chemicals (“TM-DAR” grade) 0.4% by mass, europium oxide manufactured by Shin-Etsu Chemical Co., Ltd. Powder (“RU” grade) 0.8% by mass was blended to obtain 1 kg of a raw material mixture.
- the above-mentioned raw material mixture was mixed by a dry mixer for 60 minutes using a rocking mixer ("RM-10" manufactured by Aichi Electric Co., Ltd.), and further passed through a stainless steel sieve having an opening of 150 m for phosphor synthesis.
- Raw material powder was obtained.
- the raw material powder is filled into a 100 ml measuring cylinder and the quality of the powder is The force and bulk density were measured by dividing the quantity by the bulk volume and found to be 0.4 g / cm 3 .
- JES-FE2XG type ESR measuring device manufactured by JEOL Ltd. was used.
- the measurement conditions were as follows.
- Magnetic field sweep range 3200-3400gauss (320-340mT)
- Irradiation microwave 10mW, 9.25GHz,
- the ESR spectrum is usually observed as a first-order differential curve in order to sharply observe the unevenness of the absorption spectrum of electromagnetic waves. Since the absorption intensity is proportional to the number of spins, the ESR absorption spectrum was integrated twice, the differential curve was converted to an integral curve, and quantified from the area ratio with the standard sample.
- the number of spins of the standard sample is 1.0 X of 1,1-diphenyl-2-rucyclylhydrazyl ((CH 3) NNC H (NO 2), hereinafter referred to as “DPPH”) whose spin number is known. 10- 5 mol
- ESR measurement was performed on 0.5 mL of L / L benzene solution (3.0 X 10 15 spins), and the peak area ratio between the standard sample and the DPPH solution was obtained.
- FIG. 1 shows the results of excitation'fluorescence spectrum measurement of the phosphor powder obtained in Comparative Example 1.
- the phosphor of Comparative Example 1 was excited at a wide range of wavelengths from ultraviolet to blue, and exhibited a relatively sharp fluorescence spectrum with a peak wavelength of 540 nm and a half-value width of 54 nm.
- a cylindrical boron nitride container with a lid of 60 mm in diameter and 40 mm in height (“N-1” grade manufactured by Denki Kagaku Kogyo Co., Ltd.) was filled with 20 g of the powder synthesized in Comparative Example 1, and atmospheric pressure nitrogen was applied in a carbon heater electric furnace. Heat treatment was performed at 1600 ° C for 8 hours in the atmosphere. The obtained powder passed through a sieve with an opening of 45 m, which had almost the same properties as before heating without shrinkage due to sintering.
- Example 1 Except as in Example 1 except that the conditions are 9 atmospheres of N gas pressure atmosphere and 1950 ° C for 8 hours.
- the same heat treatment was performed.
- the obtained powder showed some shrinkage due to sintering between particles, and the passing rate of a sieve having an opening of 45 ⁇ m was about 60%.
- Example 2 Exactly the same heat treatment as in Example 1 except for 1 hour at 1400 ° C in a vacuum of l Pa Went. The color of the resulting powder changed from green before treatment to brownish green
- the obtained powder did not shrink due to sintering or the like, and all passed through a 45 ⁇ sieve.
- the powder obtained in Comparative Example 3 was treated in a 1: 1 mixed acid of 50% hydrofluoric acid and 70% nitric acid.
- FIG. 1 shows the results of excitation and fluorescence spectrum measurement of the phosphor powder obtained in Example 2.
- the heat treatment was performed in exactly the same manner as in Example 1 except that the conditions were 1450 ° C and 8 hours in an atmospheric pressure argon atmosphere.
- the color of the obtained powder changed from green before processing to dark green.
- the obtained powder did not shrink due to sintering or the like, and all passed through a sieve with an opening of 45 am.
- the suspension changed from dark green to bright green. Thereafter, the acid-treated powder was washed with water and dried to obtain a phosphor powder.
- a powder composed mainly of type 0 sialon was synthesized under the same conditions as in Comparative Example 1 except that the raw material composition containing no europium oxide powder was used.
