JP6606841B2 - Method for producing fluorescent material molded body, light emitting device - Google Patents

Description

  The present invention relates to a method for manufacturing a fluorescent material molded body and a light emitting device.

  As a light emitting device using a phosphor, there is known a light emitting device that emits white light by combining an LED chip that emits blue light and a YAG (yttrium, aluminum, garnet) phosphor that converts blue light into yellow. Yes. Such a light-emitting device is characterized by being small in size and low in power consumption, and has been developed for further improvement in efficiency and reliability as a light source for various display devices or lighting devices. In the future, further increase in output of the light emitting device is desired, and improvement in reliability of the phosphor is demanded.

  In addition, a projector is used as an image projection apparatus that projects a screen of a personal computer, a video image, an image based on image data stored in a memory card or the like onto a screen. Conventionally, projectors using a high-intensity discharge lamp as a light source have been the mainstream, but projectors using light emitting diodes (LEDs) and laser diodes (LDs) have been developed in recent years. Phosphors are also used in projectors using these LEDs, and there is a demand for improved phosphor reliability.

For example, a wavelength conversion member in which a specific phosphor is dispersed in a glass having a softening point of 700 ° C. or higher is known as a phosphor used for such a light emitting device or projector (for example, Patent Document 1). reference). Here, it is described that oxynitride glass is used as a glass having a softening point of 700 ° C. or higher, and α sialon phosphor, β sialon phosphor, and CaAlSiN ₃ phosphor are used as specific phosphors. Thus, it is described that a wavelength conversion member capable of obtaining fluorescence with higher efficiency than conventional can be provided.

  Further, a method for manufacturing a fluorescent material molded body using a discharge plasma sintering method for a mixture of phosphor powder and inorganic member powder is known (for example, see Patent Document 2).

Japanese Patent No. 4895541 JP 2009-91546 A

  However, since the output from the light emitting diode is very high in the projector application, it has been a problem that the wavelength conversion member described in Patent Document 1, particularly oxynitride glass, is melted by light energy or heat.

  Moreover, since the fluorescent substance molded body described in Patent Document 2 uses an inorganic member powder made of oxide for a nitride-based phosphor, an oxynitride-based phosphor, and a sialon-based phosphor, the phosphor and the phosphor The inorganic member powder reacted to cause a decrease in light emission characteristics.

  Therefore, an object of this invention is to provide the manufacturing method of the reliable fluorescent substance molded object which has heat resistance.

  In the method for producing a phosphor molded body according to an embodiment of the present invention, a mixture of aluminum nitride powder and phosphor powder is melted by a discharge plasma sintering method, and then cooled.

  A light-emitting device according to an embodiment of the present invention includes a light-emitting element that emits light having an emission peak wavelength of 300 nm to 500 nm, and a phosphor molded body that contains phosphor powder with aluminum nitride as a main component.

  Thereby, the manufacturing method of the reliable fluorescent substance molded object which has heat resistance can be provided. In addition, a light-emitting device using a highly reliable fluorescent material molded body having heat resistance can be provided.

It is a schematic perspective view which shows the fluorescent substance molded object which concerns on embodiment. It is a schematic explanatory drawing which shows the discharge plasma sintering apparatus 100 which concerns on embodiment. It is a schematic explanatory drawing which shows the measuring method using an integrating sphere. It is a figure which shows the measurement result of the light beam and excitation light output of the fluorescent substance molded body plate 250 obtained in Example 1, 2 and Comparative Examples 1 thru | or 3. It is a figure which shows the emission spectrum of the fluorescent substance molded object plate 250 which concerns on Example 1. FIG. It is a figure which shows the emission spectrum of the fluorescent substance molded object plate 250 which concerns on Example 2. FIG.

  Hereinafter, a fluorescent substance molded body, a manufacturing method thereof, and a light emitting device according to an embodiment of the present invention will be described with reference to the drawings. However, the present invention is not limited to this embodiment and example. FIG. 1 is a schematic perspective view showing a fluorescent material molded body according to an embodiment. FIG. 2 is a schematic explanatory view showing a discharge plasma sintering apparatus according to the embodiment.

