WO2012043659A1 - 発光素子搭載用セラミックス基体および発光装置 - Google Patents

発光素子搭載用セラミックス基体および発光装置 Download PDF

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Publication number
WO2012043659A1
WO2012043659A1 PCT/JP2011/072247 JP2011072247W WO2012043659A1 WO 2012043659 A1 WO2012043659 A1 WO 2012043659A1 JP 2011072247 W JP2011072247 W JP 2011072247W WO 2012043659 A1 WO2012043659 A1 WO 2012043659A1
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Prior art keywords
light emitting
emitting element
light
mounting
ceramic substrate
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PCT/JP2011/072247
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English (en)
French (fr)
Inventor
邦英 四方
一英 草野
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京セラ株式会社
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Application filed by 京セラ株式会社 filed Critical 京セラ株式会社
Priority to EP11829212.7A priority Critical patent/EP2623479B1/en
Priority to US13/876,366 priority patent/US8981630B2/en
Priority to JP2012512124A priority patent/JP5111686B2/ja
Priority to CN201180046312.0A priority patent/CN103124705B/zh
Publication of WO2012043659A1 publication Critical patent/WO2012043659A1/ja

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Definitions

  • the present invention relates to a ceramic substrate for mounting a light emitting element and a light emitting device in which a light emitting element is mounted on the ceramic substrate for mounting a light emitting element.
  • LEDs light-emitting diodes
  • LEDs have attracted attention as light-emitting elements that can be mass-produced and have high brightness and low power consumption. And it is being widely used as a backlight for light sources for general lighting to electric display panels, mobile phones, personal computers and televisions.
  • the substrate For a substrate on which such a light emitting element is mounted, the substrate itself is required to have high reflectivity and to improve heat dissipation.
  • Patent Document 1 discloses that a highly reflective white ceramic substrate for a semiconductor light emitting element is composed of aluminum oxide and a vitreous component and has a porosity of 5%, and a content of aluminum oxide is 75%. 85% by weight, containing silica, calcium, magnesium and barium as vitreous components, and the average crystal grain size of aluminum oxide is 0.5 ⁇ m or less, so that the reflectance of light at a wavelength of 400 to 740 nm is 90 to It is disclosed that it was 93% or more.
  • the highly reflective white ceramics for semiconductor light-emitting devices disclosed in Patent Document 1 are, according to the example, 75 to 85% by weight of alumina, silica as a vitreous component, and oxides of barium, calcium and magnesium.
  • a sintered body containing about 25 to 15% by weight and having a reflectance of 90% or more with a wavelength of 400 to 740 nm is obtained, but since the crystal grain size of alumina is 0.5 ⁇ m or less, heat conduction There is a problem that the life of the light emitting element is shortened because the rate of the light emitting element is lowered and the action of cooling the light emitting element is reduced.
  • the present invention has been devised in order to solve the above-described problems, and has a high thermal conductivity that can provide high reflectivity and can improve heat dissipation and extend the life of the light-emitting element.
  • An object of the present invention is to provide a ceramic substrate.
  • the ceramic substrate for mounting a light emitting element according to the present invention is a ceramic sintered body for mounting a light emitting element, which is made of a ceramic sintered body and has a mounting portion on which the light emitting element is mounted.
  • the ratio of crystals with a diameter equivalent to a circle of 0.2 ⁇ m or more and 1.0 ⁇ m or less is 45% or more and 80% or less, and the ratio of crystals with a circle equivalent diameter of 2.0 ⁇ m or more and 6.0 ⁇ m or less is 5% or more and 15% or less.
  • the ratio of crystals having an equivalent circle diameter exceeding 6.0 ⁇ m is 2.7% or less.
  • the light-emitting device of the present invention is characterized by mounting the ceramic substrate for mounting a light-emitting element having the above-described configuration.
  • the ceramic substrate for mounting a light emitting element is a ceramic sintered body for mounting a light emitting element comprising a ceramic sintered body and having a mounting portion on which the light emitting element is mounted.
  • the ratio of crystals with an equivalent circle diameter of 0.2 ⁇ m or more and 1.0 ⁇ m or less is 45% or more and 80% or less, and the ratio of crystals with an equivalent circle diameter of 2.0 ⁇ m or more and 6.0 ⁇ m or less is 5% or more and 15% or less, Since the proportion of crystals having an equivalent circle diameter exceeding 6.0 ⁇ m is 2.7% or less, it has a high reflectance and it is easy to maintain a high thermal conductivity.
  • a light emitting device in which a light emitting element is mounted on the ceramic substrate for mounting a light emitting element having the above-described structure, it has high reflectivity and can improve heat dissipation of the light emitting element, thereby extending the life. it can.
  • FIG. 1 is a cross-sectional view showing an example of the configuration of a light emitting device in which a light emitting element is mounted on a ceramic substrate for mounting a light emitting element of this embodiment.
  • the light emitting device 21 using the ceramic substrate 1 for mounting a light emitting element (hereinafter also referred to as the substrate 1) of the present embodiment uses a thick film printing method or the like on one surface 1a of the substrate 1 on which the light emitting element 2 is mounted. Then, electrodes (surface electrodes) 3c and 3d are deposited, and electrode pads 3a and 3b are formed on the portions where the electrodes 3c and 3d are formed by plating or the like, and light emission made of semiconductor is formed on the electrode pads 3a.
  • the element 2 is mounted.
  • the light emitting element 2 and the electrode pad 3b are electrically joined by the bonding wire 32.
  • the bonding between the electrode pad 3a and the light emitting element 2 is bonding using a conductive adhesive, bonding by a bonding wire 32, or bonding by a solder bump, as long as it can be electrically bonded.
  • the electrodes 3c and 3d including the light emitting element 2 and the electrode pads 3a and 3b are covered with a sealing member 31 made of resin or the like, and the sealing member 31 has both the protection of the light emitting element 2 and the function of the lens 31a.
  • a transparent overcoat glass is usually applied as a protective layer to the exposed portions of the electrodes 3c and 3d and the pad electrodes 3a and 3b, but the description thereof is omitted here.
  • the electrodes (front electrodes) 3c and 3d are electrically connected to the electrodes (back electrodes) 3g and 3h formed on the other surface 1b via the electrodes (penetrating conductive layers) 3e and 3f penetrating the substrate 1. It is joined to.
  • the light emitting element 2 emits light by connecting an external DC power supply (not shown) or an AC-DC switching power supply (not shown) to the electrodes (back electrodes) 3g and 3h and applying a voltage.
  • an external DC power supply not shown
  • an AC-DC switching power supply not shown
  • many of the sealing members 31 have a function of not only protecting the light emitting element 2 but also selectively converting the wavelength of light, and further, light is transmitted by a lens 31a which is an outer shell of the sealing member 31. It is a diffusing and radiating structure.
  • FIG. 2 is a conceptual diagram showing a state in which incident light is scattered to the surface of the ceramic substrate for mounting a light emitting element of this embodiment.
  • Incident light 11 applied to the surface 1 a of the ceramic substrate 1 for mounting light emitting elements of the present embodiment is reflected by the surface 1 a of the substrate 1 and the inside of the substrate 1 to be irradiated with the incident light 11.
  • the transmitted light 12 emerges from the side opposite to the one surface 1a.
  • incident light 11 becomes a regular reflection light 13a that is partially reflected on the surface 1a in the opposite direction at the same angle as the incident angle, and a diffuse reflection light 13b that is reflected in an unspecified direction on the surface 1a.
  • the remainder proceeds inside the substrate 1.
  • the light traveling inside the substrate 1 is partially reflected at the interface 7 between the crystal particles 4 and the glass phase 5 in the substrate 1 as regular reflected light 13c and diffuse reflected light 13d.
  • the specular reflection light 13 e and the diffuse reflection light 13 f become, and the remaining light further travels inside the substrate 1, and the interface 7 between the crystal particles 4 and the glass phase 5;
  • regular reflection light 13e and diffuse reflection light 13f are produced and become reflected light from the surface 1a.
  • the light traveling in the substrate 1 comes out as transmitted light 12 from the opposite side.
  • the internal regular reflection light 13c, 13e and the diffuse reflection light 13d, 13f are increased so as to be reflected toward one surface 1a, or from the other surface 1b. It is necessary to reduce the transmitted light 12 that is transmitted through.
  • FIG. 3 is an electron micrograph showing crystal particles of the ceramic substrate for mounting a light emitting device of this embodiment.
  • the electron micrograph showing the crystal particles is taken with a scanning electron microscope after the surface of the substrate 1 is mirror-finished and fire-etched.