- Comparative Example 2 The powder obtained in Comparative Example 2 was heat-treated under exactly the same conditions as in Example 1 to obtain a powder
- the intensity is strong with UV LED or blue LED emitting light with a wavelength of 350-500 nm as excitation light. Green light can be emitted.
- a blue or ultraviolet light emitting diode is used as the excitation light source of the phosphor of the above-described embodiment, and in addition to the phosphor of the above-described embodiment, another phosphor that emits light of other colors is used in combination. A white LED with good emission characteristics can be realized.
- Type sialon Eu phosphor (emission peak wavelength: 585 nm, luminous efficiency when excited at 450 nm: 60%) was each treated with a silane coupling agent (“KBE402” manufactured by Shin-Etsu Silicone). Appropriate amounts of these two types of phosphors treated with silane coupling in various ratios are kneaded with epoxy resin (“NLD-SL-2101” manufactured by Sanurec) and placed on a blue LED device with an emission wavelength of 450 nm. Potting, vacuum degassing and heat curing were carried out to produce a surface mount LED (light emitting device) of Example 4.
- a silane coupling agent (“KBE402” manufactured by Shin-Etsu Silicone).
- Appropriate amounts of these two types of phosphors treated with silane coupling in various ratios are kneaded with epoxy resin (“NLD-SL-2101” manufactured by Sanurec) and placed on a blue LED device with an emission wavelength of 450 nm. Pot
- the white light-emitting device of Comparative Example 6 was produced using the phosphor of Comparative Example 1.
- Example 4 The light emitting devices of Example 4 and Comparative Example 6 were made to emit light under the same energization conditions, and the central illuminance and chromaticity (CIE1931) under the same conditions were measured with a luminance meter. Comparing the central illuminance with a white light emitting device with chromaticity coordinates (x, y) of (0.31, 0.32), the light emitting device of Example 4 is 1.5 times that of the light emitting device of Comparative Example 6. Was the brightness. [0118] (Example 5)
- a red phosphor having a composition of Ca Eu AlSiN and the phosphor obtained in Example 2 (light emitting pin).
- the light emitting device of Example 5 was superior in color rendering properties to the light emitting devices of Example 4 and Comparative Example 6.
- ⁇ -type nitride nitride powder manufactured by Ube Industries, Ltd. (“SN-E10” grade, oxygen content 1.2 mass%, / 3-phase content 4.5 mass%) 95.4 mass%, aluminum nitride powder manufactured by Tokuyama (“E” grade, oxygen content 0.8% by mass) 3.0% by mass, aluminum oxide powder made by Daimei Chemicals (“TM-DAR” grade) 0.7% by mass, europium oxide by Shin-Etsu Chemical Co., Ltd. Powder (“RU” grade) 0.8% by mass was blended to obtain 1 kg of a raw material mixture.
- the raw material mixture was mixed by dry using a V-type mixer for 30 minutes, passed through a sieve with an opening of 150 ⁇ m, and cylindrical nitriding with a lid with a diameter of 16 cm x height of 16 cm Fill a boron container (N-1 grade, manufactured by Denki Kagaku Kogyo Co., Ltd.) with 900g, and heat it at 2000 ° C for 15 hours in a pressurized nitrogen atmosphere of 0.9MPa in a carbon heater electric furnace. It was. The resulting product was a loose, agglomerated mass that could be lightly loosened by hand wearing clean rubber gloves. In this way, the lightly pulverized powder was able to pass through a sieve with an opening of 150 m. By these operations, about 880 g of synthetic powder was obtained.
- the above-mentioned synthetic powder was pulverized with a supersonic jet pulverizer (PJM-80SP, manufactured by Nippon Pneumatic Industry Co., Ltd.) to obtain pulverized powders of Examples 6-8.
- a supersonic jet pulverizer (PJM-80SP, manufactured by Nippon Pneumatic Industry Co., Ltd.)
- the particle size of the pulverized powder can be controlled by the sample supply speed to the pulverization chamber and the pulverization air pressure.
- Table 4 shows the grinding conditions and the particle size distribution of the ground powder.
