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US20160033679A1 - Light reflective substrate and light emitting device using the same - Google Patents

Light reflective substrate and light emitting device using the same Download PDF

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Publication number
US20160033679A1
US20160033679A1 US14/880,797 US201514880797A US2016033679A1 US 20160033679 A1 US20160033679 A1 US 20160033679A1 US 201514880797 A US201514880797 A US 201514880797A US 2016033679 A1 US2016033679 A1 US 2016033679A1
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US
United States
Prior art keywords
light reflective
reflective substrate
glass
crystal
powder
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Abandoned
Application number
US14/880,797
Inventor
Yoshio Umayahara
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nippon Electric Glass Co Ltd
Original Assignee
Nippon Electric Glass Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Nippon Electric Glass Co Ltd filed Critical Nippon Electric Glass Co Ltd
Priority to US14/880,797 priority Critical patent/US20160033679A1/en
Assigned to NIPPON ELECTRIC GLASS CO., LTD. reassignment NIPPON ELECTRIC GLASS CO., LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: UMAYAHARA, YOSHIO
Publication of US20160033679A1 publication Critical patent/US20160033679A1/en
Abandoned legal-status Critical Current

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Classifications

    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C14/00—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix
    • C03C14/004—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix the non-glass component being in the form of particles or flakes
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C14/00—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix
    • C03C14/006—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix the non-glass component being in the form of microcrystallites, e.g. of optically or electrically active material
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F21—LIGHTING
    • F21V—FUNCTIONAL FEATURES OR DETAILS OF LIGHTING DEVICES OR SYSTEMS THEREOF; STRUCTURAL COMBINATIONS OF LIGHTING DEVICES WITH OTHER ARTICLES, NOT OTHERWISE PROVIDED FOR
    • F21V7/00—Reflectors for light sources
    • F21V7/22—Reflectors for light sources characterised by materials, surface treatments or coatings, e.g. dichroic reflectors
    • F21V7/24—Reflectors for light sources characterised by materials, surface treatments or coatings, e.g. dichroic reflectors characterised by the material
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/02—Diffusing elements; Afocal elements
    • G02B5/0205—Diffusing elements; Afocal elements characterised by the diffusing properties
    • G02B5/0236—Diffusing elements; Afocal elements characterised by the diffusing properties the diffusion taking place within the volume of the element
    • G02B5/0242—Diffusing elements; Afocal elements characterised by the diffusing properties the diffusion taking place within the volume of the element by means of dispersed particles
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/02—Diffusing elements; Afocal elements
    • G02B5/0273—Diffusing elements; Afocal elements characterized by the use
    • G02B5/0284—Diffusing elements; Afocal elements characterized by the use used in reflection
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/08—Mirrors
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2214/00—Nature of the non-vitreous component
    • C03C2214/04—Particles; Flakes