  • crystal grains 4 As shown in FIG. 3, on the surface of the substrate 1 of the present embodiment, crystal grains 4, a glass phase (grain boundary phase) 5, and pores 6 formed in the process of sintering ceramics are formed on the surface by processing. There are open pores 6a that appear or are formed by crystal grains shed during processing.
  • the light emitting element mounting ceramic substrate 1 of the present embodiment is made of a ceramic sintered body, and is a light emitting element mounting ceramic sintered body having a mounting portion on which the light emitting element is mounted.
  • the ratio of the number of crystals having an equivalent circle diameter of 0.2 ⁇ m to 1.0 ⁇ m is 45% to 80%, and the ratio of the number of crystals having a circle equivalent diameter of 2.0 ⁇ m to 6.0 ⁇ m is 5 It is important that the ratio of the number of crystals having an equivalent circle diameter exceeding 6.0 ⁇ m is 2.7% or less.
  • the mounting portion on which the light emitting element of the light emitting element mounting ceramic substrate 1 of the present embodiment is mounted is one surface of the substrate 1 on which the electrodes 3c and 3d for mounting the light emitting element are formed.
  • the surface layer portion refers to a portion of the surface layer from one surface 1a of the substrate 1 to about 50 ⁇ m in the thickness direction.
  • the substrate 1 of the present embodiment is a light-emitting element mounting ceramic sintered body having a mounting portion on which the light-emitting element of the substrate 1 is mounted, and the crystal grain size in the surface layer portion on the mounting portion side is 0.2 in terms of the equivalent circle diameter. Since the ratio of the number of crystals of ⁇ m or more and 1.0 ⁇ m or less is 45% or more and 80% or less, the interface 7 between the crystal particle 4 that reflects the incident light 11 and the glass phase 5 is formed as shown in FIG. As a result, the number of regular reflection light 13c and diffuse reflection light 13d increases, and it becomes easy to have a high reflectance. Further, scattering of phonons, which are vibrations of the crystal lattice that conducts heat, can be reduced at the interface 7 and the thermal conductivity can be maintained at a high level.
  • the substrate 1 of the present embodiment has a high reflectivity because the ratio of the number of crystals having a crystal grain size of an equivalent circle diameter of 2.0 ⁇ m or more and 6.0 ⁇ m or less is 5% or more and 15% or less. It becomes easy to maintain the thermal conductivity of 1 high.
  • the ratio of the number of crystals having an equivalent circle diameter of 2.0 ⁇ m or more and 6.0 ⁇ m or less is 5% or more and 15% or less.
  • the substrate 1 can suppress a short wavelength component in visible light from being absorbed or attenuated by the crystal particles. Therefore, a high reflectivity can be achieved for all wavelengths of visible light.
  • the interface 7 between the crystal particles 4 and the glass phase 5 is reduced as compared with a ceramic substrate for mounting a light emitting element made of crystals having a crystal grain size of 1.0 ⁇ m or less, the vibration of crystal particles conducting heat is present. The scattering of phonons is reduced, it is easy to maintain high thermal conductivity, and further, the problem that the reflectance of visible light is lowered due to the reduction of the interface 7 between the crystal particles 4 and the glass phase 5 is suppressed. It becomes easy.
  • a dividing groove for dividing the plate-like body into pieces is formed on the surface of the substrate 1.
  • burrs are less likely to be generated on the divided surface obtained by dividing the plate-like body along the dividing groove.
  • the substrate 1 contains 5% or more and 15% or less of crystals having a crystal grain diameter of 2.0 ⁇ m or more and 6.0 ⁇ m or less in an equivalent circle diameter, so that the destruction sources such as pores are appropriately dispersed in the substrate 1 and the divided grooves This is thought to be because the cracks generated from the cracks propagate linearly.
  • the three-point bending strength of the substrate 1 is in the range of 280 to 400 MPa, burrs are less likely to remain, and further, chipping hardly occurs at the end of the substrate 1 during the manufacturing process.
  • the ratio of the number of crystals whose crystal grain size, which is a large crystal grain that easily absorbs or attenuates a short wavelength, exceeds 6.0 ⁇ m in terms of the equivalent circle diameter is suppressed to 2.7% or less, so it is short in visible light. Since it can further suppress that the component of a wavelength is absorbed and attenuate
  • the crystal grain size is measured by mirror-finishing the surface of the substrate 1, performing fire etching at a temperature lower by 50 to 100 ° C than the firing temperature, and using a scanning electron microscope (for example, JSM-7001F manufactured by JEOL Ltd.) Take images at 1000 to 3000 times magnification to create image data, use an image analyzer (for example, Win ROOF manufactured by Mitani Corporation) to determine the area of each crystal grain, and use the area to calculate the equivalent circle diameter of each crystal Is calculated to obtain the distribution of the crystal grain size.
  • a scanning electron microscope for example, JSM-7001F manufactured by JEOL Ltd.
  • the substrate 1 may contain crystals having a crystal grain size of less than 0.2 ⁇ m.
  • the crystal grain size is less than 0.2 ⁇ m. Omitted because it cannot detect crystals.
  • the light reflectance of the substrate 1 of the present embodiment is measured using a spectrophotometer using an integrating sphere unit (for example, a spectrophotometer model UV-315 manufactured by Shimadzu Corporation) and an integrating sphere unit model name. ISR-3100), a 50W halogen lamp and deuterium lamp as the light source, a wavelength range of 200 to 1000 nm, a measurement range of diffuse reflectance (slit 20 nm, 7 x 9 mm), no mask used Thus, the measurement may be performed using barium sulfate powder as a reference.
  • an integrating sphere unit for example, a spectrophotometer model UV-315 manufactured by Shimadzu Corporation
  • ISR-3100 integrating sphere unit model name.
  • a 50W halogen lamp and deuterium lamp as the light source
  • a wavelength range of 200 to 1000 nm a measurement range of diffuse reflectance (slit 20 nm, 7 x 9 mm)
  • no mask used no mask used
  • the measurement may be
  • the thermal conductivity may be measured by processing the substrate 1 to a thickness of 2 mm and measuring by a laser flash method (for example, TC-7000 manufactured by Vacuum Riko).
  • a laser flash method for example, TC-7000 manufactured by Vacuum Riko.
  • the three-point bending strength may be measured according to JIS R 1601, but when the substrate 1 is a plate-like body, for example, the sample shape has a length of about 40 mm, a width of 25 mm, and a thickness.
  • a sintered body with a thickness of 0.5 to 0.8 mm is used.
  • the surface of the sintered body is a burnt surface, the span of the fulcrum is 30 mm, and a load is applied to the center of the span at a speed of 0.5 mm / min. What is necessary is just to perform intensity
  • the ceramic sintered body of the ceramic substrate for mounting the light emitting device of the present embodiment white ceramics mainly composed of aluminum oxide (Al 2 O 3 ), zirconium oxide (ZrO 2 ), or titanium oxide (TiO 2 ). It is preferable that High reflectance can be obtained by using these white ceramics. Among these, high thermal conductivity can be obtained by using aluminum oxide.
  • the main component means that the total amount of aluminum oxide, zirconium oxide or titanium oxide is 94% by mass or more in the proportion of the total mass of the ceramic sintered body.
  • the base 1 of the present embodiment contains 94% by mass or more of aluminum oxide.
  • the substrate 1 of the present embodiment contains 94% by mass or more of aluminum oxide is to maintain high reflectivity and not lower the thermal conductivity.
  • aluminum oxide is less than 94% by mass, the components that form a glass phase that is a sintering aid increase. Therefore, the incident light is easily transmitted to the back surface of the substrate 1 and the reflectance is easily lowered. Furthermore, since the glass phase has a low thermal conductivity, when the glass phase increases, the thermal conductivity of the substrate tends to decrease.
  • the ceramic substrate 1 for mounting a light emitting element of the present embodiment contains 94% by mass or more of aluminum oxide, silicon oxide excluding inevitable impurities added as a sintering aid, calcium oxide, and oxidation
  • the total content of at least one of magnesium is 6% by mass or less (not including 0) of the balance, and it can be fired at a temperature lower than the normal firing temperature, and the production cost can be reduced.
  • These compounds may also be included. For example, when a barium compound is added, this barium compound is present in the grain boundary phase 5, and the reflectance can be further improved.
  • the electrodes 3c and 3d for forming the electrodes 3c and 3d on the one surface 1a on which the light emitting element 2 of the substrate 1 is mounted.
  • the metal component contained in the paste diffuses from the surface 1a through the glass phase 5 to the inside, so that the adhesion strength between the electrodes 3c and 3d and the substrate 1 can be easily increased.