<Fluorescent material compact>
The phosphor molded body 10 according to the embodiment is obtained by cooling the aluminum nitride powder after melting the mixture of the phosphor powder 20 and the aluminum nitride powder 30 using a discharge plasma sintering method. Thereby, it can suppress that the conversion efficiency of fluorescent substance powder falls by the melt diffusion or thermal diffusion of fluorescent substance powder and aluminum nitride in a discharge plasma sintering process. In addition, since the interface between the phosphor powder and aluminum nitride can be made substantially continuous in terms of composition and crystallinity, light loss at the junction interface between the phosphor powder and aluminum nitride can be reduced. The shape of the fluorescent material molded body 10 is not particularly limited, but may be a flat plate shape, a cylindrical shape, a rectangular parallelepiped shape, or the like. Although the thickness of the fluorescent substance molded object 10 is not specifically limited, It can be set as the thickness which the light radiate | emitted from the light emitting element permeate | transmits. For example, the thickness of the fluorescent substance molded body 10 can be set to 0.5 mm to 5.0 mm. Further, a thin fluorescent material molded body 10 having a high density of the phosphor 20 that can block most of the light emitted from the light emitting element, but can emit light from the fluorescent material molded body 10 with high output. You can also The magnitude | size of the fluorescent substance molded object 10 is not specifically limited. The fluorescent material molded body 10 can be used as it is obtained by the discharge plasma sintering method. However, in order to obtain a predetermined size, the side surface of the fluorescent material molded body 10 is cut by a cutting machine, or the fluorescent material molded body 10 A part may be scratched, and stress may be applied along the wound to be divided. Further, after the cutting or dividing, the side surface of the fluorescent material molded body 10 may be polished. Moreover, although it can be used even if it does not grind | polish the surface of the fluorescent substance molded object 10, what grind | polished the surface of the fluorescent substance molded object 10 and made unevenness | corrugation small can also be used. The concentration of the phosphor 20 in the phosphor molded body 10 is preferably 10% by weight or more, but 5% by weight or more can also be used.

  The phosphor powder 20 and the aluminum nitride powder 30 that are the raw materials of the phosphor molded body 10 will be described in detail.

(Phosphor, phosphor powder)
The phosphor molded body 10 contains a phosphor (phosphor powder) 20. In the specification, “phosphor powder” mainly means a state used as a raw material before being compounded as a phosphor molded body, and “phosphor” means a state after being compounded as a phosphor molded body. To do. The phosphor 20 only needs to absorb light emitted from the light emitting element, perform wavelength conversion, and emit light having a wavelength different from that of the light emitting element. The magnitude | size of the fluorescent substance powder 20 is not specifically limited, The thing of about several nm to several dozen micrometer can be used. The phosphor powder 20 is preferably about 3 μm to 10 μm from the viewpoint of ease of handling.

  Here, in the present specification, the particle size value indicates a value of an average particle size using an air permeation method called Fisher Sub Sieve Sizer's No (Fisher, sub, sheave, sizers, number).

  Specific examples of the phosphor powder 20 used as a raw material include the following. For example, it is preferably at least one selected from a nitride phosphor mainly activated by a lanthanoid element such as Eu or Ce, or an aluminate phosphor. Nitride-based phosphors include oxynitride-based phosphors and sialon-based phosphors. As specific examples, the following phosphors can be used, but are not limited thereto.

Nitride phosphors are mainly activated by lanthanoid elements such as Eu and Ce. Examples of the nitride-based phosphor include M ₂ Si ₅ N ₈ : Eu, MAlSiN ₃ : Eu (wherein M is at least one selected from Sr, Ca, and Ba). In addition to M ₂ Si ₅ N ₈ : Eu, there are MSi ₇ N ₁₀ : Eu, (La, Y, Gd) ₃ Si ₆ N ₁₁ : Ce, and the like.

The oxynitride phosphor is mainly activated by a lanthanoid element such as Eu or Ce. Examples of the oxynitride phosphor include MSi ₂ O ₂ N ₂ : Eu (M is at least one selected from Sr, Ca, and Ba).