- Example 7 4 8 0 0-5 4.3 8 .0 1 2 .2
- the pulverized powder was subjected to the same heat treatment in an atmospheric pressure argon atmosphere as in Example 3 and a treatment with a mixed acid of hydrofluoric acid and nitric acid.
- Spin density on the absorption of g 2. 00 ⁇ 0. 02 at room temperature in ESR spectrum measurement are both less IX 10- 17 pieces / g, XRD measurement results, any crystalline phase / 3-inch sialon single
- the lattice constant a was 7.61 Onm and the lattice constant c was 2.913 nm.
- Table 5 shows the particle size distribution measured by the particle size distribution analyzer and the gas adsorption method. Table 5 shows the BET multipoint analysis, and Table 6 shows the fluorescence characteristics when excited with blue light at a wavelength of 450 nm.
- Example 6 Under the very weak grinding conditions of Example 6, the secondary particles are mainly loosened into the primary particles, and the destruction of the primary particles does not progress so much. Therefore, the average particle size is Compared to the light body (for example, Example 3), it has the same light emission characteristics although it is small. When the pulverization conditions were further strengthened, the phosphor particle size was reduced, and the light emission efficiency, particularly the light absorption rate, was reduced.
- Example 6 and Example 8 were subjected to fine powder removal treatment by wet precipitation (Example 9 and Example 10 respectively). After thoroughly dispersing in 10 ml of distilled water to which sodium hexametaphosphate was added using 10 g of the phosphor powder as a dispersant, it was transferred to a container with an inner size of 80 mm and a height of 140 mm. Then, it was left to stand for 80 minutes, and the supernatant liquid of 90 mm was removed from the water surface. Again, the operation of adding an aqueous hexametaphosphoric acid solution, dispersing and allowing to stand for a predetermined time, and then removing the supernatant was repeated until the supernatant became transparent.
- the phosphor of the present invention comprising a / 3-type sialon as a main component is excited at a wide wavelength range from ultraviolet to blue light and exhibits high-luminance green light emission. Therefore, a white LED using blue or ultraviolet light as a light source is used.
- the phosphor can be suitably used as a fluorescent material, and can be suitably used for lighting equipment, image display devices, and the like.
- the phosphor of the present invention has little decrease in luminance at high temperatures and is excellent in heat resistance and moisture resistance, so that the phosphor of the present invention can be used in the above-mentioned lighting equipment and image display device fields, so that the use environment temperature can be reduced. It can exhibit the characteristics of excellent long-term stability with small changes in luminance and emission color with respect to changes.
- the method for producing a phosphor of the present invention is very useful industrially because it can stably provide the phosphor having the above-mentioned characteristics.
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Description
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US12/515,335 US8404152B2 (en) | 2006-11-20 | 2007-11-20 | Fluorescent substance and production method thereof, and light emitting device |
EP07832173.4A EP2093272B1 (en) | 2006-11-20 | 2007-11-20 | Fluorescent substance and production method thereof, and light emitting device |
JP2008545403A JP4891336B2 (ja) | 2006-11-20 | 2007-11-20 | 蛍光体及びその製造方法、並びに発光装置 |
CN2007800500299A CN101600778B (zh) | 2006-11-20 | 2007-11-20 | 荧光物质及其生产方法、以及发光器件 |
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US8404152B2 (en) | 2013-03-26 |
JP2012052127A (ja) | 2012-03-15 |
EP2093272A4 (en) | 2009-12-30 |
CN101600778A (zh) | 2009-12-09 |
EP2093272A1 (en) | 2009-08-26 |
TWI357927B (en) | 2012-02-11 |
CN101600778B (zh) | 2013-10-23 |
TW200835776A (en) | 2008-09-01 |
KR100985680B1 (ko) | 2010-10-05 |
KR20090084946A (ko) | 2009-08-05 |
JPWO2008062781A1 (ja) | 2010-03-04 |
EP2093272B1 (en) | 2016-11-02 |
JP4891336B2 (ja) | 2012-03-07 |
US20100053932A1 (en) | 2010-03-04 |
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