  • the regular reflection light 13 c and the diffuse reflection light 13 d increase at the interface 7 between the crystal particles 4 and the glass phase 5, and the reflectance is easily increased.
  • the regular reflection light 13c and the diffuse reflection light 13d increase at the interface 8 between the pores 6 and the glass phase 5, and the reflectance can be easily increased.
  • the light emitting element mounting ceramic substrate 1 of the present embodiment preferably has a maximum crystal grain size of 6.0 ⁇ m or less.
  • the maximum grain size of the crystal grain size is 6.0 ⁇ m or less
  • the light that travels inside the substrate 1 is reflected by the interface 7 between the crystal particles 4 and the glass phase 5, and the regularly reflected light 13 c Since the diffused reflection light 13d has many opportunities to be reflected, it is easy to be reflected as reflected light from the surface 1a of the substrate 1 through the glass phase 5, so that the reflectance is hardly lowered.
  • the ceramic substrate 1 for light emitting element mounting of this embodiment has an average crystal grain diameter of a circle equivalent diameter of 0.7 ⁇ m or more and 1.3 ⁇ m or less.
  • the base 1 of the present embodiment has a ratio of the number of crystals having a crystal grain size of 0.2 ⁇ m or more and 1.0 ⁇ m or less of 45% or more and 80% or less and a ratio of the number of crystals of 2.0 ⁇ m or more and 6.0 ⁇ m or less. If the ratio of the number of crystals exceeding 5% to 15% and exceeding 6.0 ⁇ m satisfies 2.7% or less, and the average crystal grain size is in the range of 0.7 ⁇ m to 1.3 ⁇ m, the visible light reflectivity and thermal conductivity will be further increased. It becomes easy to maintain a high effect of improving both the characteristics of the rate.
  • FIG. 4 is a conceptual diagram showing a state in which a part of diffuse reflection light is scattered between grain boundary phases in the ceramic substrate 1 for mounting a light emitting element of the present embodiment.
  • the grain boundary phase 5 made of crystal particles 4 and silicon oxide and the like, pores (not shown), and have.
  • the diffuse reflected light in the grain boundary phase between crystal grains will be described.
  • Incident light 11 irradiated on the surface of the ceramic substrate 1 for mounting a light emitting element of the present embodiment becomes light traveling inside the substrate 1, and an interface 7 a between the crystal grain 4 a and the grain boundary phase 5 inside the substrate 1.
  • the ceramic substrate 1 for light emitting element mounting of this embodiment is that the average width of the grain boundary phase formed between crystal grains is 2 nm or less.
  • the substrate 1 for mounting a light emitting element of the present embodiment, if the substrate 1 has an average width of the grain boundary phase 5 of 2 nm or less, for example, in the case of FIG. 4, the interface 7a between the adjacent crystal particles 4a and 4b When the grain boundary phase 5 exists between the interface 7b and light enters the grain boundary phase 5, the reflection of light repeatedly repeats between the interface 7a and the interface 7b, and the diffuse reflected light 13d increases. Reflectivity tends to be high. If the average width of the grain boundary phase 5 exceeds 2 nm, the width of the grain boundary phase 5 is widened. Therefore, the number of repeated light reflections between the interface 7a and the interface 7b is reduced, and the diffuse reflected light 13d is generated. Less increase in reflectance is likely to occur.
  • the method for obtaining the average width of the grain boundary phase 7 formed between the crystal grains is as follows.
  • FIG. 5 is a conceptual diagram showing the crystal grain 4a, 4b and the grain boundary phase 5 formed between the crystal grain 4a, 4b of the ceramic substrate 1 for mounting a light emitting element of the present embodiment.
  • the width of the grain boundary phase is measured in the range 9 of the grain boundary phase 5 formed by enlarging the cross section of the substrate 1 from 40,000 times to 60,000 times by TEM observation and formed between the crystal grains 4a and 4b. Then, the same measurement may be performed at 10 places, and the average thereof may be set as the average width of the grain boundary phase.
  • the light-emitting device of this embodiment is set as the structure which mounted the light emitting element on the ceramic base
  • a light emitting element When a light emitting element is mounted on the substrate 1 of this embodiment, when the light emitting element emits light, the light is efficiently reflected on the surface of the substrate 1, so that a light emitting device with low power can be obtained.
  • the heat conductivity is high, heat dissipation is good, and it is easy to suppress deterioration of the light-emitting element, the reflective material, and the resin covering the light-emitting element, and the life can be extended.
  • the ceramic sintered body contains aluminum oxide as a main component
  • 94% by mass or more of a powder having an average particle size of aluminum oxide (Al 2 O 3 ) of 1.8 ⁇ m as a raw material is used as a sintering aid.
  • silicon oxide (SiO 2 ) and at least one powder of calcium oxide (CaO) and magnesium oxide (MgO) are prepared within a total range of 6% by mass or less.
  • the average width of the grain boundary phase 5 formed between the crystal grains can be adjusted by adjusting the weighing of the sintering aid.
  • the ceramic sintered body is mainly composed of zirconium oxide, aluminum oxide is used as a sintering aid. If the ceramic sintered body is composed mainly of titanium oxide, silicon oxide and aluminum oxide are used as sintering aids. At least one of them may be selected and weighed so that the main component is 94% by mass or more and the balance is a sintering aid.
  • the aluminum oxide is 94% by mass and the sintering aid is 6% by mass
  • the aluminum oxide is divided into 60% by mass and 34% by mass using a rotating mill or bead mill together with a solvent such as water.
  • a solvent such as water.
  • Each is pulverized into a slurry using high-purity alumina balls.
  • the crystal grain size of the substrate 1 can be adjusted by grinding the aluminum oxide into two or more types and preparing and mixing slurries with different particle sizes.
  • a sheet is formed by a doctor blade method, or by using a granulated body prepared by using this slurry by using a spray dryer, a known powder press forming method or a roll compaction method is used to form ceramics.
  • a sheet is formed, and an unfired molded body is produced by processing using a mold or laser processing to obtain a product shape.
  • the molded body is a multi-piece molded body in consideration of mass productivity.
  • the obtained compact is then used in an air (oxidizing) atmosphere firing furnace (for example, a roller-type tunnel furnace, a batch-type atmosphere furnace, and a pusher-type tunnel furnace).
  • the ceramic substrate 1 for mounting the light-emitting element of the present embodiment is manufactured by adjusting and firing in the range of 1420 to 1650 ° C., 1350 to 1550 ° C. in the case of zirconium oxide, and 1200 to 1400 ° C. in the case of titanium oxide. Can do. Further, the maximum firing temperature may be appropriately adjusted according to the mass of the main component. Furthermore, the crystal grain size and the average width of the grain boundary phase 5 can also be adjusted by adjusting the firing time.
  • aluminum oxide is divided into 60% by mass and 34% by mass so that the aluminum oxide is 94% by mass and the sintering aid is 6% by mass. It was pulverized into a slurry using pure alumina balls.
  • the particle size measured by the laser diffraction scattering method manufactured by Nikkiso Co., Ltd., Microtrac 9320-X100
  • D50 about 1.0 to 1.3
  • 34% by mass of aluminum oxide is charged.
  • these slurries were added to a rotary mill together with a separately pulverized sintering aid and mixed, and then a molding binder such as an acrylic resin was added thereto and mixed to obtain a slurry.
  • a molding binder such as an acrylic resin
  • the amount of the molding binder added was about 4 to 8% by mass with respect to 100% by mass of the mixed powder.
  • a slurry obtained by mixing the mixed powder and the molding binder was spray-dried into powder granules, and a molded body was produced by a known powder press molding method.
  • the distribution of crystal grain size, reflectance and thermal conductivity are measured by the following method, and the distribution of crystal grain size of 0.2 to 1 ⁇ m, 2 to 6 ⁇ m. The relationship between reflectivity and thermal conductivity was evaluated.
  • the crystal grain size distribution is measured by mirror-finishing the surface of each sample to a depth of 30 ⁇ m from the surface, performing fire etching at a temperature 80 ° C. lower than the firing temperature of each sample, and using a scanning electron microscope to 3000 Image data was created by shooting at double magnification and digitized from the image data using an image analyzer. More specifically, JSM-7001F made by JEOL is used for the scanning electron microscope, and Win ROOF made by Mitani Corporation is used for the image analyzer, and analysis is performed for a range of 835 ⁇ m 2. I did it. Here, since the crystal diameter of the circle equivalent diameter of 0.2 ⁇ m or less is indistinguishable from noise, it was automatically deleted from the image data.
  • the reflectance is spectrophotometer model name: UV-315 manufactured by Shimadzu Corporation, integrating sphere unit model name ISR-3100, and a 50 W halogen lamp and deuterium lamp are used as the light source.