Sialon phosphors are mainly activated by lanthanoid elements such as Eu and Ce. Sialon _{phosphor, M m / n Si 12- (} m + n) Al (m + n) O n N (16-n): Eu (M is at least one selected Sr, Ca, Li, from Y N = 0 to 2.5, m = 0.5 to 5, n: M charge, x = 0.75 to 1.5), or Si _6-z Al _z O _z N _8-z : Eu (0 <z <4.2).

The aluminate phosphor is mainly activated by a lanthanoid element such as Ce. The aluminate phosphor is composed of Y ₃ Al ₅ O ₁₂ : Ce, (Y _0.8 Gd _0.2 ) ₃ Al ₅ O ₁₂ : Ce, Y ₃ (Al _0.8 Ga _0.2 ) ₅ O ₁₂ : Ce, (Y, Gd) ₃ (Al, Ga) ₅ O ₁₂ : There is a YAG-based phosphor represented by a composition formula of Ce. Further, there are Tb ₃ Al ₅ O ₁₂ : Ce, Lu ₃ Al ₅ O ₁₂ : Ce, etc. in which a part or all of Y is substituted with Tb, Lu or the like.

  The phosphor described above contains at least one selected from Tb, Cu, Ag, Au, Cr, Nd, Dy, Co, Ni, and Ti instead of Eu or in addition to Eu as desired. You can also.

  Moreover, it is fluorescent substance other than the said fluorescent substance, Comprising: The fluorescent substance which has the same performance and effect can also be used.

These phosphors can be used with those having emission spectra in yellow, red, green, and blue by the excitation light from the light-emitting element, and also have emission spectra in yellow, blue-green, orange, etc., which are intermediate colors of these phosphors. It can also be used. By using these phosphors in various combinations, light emitting devices having various emission colors can be manufactured.
(Aluminum nitride, aluminum nitride powder)
The fluorescent material molded body 10 contains an aluminum nitride powder 30. In the specification, “aluminum nitride powder” mainly means a state used as a raw material before being compounded as a fluorescent material molded body, and “aluminum nitride” means a state after being compounded as a fluorescent material molded body. To do. The aluminum nitride powder 30 is used to hold the phosphor powder 20. Further, there is no particular limitation as long as a part of the light emitted from the light emitting element or a part of the light emitted from the phosphor 20 is transmitted. Specifically, the aluminum nitride powder 30 is a ceramic.

Part of the aluminum nitride powder 30 may be added with aluminum oxide powder or other inorganic member powder. It is preferable that aluminum oxide is 30 wt% or less with respect to the aluminum nitride powder.
(Discharge plasma sintering method)
The discharge plasma sintering apparatus 100 used for the discharge plasma sintering method applies a pulsed large current to the powder mixture of the phosphor powder 20 and the aluminum nitride powder 30 at a low voltage, and instantaneously occurs due to a spark discharge phenomenon. The aluminum nitride powder is melted by the high energy of the discharge plasma. In the discharge plasma sintering apparatus 100, a powder mixture is sandwiched between an upper punch 110, a lower punch 120, and a sintering die 130 made of carbon. The sintering die 130 has a cylindrical shape, and a powder mixture is disposed inside the cylindrical shape. At least one of the upper punch 110 and the lower punch 120 can move up and down in the cylindrical interior of the sintering die 130. The upper punch 110 and the lower punch 120 are sandwiched between the upper punch electrode 140 and the lower punch electrode 150. The upper punch electrode 140 is connected to the upper punch 110, and the lower punch electrode 150 is connected to the lower punch 120. The upper punch electrode 140 and the lower punch electrode 150 can apply pressure in the direction of compressing the powder mixture through the upper punch 110 and the lower punch 120. The powder mixture, the upper punch 110, the lower punch 120, and the sintering die 130 are disposed in the vacuum chamber 160. The upper punch electrode 140 and the lower punch electrode 150 are electrically connected to a power source 170.
<Method for producing phosphor molded article>
The phosphor molded body 10 can be manufactured by melting a mixture of the phosphor powder 20 and the aluminum nitride powder 30 by using a discharge plasma sintering method, and then cooling the mixture.

  (1) A mixture of the measured phosphor powder 20 and the measured aluminum nitride powder 30 is disposed in a space sandwiched between the upper punch 110, the lower punch 120, and the sintering die 130.