  • the range was 200 to 1000 nm, the measurement range was diffuse reflectance (7 ⁇ 9 mm at 20 nm slit), and measurement was performed using barium sulfate powder as a reference without using a mask.
  • the thermal conductivity was measured by processing the ceramic substrate for mounting a light emitting element into a sample having a diameter of 10 mm and a thickness of 2 mm using the same material as each sample No., and measuring by a laser flash method.
  • the measuring device used was a model name TC-7000 manufactured by Vacuum Riko, and conformed to JIS R 1611-1997.
  • the overall evaluation of each sample is that the reflectance at a wavelength of 400 nm and a wavelength of 600 nm is 86% or more or 90% or more, respectively, and the thermal conductivity is 17 W / (m ⁇ K) or more. “Excellent” is displayed as A, “Satisfied” is displayed as “Good” as B, and “Satisfied” is displayed as “C”.
  • the reflectance of the sample No. For 3-6, 9-12, the ratio of the number of crystals whose crystal grain size is 0.2 to 1 ⁇ m in equivalent circle diameter is 45% to less than 80%, and the crystal grain size is 2.0 to 6.0 ⁇ m in equivalent circle diameter
  • the evaluation is A because the ratio of the number of crystals is 5% or more and 15% or less.
  • the interface 7 between the crystal particle 4 and the glass phase in which the incident light 12 is reflected in the substrate 1 is increased, and the short wavelength component in the visible light is prevented from being absorbed or attenuated by the crystal particle. Therefore, it can be seen that the reflectivity tends to be high at 86% or more at 400 nm and 90% or more at 600 nm.
  • Example 2 In the same manner as in Example 1, a ceramic substrate 1 for mounting a light emitting element was produced. At this time, the slurry was prepared by adjusting the particle size of the slurry and the firing temperature so that crystals having a crystal grain size equivalent to an equivalent circle diameter of 6 ⁇ m or more were included. Samples of 14 to 20 ceramic substrates for mounting light emitting elements were obtained.
  • the reflectance measurement method was the same as in Example 1, and “A” was defined as “excellent” when the reflectance at wavelengths of 400 nm and 600 nm was 86% or more or 90% or more, respectively.
  • the results are shown in Table 2 as “good” for items satisfying the items and B for “good” for those not satisfying both.
  • the sample No. In No. 14 the ratio of the number of crystals whose crystal grain diameter is equivalent to a circle and exceeding 6 ⁇ m exceeds 2.7%. Therefore, the light incident on the ceramic substrate for mounting the light emitting element is transmitted through the crystal and is reflected on the back surface.
  • the reflectivity at a wavelength of 600 nm was a value that slightly fell below 90%, and the reflectivity at a wavelength of 400 nm was less than 86%.
  • Sample No. Nos. 15 to 18 include a crystal grain size ratio of 1% to 2.7% of the number of crystals with an equivalent circle diameter of more than 6 ⁇ m, so that light incident on the ceramic substrate for mounting a light emitting element enters the crystal.
  • the transmittance was slightly apt to pass through to the back surface, and the reflectance at a wavelength of 600 nm slightly exceeded 90%, whereas the reflectance at a wavelength of 400 nm was less than 86%.
  • the reflected light is enhanced and the reflectivity at a wavelength of 600 nm is as high as 91% or more, and since there are few large crystal particles that absorb or attenuate short wavelengths, the reflectivity at a wavelength of 400 nm is as high as 88.1% or more. It turns out that it became easy to maintain in a state.
  • Example 2 In the same manner as in Example 1, a ceramic substrate for mounting a light emitting element was produced. At this time, the base 1 was prepared by adjusting the particle size of the slurry and the firing temperature so that the crystal grain size would be the equivalent circle diameter shown in Table 3. 21 to 27 light emitting element mounting ceramic substrate samples were obtained.
  • the sample No. Nos. 22 to 27 have an average crystal grain size of 1.3 ⁇ m or less, so that there are sufficient grain boundaries 7 to reflect the incident light in the ceramic substrate for mounting a light emitting element, and further, there are a glass phase 5 that scatters phonons, and The interface 7 between the layers is reduced, the reflectance at a wavelength of 600 nm is 91% or more, and the thermal conductivity is as high as 17 W / (m ⁇ K) or more, so that both characteristics can be satisfied. I understand.
  • Example 2 the influence of the grain boundary phase 5 formed between crystal grains on the reflectance was evaluated.
  • a ceramic substrate 1 for mounting a light emitting element was produced.
  • the base 1 was prepared by adjusting the amount of sintering aid and the firing temperature so that the grain boundary phase 5 had the values shown in Table 4. Samples of ceramic substrate 1 for mounting light emitting elements 28 to 31 were obtained.
  • the reflectance measurement method is the same as in Example 1, and the average width of the grain boundary phase is measured by magnifying an arbitrary cross section of the substrate 1 by TEM observation up to 50,000 times, Measure the width of the field phase. This work was obtained by measuring and averaging the width of the grain boundary phase in a total of 10 visual fields. The overall evaluation of each sample was the same as in Example 2.
  • the ceramic substrate 1 for mounting a light-emitting element of the embodiment is a ceramic substrate 1 suitable for mounting a light-emitting element that has a high reflectance and can maintain a high thermal conductivity.
  • the light-emitting device 21 in which the light-emitting element 2 is mounted on the ceramic substrate 1 for mounting the light-emitting element can efficiently reflect the light emitted from the light-emitting element 2 and has excellent heat dissipation due to high thermal conductivity. Deterioration of the light emitting element due to heat can be easily reduced.

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Abstract

　【課題】　高反射率が得られるとともに、放熱性を良くし発光素子の寿命を延ばすために熱伝導率の高い発光素子搭載用のセラミックス基体を提供する。　【解決手段】　セラミック焼結体からなり、発光素子が搭載される搭載部を有する発光素子搭載用セラミック焼結体であって、この搭載部側の表層部における結晶粒径が円相当径で０．２μｍ以上１．０μｍ以下の結晶の割合が４５％以上８０％以下であり、円相当径で２．０μｍ以上６．０μｍ以下の結晶の割合が５％以上１５％以下であるとともに、円相当径で６．０μｍを超える結晶の割合が２．７％以下であることから、発光素子搭載用セラミックス基体１の反射率を向上させることができるとともに、熱伝導率の高い発光素子搭載用セラミックス基体とすることができる。

Description

発光素子搭載用セラミックス基体および発光装置
　本発明は、発光素子搭載用セラミックス基体およびこの発光素子搭載用セラミックス基体に発光素子を搭載してなる発光装置に関する。
　近年、大量生産が可能な高輝度で消費電力の少ない発光素子としてＬＥＤ（発光ダイオード）が注目されている。そして、一般照明用から電光表示板用の光源、携帯電話機，パソコンおよびテレビ等のバックライトとしても広く利用されつつある。
　このような発光素子を搭載するための基体には、基体自体が高反射率を有し、放熱性を良くすることが求められている。
　このような要求に対し、特許文献１には、半導体発光素子用の高反射白色セラミックス基板が、酸化アルミニウムとガラス質成分とからなり気孔率が５％であること、酸化アルミウムの含有率が75～85重量％で、ガラス質成分としてシリカ，カルシウム，マグネシウムおよびバリウムを含有し、酸化アルミニウムの平均結晶粒径が0.5μｍ以下であることから、波長が400～740ｎｍにおける光の反射率を90～93％以上としたことが開示されている。
特開2007－284333号公報
　しかしながら、特許文献１に開示された半導体発光素子用の高反射白色セラミックスは、実施例によると、アルミナが75～85重量％に、ガラス質成分としてシリカと、バリウム，カルシウムおよびマグネシウムの酸化物を約25～15重量％含有した焼結体であって、波長が400～740ｎｍの反射率が90％以上のものが得られるものの、アルミナの結晶粒径が0.5μｍ以下であることから、熱伝導率が低くなり、発光素子を冷却する作用が低下することで、発光素子の寿命が短くなるという問題があった。
　本発明は、上記課題を解決するために案出されたものであり、高反射率が得られるとともに、放熱性を良くし発光素子の寿命を延ばすことができる熱伝導率の高い発光素子搭載用セラミックス基体を提供することを目的とするものである。
　本発明の発光素子搭載用セラミックス基体は、セラミック焼結体からなり、発光素子が搭載される搭載部を有する発光素子搭載用セラミック焼結体であって、前記搭載部側の表層部における結晶粒径が円相当径で0.2μｍ以上1.0μｍ以下の結晶の割合が45％以上80％以下であり、円相当径で2.0μｍ以上6.0μｍ以下の結晶の割合が５％以上15％以下であるとともに、円相当径で6.0μｍを超える結晶の割合が2.7％以下であることを特徴とするものである。
　また、本発明の発光装置は、上記構成の発光素子搭載用セラミックス基体を搭載したことを特徴とする。
　本発明の発光素子搭載用セラミックス基体は、セラミック焼結体からなり発光素子が搭載される搭載部を有する発光素子搭載用セラミック焼結体であって、前記搭載部側の表層部における結晶粒径が円相当径で0.2μｍ以上1.0μｍ以下の結晶の割合が45％以上80％以下であり、円相当径で2.0μｍ以上6.0μｍ以下の結晶の割合が５％以上15％以下であるとともに、円相当径で6.0μｍを超える結晶の割合が2.7％以下であることから、高反射率を有し、熱伝導率を高い状態に維持しやすくなる。
　また、上記構成の発光素子搭載用セラミックス基体上に発光素子を搭載した発光装置とすることにより、高反射率を有するとともに、発光素子の放熱性を高めることができることから、寿命を長くすることができる。
本実施形態の発光素子搭載用セラミックス基体に発光素子を搭載した発光装置の構成の一例を示す断面図である。 本実施形態の発光素子搭載用セラミックス基体の表面への入射光が散乱する状態を示す概念図である。 本実施形態の発光素子搭載用セラミックス基体の結晶粒子を示す電子顕微鏡写真である。 本実施形態の発光素子搭載用セラミックス基体において、粒界相で拡散反射光が散乱する状態を示す概念図である。 本実施形態の発光素子搭載用セラミックス基体において、結晶粒子および結晶粒子間に形成される粒界相を示す概念図である。
　以下、本発明の発光素子搭載用セラミックス基体の実施の形態の例を説明する。
　図１は本実施形態の発光素子搭載用セラミックス基体に発光素子を搭載した発光装置の構成の一例を示す断面図である。
　本実施形態の発光素子搭載用セラミックス基体１（以下、基体１ともいう。）を用いた発光装置21は、発光素子２が搭載される基体１の一方の表面１aに厚膜印刷法等を用いて、電極（表電極）３ｃ，３ｄを被着させ、電極３ｃ，３ｄが形成された一部に、電極パッド３ａ，３ｂをメッキ等により形成し、この電極パッド３ａの上に半導体からなる発光素子２を搭載している。そして、発光素子２と電極パッド３ｂとをボンディングワイヤ32により電気的に接合している。なお、ここでは、電極パッド３ａと発光素子２との接合については、電気的に接合できるものであれば、導電性接着剤を用いた接合，ボンディングワイヤ32による接合または半田バンプによる接合であっても何ら構わない。そして、発光素子２および電極パッド３ａ，３ｂを含む電極３ｃ，３ｄを樹脂等からなる封止部材31で被覆し、この封止部材31が発光素子２の保護とレンズ31ａの機能を併せ持っている。なお、電極３ｃ，３ｄおよびパッド電極３ａ，３ｂの露出部分には通常、透明のオーバーコートガラスを保護層として被着するが、ここでは説明を省略する。