  (2) A predetermined voltage is applied from the power source 170 using the upper punch electrode 140 and the lower punch electrode 150, and a predetermined current flows. The upper punch 110 connected to the upper punch electrode 140 and the lower punch 120 connected to the lower punch electrode 150 generate heat. The current is applied in the form of pulses at microsecond intervals. The voltage is around 10 volts and the current is several hundred amperes or more, but it is appropriately changed depending on the amount and type of the mixture. Further, the charging time is appropriately changed depending on the amount and type of the mixture, but it is an extremely short time of about 1 minute to 15 minutes. The heating rate can be appropriately changed according to the amount and type of the mixture, and can be set to, for example, a current of 100 A / min to 300 A / min. While passing an electric current, a vertical pressure is applied to the upper punch 110 and the lower punch 120. Although the pressure to apply changes suitably, it is 15KN or more, Preferably it is 30KN-3MN. It corresponds to the pressure per unit area (punch). The temperature in the vacuum chamber is preferably 2000 ° C. or lower. Although a vacuum chamber is used, air, an argon atmosphere, a nitrogen atmosphere, or the like can also be used. In this way, since the current flows in the form of pulses at microsecond intervals, discharge plasma is generated at the contact portion between the mixtures. By effectively applying the high energy of the high temperature plasma generated instantaneously by this discharge plasma to thermal diffusion, electric field diffusion, etc., it takes about 3 to 20 minutes including temperature rise and hold in the ultrahigh temperature range from low temperature to 2000 ° C or higher. “Sintering” and “sinter bonding” can be performed in a short time. The above is referred to as a discharge plasma sintering method.

  (3) Thereby, the fluorescent material molded body 10 in which aluminum nitride is melted is obtained.

  In consideration of light extraction efficiency and mechanical strength, the sintered density of the phosphor molded body 10 is preferably 85% or more with respect to the true density.

  However, when the sintered compact 10 is formed with a high sintering density, chromaticity / luminance unevenness is likely to occur. Therefore, when the sintered density of the fluorescent material molded body 10 is increased, it is preferable to perform an annealing treatment after the cooling step of the discharge plasma sintering method. The annealing process is performed under a temperature and an atmosphere selected according to the type of the phosphor molded body. For example, it is performed in the air, in nitrogen, or in a hydrogen / nitrogen mixed gas. The annealing treatment may be performed immediately after the molded body is sintered, or may be performed after cutting the molded body. Thereby, the light-diffusion effect can be brought about to the fluorescent substance molded object 10. FIG. The reason why the light diffusion effect is increased by the annealing process is that the activator in the vicinity of the grain boundary of the phosphor powder deactivated in the sintering process is reactivated and the difference in refractive index from aluminum nitride becomes remarkable. it is conceivable that. The light emitting device incorporating the fluorescent material molded body 10 obtained in this way can obtain uniform light emission without displaying the dice pattern of the light emitting element at the irradiation destination.

  Here, in this specification, the sintered density is expressed as a ratio (%) between the theoretical density calculated by the composition and crystal system of the phosphor and aluminum nitride, and the green density measured by the Archimedes method. Instead of theoretical density, true density can also be used. The true density is measured using, for example, Shimadzu AccuPick. A mixture of phosphor powder and aluminum nitride powder before sintering and molding is put into a predetermined container A and weighed. Thereafter, the container A is filled with He gas to a constant pressure, and then the He gas is released into the container B having a known volume. Finally, by measuring the parallel pressure of the connected containers A and B, the powder volume of the powder mixture can be measured using the total volume and pressure change. The target true density can be calculated from the weight and the resulting powder volume. The density of the molded body is determined by using Archimedes method in which a phosphor molded body whose weight is measured in advance is placed in a container filled with a liquid such as water and the weight of the molded body is divided by the volume of the overflowed water.