　また、電極（表電極）３ｃ、３ｄは、基体１を貫通した電極（貫通導電層）３ｅ，３ｆを経由して、他方の表面１ｂに形成された電極（裏電極）３ｇ，３ｈと電気的に接合されている。
　そして、この電極（裏電極）３ｇ，３ｈに外部の直流電源（不図示）またはＡＣ－ＤＣスイッチング電源（不図示）を接続して電圧を印加することにより発光素子２が発光する。このとき、封止部材31は、発光素子２の保護のみならず光の波長を選択的に変換する機能を持たせたものも多く、さらに封止部材31の外殻であるレンズ31ａにより光を拡散および放射する構造である。
　また、図２は本実施形態の発光素子搭載用セラミックス基体の表面への入射光が散乱する状態を示す概念図である。
　図２に示すように、本実施形態の発光素子搭載用セラミックス基体１は断面を結晶のサイズのレベルで見たとき、結晶粒子４と，酸化珪素等からなるガラス相（粒界相）５と，気孔６とを有している。なお、これらの結晶粒子４とガラス相５との間を界面７とし、気孔６とガラス相５との間を界面８としてある。
　本実施形態の発光素子搭載用セラミックス基体１の表面１ａに照射された入射光11は、基体１の表面１ａによって反射する反射光13と、基体１の内部を透過して、入射光11が照射された一方の表面１ａとは反対側から出てくる透過光12となる。
　また、入射光11は、その一部が表面１ａで入射角度に対し同じ角度で逆方向に反射される正反射光13ａと、表面１ａで不特定な方向へ反射される拡散反射光13ｂとなるが、残りは基体１の内部を進行する。そして、この基体１の内部を進行する光は、基体１内で結晶粒子４とガラス相５との間の界面７で一部は正反射光13ｃと拡散反射光13ｄとなり、また、気孔６とガラス相５との界面８で正反射光13ｅと拡散反射光13ｆとなり、残りの光は、さらに基体１の内部を進行していき、結晶粒子４とガラス相５との間の界面７と、気孔６とガラス相５との界面８とで正反射光13ｅと拡散反射光13ｆを生み出し表面１ａからの反射光となる。そして、基体１の内部を進行した光は、反対側から透過光12として出てくる。この基体１の光の反射率を大きくするには、内部の正反射光13ｃ，13ｅおよび拡散反射光13ｄ，13ｆを増やして一方の表面１ａ側に反射するようにするか、他方の表面１ｂから透過して出てくる透過光12を少なくすることが必要である。
　なお、表面１ａ，１ｂには、開気孔６ａも存在しているが、表面積における開気孔６ａの面積の占める割合は僅かであるため反射光13への影響の説明は割愛する。
　また、図３は本実施形態の発光素子搭載用セラミックス基体の結晶粒子を示す電子顕微鏡写真である。
　この結晶粒子を示す電子顕微鏡写真は、基体１の表面を鏡面加工し、ファイヤーエッチングを行なった後に走査型電子顕微鏡で撮影したものである。
　図３に示すように、本実施形態の基体１の表面には、結晶粒子４，ガラス相（粒界相）５、および、セラミックスが焼結する過程において形成された気孔６が加工により表面に現れたり、加工時に結晶粒が脱粒したりして形成された開気孔６ａが存在する。
　そして、本実施形態の発光素子搭載用セラミックス基体１は、セラミック焼結体からなり、発光素子が搭載される搭載部を有する発光素子搭載用セラミック焼結体であって、この搭載部側の表層部における結晶粒径が円相当径で0.2μｍ以上1.0μｍ以下の結晶の数の割合が45％以上80％以下であり、円相当径で2.0μｍ以上6.0μｍ以下の結晶の数の割合が5％以上15％以下であるとともに、円相当径で6.0μｍを超える結晶の数の割合が2.7％以下であることが重要である。
　ここで、本実施形態の発光素子搭載用セラミックス基体１の発光素子が搭載される搭載部とは、発光素子を搭載するための電極３ｃ，３ｄが形成される面である基体１の一方の表面１ａを言い、表層部とは、基体１の一方の表面１ａから厚み方向に50μｍ程度までの表層の部分のことを言う。
　本実施形態の基体１は、基体１の発光素子が搭載される搭載部を有する発光素子搭載用セラミック焼結体であって、この搭載部側の表層部における結晶粒径が円相当径で0.2μｍ以上1.0μｍ以下の結晶の数の割合が45％以上80％以下であることから、図２で示すように、入射光11を反射する結晶粒子４とガラス相５との間の界面７が増えて正反射光13ｃと拡散反射光13ｄとが増加し、高反射率を有することが容易となる。また、熱を伝導する結晶格子の振動であるフォノンが界面７で散乱するのを低減し熱伝導率を高い状態で維持できる。
　また、本実施形態の基体１は、結晶粒径が円相当径で2.0μｍ以上6.0μｍ以下の結晶の数の割合が５％以上15％以下であることから、高反射率を有するとともに、基体１の熱伝導率を高く維持することが容易となる。また、結晶粒径が大きくなると短い波長を吸収もしくは減衰し易くなることから、この結晶粒径が円相当径で2.0μｍ以上6.0μｍ以下の結晶の数の割合が５％以上15％以下である基体１は、可視光における短い波長の成分が結晶粒子に吸収もしくは減衰されることを抑えることができる。それゆえ、可視光の全波長に対し、高反射率を有する状態にできる。
　さらに、結晶粒径が1.0μｍ以下の結晶からなる発光素子搭載用セラミックス基体と比較して結晶粒子４とガラス相５との間の界面７が少なくなるため熱を伝導する結晶粒子の振動であるフォノンの散乱が低減し、熱伝導率を高く維持することが容易となり、さらに、結晶粒子４とガラス相５との間の界面７の減少により可視光の反射率が低下するという問題を抑制しやすくなる。
　さらに、結晶粒径が円相当径で2.0μｍ以上6.0μｍ以下の結晶の数の割合が５％以上15％以下であると、基体１の表面に板状体を個片に分割する分割溝が形成された板状体としたとき、分割溝に沿って板状体を分割した分割面にバリが発生しにくくなる。これは、基体１が、結晶粒径が円相当径で2.0μｍ以上6.0μｍ以下の結晶を５％以上15％以下含むことにより、気孔などの破壊源が基体１に適度に分散し、分割溝から発生する亀裂が直線的に進展するためと考えられる。特に基体１の３点曲げ強度が280～400ＭＰａの範囲であれば、バリが残りにくく、さらに、製造工程の途中で基体１の端部に欠けも発生しにくい。
　さらにまた、短い波長を吸収もしくは減衰しやすい大きい結晶粒子である結晶粒径が円相当径で6.0μｍを超える結晶の数の割合が、2.7％以下と少なく抑えていることから、可視光における短い波長の成分が結晶粒子に吸収および減衰されることをさらに抑えることができるので、高反射率を有する状態にできる。
　この様な結晶粒径の測定は、基体１の表面を鏡面加工し、焼成温度から50～100℃低い温度の範囲でファイヤーエッチングをし、走査型電子顕微鏡（例えば日本電子製のJSM-7001F）で1000～3000倍の倍率で撮影して画像のデータを作成し、画像解析装置（例えば三谷商事製のWin ROOF）を用いて各結晶粒の面積を求め、その面積から各結晶の円相当径を算出して結晶粒径の分布を求めればよい。
　但し、本実施形態においては、基体１に結晶粒径が0.2μｍ未満の結晶が含まれている場合もあるが、本実施形態に用いた結晶粒径の測定方法では結晶粒径が0.2μｍ未満の結晶を検知できないため割愛している。
　また、本実施形態の基体１の光の反射率の測定は、積分球ユニットを使用した分光光度計（例えば（株）島津製作所製の分光光度計 型名ＵＶ－315）と積分球ユニット 型名ＩＳＲ－3100と）を用い、光源に50Ｗハロゲンランプと重水素ランプとを使用し、波長範囲を200～1000ｎｍとし、測定範囲は拡散反射率（スリット20ｎｍ時７×９ｍｍ）として、マスクの使用はなしで、基準に硫酸バリウム粉体を用いて測定すればよい。
　さらに、熱伝導率の測定は、基体１を２ｍｍの厚みに加工し、レーザフラッシュ法（例えば真空理工製のTC-7000）で測定すればよい。
　さらにまた、３点曲げ強度の測定は、ＪＩＳ Ｒ 1601に準拠して測定すればよいが、基体１が板状体の場合は、例えば、試料形状を長さが約40ｍｍ、幅が25ｍｍ、厚みが0.5～0.8ｍｍの焼結体を用い、焼結体の表面は焼き肌面とし、支点のスパンは30ｍｍとし、スパンの中央部に0.5ｍｍ／分の速度で荷重を印加し、３点曲げ強度の計算式により強度計算を行なえばよい。
　また、本実施形態の発光素子搭載用セラミックス基体のセラミック焼結体としては、酸化アルミニウム（Ａｌ２Ｏ３），酸化ジルコニウム（ＺｒＯ２）または酸化チタン（ＴｉＯ２）を主成分とする白色のセラミックスであることが好ましい。これらの白色のセラミックスを用いることで、高反射率を得ることができる。中でも、酸化アルミニウムを用いれば高い熱伝導率を得ることができる。ここで、主成分とは、酸化アルミニウム，酸化ジルコニウムまたは酸化チタンが、セラミック焼結体の全体の質量の割合において、合計量が94質量％以上のことである。
　そして、本実施形体の基体１が酸化アルミニウムを94質量％以上含有していることが好ましい。
　本実施形態の基体１が酸化アルミニウムを94質量％以上含有するのは、高反射率を保ち、熱伝導率を低下させないためである。酸化アルミニウムが94質量％未満になると、焼結助剤であるガラス相を形成する成分が増加する。それゆえ、入射光が基体１の裏面に透過しやすくなって反射率が低下しやすくなる。さらに、ガラス相は熱伝導率が低いため、ガラス相が増加すると基体の熱伝導率が低下しやすくなる。
　また、本実施形態の発光素子搭載用セラミックス基体１は、酸化アルミニウムの含有量が94質量％以上を含有することから、焼結助剤として添加する不可避不純物を除く酸化珪素と、酸化カルシウムおよび酸化マグネシウムの少なくとも１種との合計の含有量が残部の６質量％以下（０を含まず）となり、通常の焼成温度よりも低温で焼成することができ、製造コストを抑えることができるが、その他の化合物を含んでも良い。例えば、バリウム化合物を加えると、このバリウム化合物が粒界相５に存在し、反射率をより向上することが可能である。
　また、結晶粒子４同士の間には酸化珪素等からなるガラス相５が形成されているために、基体１の発光素子２を搭載する一方の表面１ａに、電極３ｃ，３ｄを形成するための厚膜ペーストを塗布して厚膜焼成するとペーストに含まれる金属成分が表面１ａからガラス相５を伝わって内部に拡散するために、電極３ｃ，３ｄと基体１の密着強度を高くしやすくなる。
　また、入射光11を効率よく反射するために結晶粒子４とガラス相５との間の界面７とで正反射光13ｃと拡散反射光13ｄとが増加し、反射率を高くしやすくなるが、気孔６とガラス相５との間の界面８でも同じように正反射光13ｃと拡散反射光13ｄとが増加し、反射率を高くしやすくできる。
　そして、本実施形態の発光素子搭載用セラミックス基体１は、結晶粒径の最大粒径が6.0μｍ以下であることが好ましい。
　結晶粒径の最大粒径が6.0μｍ以下であると、基体１を形成したとき、基体１の内部を進行する光が結晶粒子４とガラス相５との界面７で反射した正反射光13ｃおよび拡散反射光13ｄが反射する機会が多くなることから、ガラス相５を通り、基体１の表面１ａから反射光とし出ていきやすくなるために反射率は低下しにくくなる。
　そして、本実施形態の発光素子搭載用セラミックス基体１は、平均結晶粒径が円相当径で、0.7μｍ以上1.3μｍ以下であることが好ましい。
　本実施形態の、基体１が、上記説明したように結晶粒径が0.2μｍ以上1.0μｍ以下の結晶の数の割合が45％以上80％以下、2.0μｍ以上6.0μｍ以下の結晶の数の割合が5％以上15％以下、6.0μｍを超える結晶の数の割合が2.7％以下を満たし、平均結晶粒径が0.7μｍ以上1.3μｍ以下の範囲にあると、さらに可視光の反射率と熱伝導率との双方の特性を高める作用を高く維持することが容易となる。
　図４は、本実施形態の発光素子搭載用セラミックス基体１において、粒界相間で拡散反射光の一部が散乱する状態を示す概念図である。
　図４に示すように、本実施形態の発光素子搭載用セラミックス基体１は断面を結晶サイズレベルで見たとき、結晶粒子４と酸化珪素等からなる粒界相５と、気孔（不図示）とを有している。（図２で入射光11が散乱する状態を説明したため以下では、結晶粒子間の粒界相における拡散反射光について説明する。）
　本実施形態の発光素子搭載用セラミックス基体１の表面に照射された入射光11は、基板１の内部を進行する光となり、基体１内部で結晶粒子４ａと粒界相５との間の界面７ａの内部をさらに進行していき隣接する結晶粒子４ｂと粒界相５との間の界面７ｂに進行していくが、この光の進行の過程で、一部の光が入射角度に対して同じ角度で逆方向に反射される正反射光13ｃと拡散反射光13ｄとが生じる。この拡散反射光13ｄは、界面７ａと界面７ｂとの間の粒界相５で反射を繰り返し基板１の一方の表面（不図示）から拡散反射光13ｅが出るようになっている。
　そして、本実施形態の発光素子搭載用セラミックス基体１は、結晶粒子間に形成される粒界相の平均幅が２ｎｍ以下であることが好ましい。
　本実施形態の発光素子搭載用セラミックス基体１において、基体１が、粒界相５の平均幅が２ｎｍ以下であるならば、例えば図４の場合では、隣り合う結晶粒子４ａ，４ｂの界面７ａと界面７ｂとの間に粒界相５が存在することによって、その粒界相５に光が入った場合、界面７ａと界面７ｂとの間で光の反射を繰り返し拡散反射光13ｄが増加し、反射率が高くなりやくなる。粒界相５の平均幅が２ｎｍを超えるならば、粒界相５の幅が広くなることから、界面７ａと界面７ｂとの間で光の反射が繰り返す回数が減少して拡散反射光13ｄが少なく反射率の増加が少なくなり易い。
　ここで、結晶粒子間に形成される粒界相７の平均幅を求める手法は下記の通りである。
　図５は本実施形態の発光素子搭載用セラミックス基体１の結晶粒子４ａ，４ｂおよび結晶粒子４ａ，４ｂ間に形成される粒界相５を示す概念図である。
　先ず、基体１の断面をＴＥＭ観察により、40,000倍から60,000倍まで拡大し結晶粒子４ａ，４ｂ間に形成される粒界相５の範囲９内において、粒界相の幅を測定する。そして、同様の測定を10ヶ所実施してその平均を粒界相の平均幅とすればよい。
　そして、本実施形態の発光装置は、発光素子搭載用セラミックス基体上に発光素子を搭載した構成とされる。
　本実施形態の、基体１上に発光素子を搭載すると、発光素子が発光したとき、光が基体１の表面で効率よく反射するため低電力で明るい発光装置とすることができる。また、熱伝導率が高いため放熱性がよく発光素子や反射材や発光素子を覆う樹脂などの劣化を抑制することが容易となり寿命を長くすることができる。
　次に、本実施形態の発光素子搭載用セラミックス基体の製造方法の一例を説明する。
　例えば、セラミック焼結体が、酸化アルミニウムを主成分とする場合には、原料として、酸化アルミニウム（Ａｌ２Ｏ３）の平均粒径が1.8μｍの粉末を94質量％以上と、焼結助剤として酸化珪素（ＳｉＯ２）と、酸化カルシウム（ＣａＯ）および酸化マグネシウム（ＭｇＯ）の少なくとも１種の粉末とを合計６質量％以下の範囲で準備する。そして、酸化アルミニウムと焼結助剤の合計が100質量％となるように秤量する。ここで、焼結助剤の秤量を調整することによって、結晶粒子間に形成される粒界相５の平均幅を調整することができる。
　ここで、セラミック焼結体が、酸化ジルコニウムを主成分とするならば、焼結助剤として酸化アルミニウムを、また、酸化チタンを主成分とするならば、焼結助剤として酸化珪素および酸化アルミニウムのうち少なくとも１種を選択し、主成分を94質量％以上、残部が焼結助剤となるように秤量すれば良い。
　次に、例えば、酸化アルミニウムを94質量％、焼結助剤を６質量％とした場合、酸化アルミニウムを60質量％と34質量％に分け、水等の溶媒とともに回転ミルやビーズミル等を用いてそれぞれ別に高純度のアルミナボールを用いて粉砕しスラリーにする。そして、酸化アルミニウムを55質量％投入した回転ミルではレーザ回折散乱法（例えば、日機装（株）製 Ｍｉｃｒｏｔｒａｃ 9320-X100）で測定した粒度がＤ５０＝1.2程度となるようにし、酸化アルミニウムを41質量％投入した回転ミルでは上記と同様のレーザ回折散乱法で測定した粒度がＤ５０＝1.6程度となるようにする。
　次に、これらのスラリーを別途粉砕した焼結助剤と共に回転ミル等に投入し、数時間をかけてさらに混合する。この様に酸化アルミニウムを２種類以上に分けて粉砕し、異なる粒度のスラリーを作製し混合することで、基体１の結晶粒径を調整することができる。
　次に、このスラリーを用いて、ドクターブレード法でシートを成形するか、このスラリーをスプレードライヤを用いて作製した造粒体を使用して公知の粉末プレス成形法、またはロールコンパクション法によってセラミックスのシートを成形し、製品形状とするための金型による加工もしくはレーザ加工によって未焼成の成形体を作製する。このとき成形体は、量産性を考慮すれば多数個取りの成形体とするのがより好ましい。そして、得られた成形体を、大気（酸化）雰囲気の焼成炉（例えば、ローラー式トンネル炉，バッチ式雰囲気炉およびプッシャー式トンネル炉）を用いて、最高温度は主成分が酸化アルミニウムの場合は1420～1650℃、酸化ジルコニウムの場合は1350～1550℃、酸化チタンの場合は1200～1400℃の範囲で調整して焼成することによって、本実施形態の発光素子搭載用セラミックス基体１を作製することができる。また、焼成の最高温度は主成分の質量によって適宜調整すればよい。さらに、焼成時間を調整することによっても結晶粒径および粒界相５の平均幅を調整することもできる。
　以下、本発明の実施例を具体的に説明するが、本発明では以下の実施例に限定されるものではない。
　まず、酸化アルミニウム（Ａｌ２Ｏ３）の平均粒径が1.8μｍの粉末を94質量％と、焼結助剤として酸化珪素（ＳｉＯ２）を3.5質量％と、酸化カルシウム（ＣａＯ）を1.5質量％および酸化マグネシウム（ＭｇＯ）を1.0質量％の粉末とを準備した。そして、酸化アルミニウムと焼結助剤の合計が100質量％となるように秤量した。
　次に、酸化アルミニウムを94質量％、焼結助剤を６質量％となる様に、酸化アルミニウムを60質量％と34質量％とに分け、それぞれ別々に溶媒の水とともに回転ミルを用いて高純度のアルミナボールを用いて粉砕しスラリーにした。そして、酸化アルミニウムを60質量％投入した回転ミルではレーザ回折散乱法（日機装（株）製 Ｍｉｃｒｏｔｒａｃ9320-X100）で測定した粒度がＤ５０＝1.0～1.3程度となるようにし、酸化アルミニウムを34質量％投入した回転ミルでは上記と同様のレーザ回折散乱法で測定した粒度がＤ５０＝1.4～1.8程度となるようにした。
　次に、これらのスラリーを別途粉砕した焼結助剤と共に回転ミルに投入し混合してからさらに、これにアクリル樹脂等の成形用バインダーを添加し、混合してスラリーを得た。
ここで、成形用バインダーの添加量は混合粉末100質量％に対して４～８質量％程度とした。
　次に、この混合粉末と成形用バインダーとを混合したスラリーをスプレードライで粉末の顆粒とし、公知の粉末プレス成形法で成形体を作製した。
　次に、この成形体を焼結させるために、電気炉を用いて1420～1650℃の範囲で焼成を行ない、厚みが0.63±0.05ｍｍである表１に示す様な結晶粒径の分布と平均結晶粒径である試料Ｎｏ．１～13の発光素子搭載用セラミックス基体の試料を得た。