Thereby, a fluorescent material molded body with high thermal stability can be produced in an extremely short time. Further, the phosphor powder and the aluminum nitride powder can be strongly combined. Furthermore, it is possible to suppress deterioration in characteristics due to the reaction between the nitride phosphor, the oxynitride phosphor, the sialon phosphor, the aluminate phosphor, and the aluminum nitride powder.
<Light emitting device>
The light emitting device includes at least a light emitting element and a fluorescent material molded body 10. The light emitting element is not limited as long as it excites the phosphor 20 contained in the phosphor molded body 10, but a laser element (LD) or a light emitting diode element (LED) is preferable because it is small and has a long lifetime. The light emitted from the light emitting element is applied to the fluorescent material molded body 10, and the fluorescent material molded body 10 emits light having a wavelength different from that of the light emitting element.
(Light emitting element)
As the light-emitting element, a light-emitting element that emits light in the ultraviolet region, or a light-emitting element that emits light in blue-violet, blue, blue-green, green, or the like can be used. The emission peak wavelength of the light-emitting element is preferably one having an emission peak wavelength in the range of 300 nm to 500 nm, but particularly preferably one having an emission peak wavelength in the range of 380 nm to 480 nm. The light emitting element is preferably a laser element. This is because the fluorescent substance molded body can have heat resistance to light from a laser element having high output. The light emitting element emitting blue light is preferably a group III nitride compound light emitting element. For example, the light emitting device emits light of an n-type GaN layer in which Si is undoped, an n-type contact layer made of n-type GaN doped with Si, an undoped GaN layer, and a multiple quantum well structure via a GaN buffer layer on a sapphire substrate. Layers (GaN barrier layer / InGaN well layer quantum well structure), p-type GaN layer made of p-type GaN doped with Mg, and p-type contact layer made of p-type GaN doped with Mg in this order. What has the laminated structure laminated | stacked can be used.
(Processing of fluorescent material moldings)
The fluorescent material molded body can be processed into a fluorescent material molded body chip 240 having a size of about 3 mm × 3 mm × thickness of 100 μm, for example, by slicing, polishing, dicing and the like. The fluorescent material molded body plate 250 is manufactured by bonding the fluorescent material molded body chip 240 to the heat sink 230. In order to further improve the light extraction efficiency, a dielectric film or a reflective film can be used between the fluorescent material molded body chip 240 and the heat sink 230.

  Hereinafter, the fluorescent substance molded body according to Examples 1 and 2 will be described. FIG. 1 is a schematic perspective view showing a fluorescent material molded body according to an embodiment. FIG. 3 is a schematic explanatory view showing a measurement method using an integrating sphere. FIG. 4 is a diagram showing the measurement results of the luminous flux and the excitation light output of the obtained fluorescent material molded body plate 250 by processing the fluorescent material molded body 10 manufactured in Examples 1 and 2 and Comparative Examples 1 to 3. It is. FIG. 5 is a diagram showing an emission spectrum of the fluorescent material molded body according to Example 1. FIG. FIG. 6 is a diagram showing an emission spectrum of the fluorescent material molded body according to Example 2. FIG.

  The phosphor molded body 10 according to Example 1 is manufactured by a discharge plasma sintering method using phosphor powder 20 and aluminum nitride powder 30 as raw materials.

As the phosphor powder 20, a nitride phosphor represented by CaSiAlN ₃ : Eu is used. The average particle diameter of the CaSiAlN ₃ : Eu phosphor is about 5 μm.

  The specific gravity of the aluminum nitride powder 30 is 3.26 g / cc, and the average particle size is about 1 μm.

The raw material mixing weight ratio of the phosphor powder 20 using the CaSiAlN ₃ : Eu phosphor and the aluminum nitride powder 30 is (CaSiAlN ₃ : Eu phosphor) :( aluminum nitride powder) = 80: 20, and the volume ratio is 80:20.

  As the discharge plasma sintering apparatus 100, an apparatus manufactured by SPS Shintex Co., Ltd. (apparatus type: SPS-9.40MK-VII) is used. A sintered die 130 in which the size of the fluorescent material molded body 10 is a cylindrical shape having a diameter of about 20 mm is used. The upper punch 110, the lower punch 120, and the sintering die 130 are made of graphite. 5.1 g of a mixed raw material of the phosphor powder 20 and the aluminum nitride powder 30 is charged into the sintering die. The vacuum chamber is maintained at about 10 Pa or less, and cooling water is flowing. The vertical punching of the upper punch 110 and the lower punch 120 is about 28 KN. The heating rate is about 50 to 100 ° C./min, and the current is continuously supplied at 1800 ° C. for about 5 minutes. As a result, a cylindrical phosphor molded body 10 having a diameter of about 20 mm, a thickness of 5 to 6 mm, and a sintered density of 96.6% with respect to the true density is obtained.

In Example 2, the phosphor powder 20 is a sialon phosphor (Ca-α-) represented by Ca _x (Si, Al) ₁₂ (O, N) ₁₆ : Eu (x = 0.75 to 1.5). The phosphor molded body 10 is formed in the same manner as in Example 1 except that it is a sialon phosphor) and has an annealing process after the sintering process. The raw material mixing weight ratio of the phosphor powder 20 using the sialon phosphor and the aluminum nitride powder 30 is (sialon phosphor) :( aluminum nitride powder) = 80: 20, and the volume ratio is 80:20. A charge of 5.2 g of the mixed raw material of the phosphor powder 20 and the aluminum nitride powder 30 is used. The heating rate is about 50 to 100 ° C./min, and the current is continuously supplied at 1800 ° C. for about 5 minutes. As a result, a cylindrical phosphor molded body 10 having a diameter of about 20 mm, a thickness of 5 to 6 mm, and a sintered density of 88.1% with respect to the true density is obtained. After the sintering process, annealing at 1400 ° C. is performed for 2 hours. The annealing atmosphere is preferably performed in a reducing atmosphere such as an N ₂ atmosphere or an H ₂ / N ₂ atmosphere.
(Comparative Example 1)
In place of the aluminum nitride powder of Example 1, in Comparative Example 1, an yttrium oxide powder represented by Y ₂ O ₃ is used, and the phosphor molded body 10 is formed in substantially the same manner as in Example 1. The raw material mixing weight ratio of the phosphor powder 20 using the CaSiAlN ₃ : Eu phosphor and the yttrium oxide powder is (CaSiAlN ₃ : Eu phosphor) :( yttrium oxide powder) = 72: 28, and the volume ratio is 80. : 20.

5.9 g of a mixed raw material mixture of phosphor powder 20 and yttrium oxide powder is used. The heating rate is about 50 to 100 ° C./min, and the current is continuously supplied at 1400 ° C. for about 5 minutes. As a result, a cylindrical phosphor molded body 10 having a diameter of about 20 mm, a thickness of 5 to 6 mm, and a sintered density of 84.4% with respect to the true density is obtained.
(Comparative Example 2)
Instead of the aluminum nitride powder of Example 1, in Comparative Example 2, a silicon nitride powder represented by Si ₃ N ₄ is used, and the phosphor molded body 10 is formed in substantially the same manner as in Example 1. The raw material mixing weight ratio of the phosphor powder 20 using the CaSiAlN ₃ : Eu phosphor and the silicon nitride powder is (CaSiAlN ₃ : Eu phosphor) :( silicon nitride powder) = 79: 21, and the volume ratio is 80 : 20. A charge of 5.2 g of the mixed raw material of the phosphor powder 20 and the silicon nitride powder is used. The heating rate is about 50 to 100 ° C./min, and the current is continuously supplied at 1700 ° C. for about 5 minutes. As a result, a cylindrical phosphor molded body 10 having a diameter of about 20 mm, a thickness of 5 to 6 mm, and a sintered density of 84.4% with respect to the vacuum density is obtained.
(Comparative Example 3)
Instead of the aluminum nitride powder of Example 2, in Comparative Example 3, an aluminum oxide powder represented by Al ₂ O ₃ is used, and the phosphor molded body 10 is formed in substantially the same manner as in Example 2. The raw material mixing weight ratio of the phosphor powder 20 using the sialon phosphor and the aluminum oxide powder is (sialon phosphor) :( aluminum oxide powder) = 77: 23, and the volume ratio is 80:20. 5.4 g of the charged raw material mixture of phosphor powder 20 and aluminum oxide powder is used. The temperature rise rate is about 50 to 100 ° C./min, and the current is kept flowing at 1600 ° C. for about 5 minutes. As a result, a cylindrical fluorescent substance molded body 10 having a diameter of about 20 mm, a thickness of 5 to 6 mm, and a sintered density of 92.5% of the true density is obtained. After the sintering process, annealing at 1400 ° C. was performed for 2 hours.
(Measurement)
The phosphor molded body 10 manufactured in Examples 1 and 2 and Comparative Examples 1 to 3 is processed to obtain a phosphor molded body chip 240. Furthermore, the fluorescent material molded body plate 250 is produced by joining the obtained fluorescent material molded body chip 240 to the heat sink 230. The phosphor molded body plate 250 is measured using an integrating sphere 220. The measurement system uses a laser element 200 that emits a laser beam having an emission peak at 460 nm as a light source, and an optical fiber 210 connected to the laser element 200, and a fluorescent substance molded body plate 250 is placed at a position where the laser beam is irradiated. Provide. The fluorescent material molded body plate 250 is fixed to the temperature control block 260. All the light emitted from the fluorescent material molded body plate 250 is incident on the integrating sphere 220 and the light flux is measured.