　この得られた発光素子搭載用セラミックス基体の試料について、結晶粒径の分布，反射率および熱伝導率の測定を以下の方法で行ない、0.2以上１μｍ以下，２μｍ以上６μｍ以下の結晶粒径の分布と反射率、熱伝導率の関係を評価した。
　結晶粒径の分布の測定は、各試料の表面を表面から30μｍの深さまで鏡面加工し、加工した面を各試料の焼成温度から80℃低い温度でファイヤーエッチングを行ない、走査型電子顕微鏡で3000倍の倍率で撮影して画像データを作成し、その画像データから画像解析装置を用いて数値化した。具体的には、走査型電子顕微鏡には日本電子製の型名JSM-7001Fを使用し、画像解析装置には三谷商事製の型名Win ROOFを使用し、835μｍ２の範囲に対して解析を行なった。ここで、円相当径0.2μｍ以下の結晶粒径のものはノイズと区別がつかないため画像データから自動削除した。
　次に、反射率は（株）島津製作所製の分光光度計 型名：ＵＶ－315と積分球ユニット 型名ＩＳＲ－3100とを用い、光源に50Ｗハロゲンランプと重水素ランプとを使用し、波長範囲を200～1000ｎｍとし、測定範囲は拡散反射率（スリット20ｎｍ時７×９ｍｍ）として、マスクの使用はなしで、基準に硫酸バリウム粉体を用いて測定した。
　次に、熱伝導率の測定は、各試料Ｎｏと同一の材料を用いて発光素子搭載用セラミックス基体を直径が10ｍｍで厚みが２ｍｍの試料に加工し、レーザフラッシュ法で測定した。具体的には、測定装置は真空理工製の型名TC-7000を使用し、ＪＩＳ Ｒ 1611-1997に準拠した。
　また、各試料の総合評価は、波長400ｎｍおよび波長600ｎｍでの反射率が、各々86％以上または90％以上であって、かつ、熱伝導率が17Ｗ／（ｍ・Ｋ）以上であるものを『優』としＡとして表示し、いずれか２つの項目を満足するものを『良』としＢとして表示し、いずれか１つの項目を満足するものを『可』としＣとして表示した。
　得られた結果を表１に示す。
Figure JPOXMLDOC01-appb-T000001
　表１に示す結果から分かるように、まず反射率について、試料Ｎｏ．３～６，９～12は、結晶粒径が円相当径で0.2μｍ以上１μｍ以下の結晶の数の割合が45％以上80％未満および結晶粒径が円相当径で2.0μｍ以上6.0μｍ以下の結晶の数の割合が５％以上15％以下であることから評価はＡであり、試料Ｎｏ．１，２および13に比べ基体１内に入射光12が反射する結晶粒子４とガラス相との界面７が増えるとともに、可視光における短い波長の成分が結晶粒子に吸収もしくは減衰されることを抑えることができるので、反射率が400ｎｍで86％以上、600ｎｍで90％以上と反射率が高くなる傾向にあることが分かる。
　次に、熱伝導率について、試料Ｎｏ．３～６，９～12は、結晶粒径が円相当径で0.2μｍ以上１μｍ以下の結晶の数の割合が45％以上80％未満および結晶粒径が円相当径で2.0μｍ以上6.0μｍ以下の結晶の数の割合が５％以上15％以下であることから評価はＡであり、試料Ｎｏ．７および８に比べ、フォノンを散乱するガラス相５との間の界面７が減少し、熱伝導率が17Ｗ／（ｍ・Ｋ）以上と高くなる傾向にあることが分かる。
　次に、６μｍ以上の結晶粒径の分布が、反射率に及ぼす影響について評価した。
　実施例１と同様にして発光素子搭載用セラミックス基体１を作製した。このときスラリーの粒度と焼成温度とを結晶粒径が円相当径で６μｍ以上の結晶が含まれるよう調整して作製し、試料Ｎｏ．14～20の発光素子搭載用セラミックス基体の試料を得た。
　また、反射率の測定方法は、実施例１と同様とし、波長400ｎｍおよび波長600ｎｍでの反射率が各々86％以上または90％以上で得られたものを『優』としてＡ、いずれか１つの項目を満足するものを『良』としＢ、両方を満足していないものを『可』としてＣとして結果を表２に示す。
Figure JPOXMLDOC01-appb-T000002
　表２に示す結果から分かるように、試料Ｎｏ．14は、結晶粒径が円相当径で６μｍを越える結晶の数の割合が2.7％を超えていることから、発光素子搭載用セラミックス基体内に入射した光が結晶の中を透過して裏面に抜けやすくなり、波長600ｎｍでの反射率が90％を僅かに割り込んだ数値となり、波長400ｎｍでの反射率は86％未満であった。試料Ｎｏ．15～18は、結晶粒径が円相当径で６μｍを越える結晶の数の割合が１％以上2.7％以下で含まれることから、発光素子搭載用セラミックス基体内に入射した光が結晶の中を透過して僅かに裏面に抜けやすくなり、波長600ｎｍでの反射率が90％を僅かに越えた数値となったのに対して、波長400ｎｍでの反射率は86％未満であった。これに対して、試料Ｎｏ．19～20は、結晶粒径が円相当径で６μｍを越える結晶の数の割合が０％であることから、発光素子搭載用セラミックス基体内に入射した光が反射する界面７が十分に存在し、反射光を高められ波長600ｎｍでの反射率が91％以上と高い状態であるうえに、短い波長を吸収もしくは減衰する大きな結晶粒子が少ないので、波長400ｎｍでの反射率が88.1％以上と高い状態で維持しやすくなったことが分かる。
　次に、平均結晶粒径が反射率と熱伝導率に及ぼす影響について評価した。
　実施例１と同様にして発光素子搭載用セラミックス基体を作製した。このときスラリーの粒度と焼成温度とを結晶粒径が円相当径で表３に示す値となるように調整し基体１を作製し、試料Ｎｏ．21～27の発光素子搭載用セラミックス基体の試料を得た。
　また、測定方法と、各試料の総合評価は実施例１と同様にした。
　得られた結果を表３に示す。
Figure JPOXMLDOC01-appb-T000003
　表３に示す結果から分かるように、試料Ｎｏ．22～27は、平均結晶粒径が1.3μｍ以下であることから発光素子搭載用セラミックス基体内に入射した光が反射する粒界７が十分に存在し、さらに、フォノンを散乱するガラス相５との間の界面７が減少し、波長600ｎｍでの反射率が91％以上であるとともに熱伝導率が17Ｗ／（ｍ・Ｋ）以上と高く、双方の特性を満足することができていることが分かる。
　次に、結晶粒子間に形成される粒界相５が反射率に及ぼす影響について評価した。実施例１と同様にして発光素子搭載用セラミックス基体１を作製した。このとき焼結助剤の量と焼成温度とを粒界相５が表４に示す値となるように調整し基体１を作製し、試料Ｎｏ．28～31の発光素子搭載用セラミックス基体１の試料を得た。
　また、反射率の測定方法は実施例１と同様にし、粒界相の平均幅の測定方法は、基板１の任意の断面をＴＥＭ観察により、任意の点において50,000倍まで拡大し測定し、粒界相の幅を測定する。そしてこの作業を計10点の視野において、粒界相の幅を測定し、平均することで求めた。そして各試料の総合評価は実施例２と同様にした。
　得られた結果を表４に示す。
Figure JPOXMLDOC01-appb-T000004
　表４に示す結果から分かるように、試料Ｎｏ．29～31は、粒界相５が２ｎｍ以下であることから、熱伝導率の低い粒界相が薄いので、光の反射を繰り返し拡散反射光13ｄが増加し、反射率が増加しやすくなるので、波長400ｎｍおよび波長600ｎｍでの反射率がそれぞれ各々86％以上および90％以上を維持した状態を満足することができていることが分かる。
　以上のように、実施形態の発光素子搭載用セラミックス基体１は、反射率が高く、熱伝導率も高い状態に維持することができる発光素子搭載用に好適なセラミックス基体１であることが分かる。
　そして、発光素子搭載用セラミックス基体１上に発光素子２を搭載した発光装置21は、発光素子２が発光する光を効率的に反射することができるとともに、熱伝導率が高いため放熱性に優れ熱による発光素子の劣化も低減しやすくなる。
１：発光素子搭載用セラミックス基体（基体）
１ａ：一方の表面、１ｂ：他方の表面
２：発光素子
３：導体
３ａ，３ｂ：電極パッド、３ｃ，３ｄ：電極（表電極）、３ｅ，３ｆ：貫通導体、３ｇ，３ｈ：電極（裏電極）
４：結晶粒子
５：ガラス相（粒界相）
６：気孔
７：界面（結晶粒子とガラス相との界面）
８：界面（気孔とガラス相との界面）
９：粒界相の範囲
11：入射光
12：透過光
13：反射光
13ａ：正反射光、13ｂ：拡散反射光、13ｃ：正反射光、13ｄ：拡散反射光、13ｅ：正
散反射光、13ｆ：拡散反射光
21：発光装置
31：封止部材
31ａ：レンズ
32：ボンディングワイヤ

Claims (6)

  1. 　セラミック焼結体からなり、発光素子が搭載される搭載部を有する発光素子搭載用セラミック焼結体であって、前記搭載部側の表層部における結晶粒径が円相当径で０．２μｍ以上１．０μｍ以下の結晶の割合が４５％以上８０％以下であり、円相当径で２．０μｍ以上６．０μｍ以下の結晶の割合が５％以上１５％以下であるとともに、円相当径で６．０μｍを超える結晶の割合が２．７％以下であることを特徴とする発光素子搭載用セラミックス基体。
  2. 　前記セラミック焼結体が、酸化アルミニウムを９４質量％以上含有してなることを特徴とする請求項１に記載の発光素子搭載用セラミックス基体。
  3. 　前記結晶粒径の最大粒径が６．０μｍ以下であることを特徴とする請求項１または請求項２に記載の発光素子搭載用セラミックス基体。
  4. 　平均結晶粒径が円相当径で、０．７μｍ以上１．３μｍ以下であることを特徴とする請求項１～３のいずれかに記載の発光素子搭載用セラミックス基体。
  5. 　前記セラミック焼結体が、前記結晶の結晶粒子間に形成される粒界相を有しており、前記粒界相の平均幅が２ｎｍ以下であることを特徴とする請求項１～４のいずれかに記載の発光素子搭載用セラミックス基体。
  6. 　請求項１～５のいずれかに記載の発光素子搭載用セラミックス基体上に発光素子を搭載したことを特徴とする発光装置。
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