  From this result, Examples 1 and 2 were able to obtain a higher light output than Comparative Examples 1 to 3. In particular, when the pumping light output is 2000 mW, the output difference is significant. From now on, in the situation where the light output of the light emitting element is intended, the heat resistance and light resistance of the fluorescent material molded body are very important issues, and this embodiment is very meaningful in that this can be solved. .

  Since the fluorescent material molded body manufactured by the method for manufacturing a fluorescent material molded body according to the present embodiment is excellent in heat resistance and light resistance, it can be used in a light emitting device using a high-output light source such as a laser element. Can do. The light-emitting device can be used for projectors, automobile headlights, lighting, and the like.

10 Fluorescent substance molded body 20 Fluorescent substance powder (phosphor)
30 Aluminum nitride powder (aluminum nitride)
100 discharge plasma sintering apparatus 110 upper punch 120 lower punch 130 sintering die 140 upper punch electrode 150 lower punch electrode 160 vacuum chamber 170 power source 200 laser element 210 optical fiber 220 integrating sphere 230 heat sink 240 fluorescent material molded chip 250 fluorescent material molding Body plate 260 Temperature control block

Claims (9)

  A method for producing a fluorescent material molded body, comprising: melting a mixture of an aluminum nitride powder and a nitride phosphor powder by a discharge plasma sintering method, and then cooling the mixture.   The method for manufacturing a fluorescent substance molded body according to claim 1, wherein the aluminum nitride powder is melted and then annealed. The nitride-based phosphor includes M ₂ Si ₅ N ₈ : Eu, MAlSiN ₃ : Eu, MSi ₇ N ₁₀ : Eu, or (La, Y, Gd) ₃ Si ₆ N ₁₁ : Ce (M is Sr, The method for producing a fluorescent substance molded body according to claim 1, wherein the phosphor is a compound of at least one selected from Ca and Ba. The method for producing a fluorescent substance molded body according to any one of claims 1 to 3, wherein a size of the nitride-based phosphor is 3 µm to 10 µm. A light emitting element that emits light having an emission peak wavelength of 300 nm to 500 nm;
As the main component material, it possesses an aluminum nitride, nitride-based fluorescent material and a fluorescent material molded body that is contained in the,
The phosphor molded body has the nitride-based phosphor held by the molten aluminum nitride,
The nitride-based phosphor includes M ₂ Si ₅ N ₈ : Eu, MAlSiN ₃ : Eu, MSi ₇ N ₁₀ : Eu, or (La, Y, Gd) ₃ Si ₆ N ₁₁ : Ce (M is Sr, A light emitting device which is at least one selected from Ca and Ba) .   The light-emitting device according to claim 5, wherein the fluorescent material molded body has a thickness of 0.5 mm to 5.0 mm. The light emitting element, the light emitting device according to claim 5 or 6 which is a laser element that emits light in the blue wavelength band. The light emitting device according to any one of claims 5 to 7, wherein the fluorescent material molded body has a sintered density of 85% or more with respect to a true density. The raw material mixing weight ratio of the nitride-based phosphor and the aluminum nitride is (nitride-based phosphor) :( aluminum nitride powder) = 8 0 : 20 The light-emitting device of description.

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