Definitions

  • the present invention relates to a light reflective substrate having high optical reflectivity and a light emitting device using the same.
  • LED and an organic EL device consume less electricity, and recently attract the attention as a new lighting device.
  • a substrate and a package material, having high optical reflectance are required in order to effectively utilize light emitted from a luminous body.
  • alumina ceramic having relatively high optical reflectance, or a substrate having provided on the alumina ceramic an light reflective film comprising a metal has been used as the conventional package material of LED element.
  • optical reflectance of a substrate and a package material is required to be further improved in order to obtain sufficient quantity of light as automotive lighting, display lighting and general lighting.
  • Patent Document 1 describes a light reflective substrate obtained by sintering a mixture of a glass powder and a ceramic powder, as a substrate having relatively high optical reflectivity.
  • the light reflective substrate described in Patent Document 1 comprises glass-ceramic containing a glass powder and a ceramic powder, wherein in a cross-section of the glass-ceramic, an area occupied by particles having a particle diameter of from 0.3 to 1 ⁇ m of the ceramic particles is from 10 to 70%.
  • high optical reflectivity is achieved by containing a large amount of ceramic particles having very fine particle size in the substrate.
  • Patent Document 1 JP-A-2007-121613
  • Light reflective substrate is obtained by, for example, forming a mixture of a glass powder and a ceramic powder into a slurry, forming the slurry into a green sheet, and firing the green sheet obtained.
  • a large amount of fine particles is contained in a substrate as in the light reflective substrate described in Patent Document 1, problems on production occur such that fluidity of the powder is deteriorated, and forming of a green sheet becomes difficult to be conducted.
  • the present invention has been made in view of the above circumstances, and has an object to provide a light reflective substrate capable of achieving high optical reflectance even though fine particles are not used as a material, and a light emitting device using the same.
  • the present inventors found that high optical reflectance can easily be realized by containing specific crystals having high refractive index characteristics in a glass matrix, and proposes the finding as the present invention.
  • the present invention relates a light reflective substrate comprising: a glass matrix; and RNb 2 O 6 crystal and/or R 4 Nb 2 O 9 crystal (R is at least one of Mg, Ca, Sr and Ba) in the glass matrix.
  • Refractive index of RNb 2 O 6 crystal and R 4 Nb 2 O 9 crystal is from 2.07 to 2.20, and those crystals have very high refractive index as compared with that of the other conventional oxide crystals.
  • a refractive index of a glass generally used as a light reflective substrate is generally from 1.5 to 1.6, and therefore, refractive index difference between a glass phase and a crystal phase can be increased. As a result, light reflectance on a surface of a light reflective substrate can remarkably be improved.
  • the light reflective substrate of the present invention is characterized that R is Ca.
  • the light reflective substrate of the present invention is characterized that the content of RNb 2 O 6 crystal and/or R 4 Nb 2 O 9 crystal is 0.3% by mass or more.
  • a light reflective substrate wherein RNb 2 O 6 crystal powder and/or R 4 Nb 2 O 9 crystal powder is uniformly dispersed in a glass matrix can easily be produced.
  • the light reflective substrate of the present invention is characterized to comprise a sintered body of a mixed powder containing a glass powder containing at least RO as a composition, and an Nb 2 O 5 powder.
  • a glass powder and an Nb 2 O 5 powder are reacted to each other to crystallize RNb 2 O 6 and/or R 4 Nb 2 O 9 .
  • light-absorbing defects are difficult to be foamed in an interface between those crystals and the glass matrix. Therefore, light scattering can be enhanced, and as a result, optical reflectance can be enhanced.
  • the light reflective substrate of the present invention is characterized to further comprise at least one ceramic powder selected from alumina, quartz, zirconia, titanium oxide, forsterite, cordierite, mullite and zircon.
  • the light reflective substrate of the present invention is characterized that the content of the ceramic powder is from 0.1 to 75% by mass.
  • the light reflective substrate of the present invention is characterized to have average optical reflectance at a wavelength of from 400 to 800 nm of 80% or more.
  • the present invention relates to a light emitting device using any one of the light reflective substrate described above.
  • the present invention relates to a light reflective substrate material, comprising a mixed powder containing a glass powder containing at least RO (R is at least one of Mg, Ca, Sr and Ba) as a composition, and Nb 2 O 5 powder.
  • RO is at least one of Mg, Ca, Sr and Ba
  • the light reflective substrate material of the present invention is characterized that the R is Ca.
  • the present invention relates to a green sheet for a light reflective substrate, using any one of the light reflective substrate material above.
  • the light reflective substrate according to the present invention comprises: a glass matrix; and RNb 2 O 6 crystal and/or R 4 Nb 2 O 9 crystal (R is at least one of Mg, Ca, Sr and Ba) in the glass matrix.
  • total content of RNb 2 O 6 crystal and R 4 Nb 2 O 9 crystal in the light reflective substrate is 0.3% by mass or more, 1.0% by mass or more, and particularly, 1.5% by mass or more.
  • the upper limit is not particularly limited. However, excessively large content of RNb 2 O 6 crystal and R 4 Nb 2 O 9 crystal is not preferred from the standpoint of production costs. Therefore, it is preferable that the content of RNb 2 O 6 crystal and R 4 Nb 2 O 9 crystal is 30% by mass or less, 20% by mass or less, and particularly, 10% by mass or less.
  • Particle diameter of RNb 2 O 6 crystal and R 4 Nb 2 O 9 crystal is not particularly limited. However, good optical reflectance can be obtained even at short wavelength in the vicinity of, for example, 400 nm with decreasing the particle diameter. On the other hand, an interface between the crystals and a glass matrix is decreased with increasing the crystal particle diameter, resulting in decrease in optical reflectance. From the standpoint of this, it is preferable that the crystal particle diameter is 10 ⁇ m or less, 5 ⁇ m or less, and particularly, 1 ⁇ m or less. As described before, in the case that the crystal particle diameter is small, fluidity of a powder is deteriorated, and green sheet forming tends to be difficult. Therefore, special attention is needed such that the crystal content is not excessive.
  • the light reflective substrate of the present invention can be produced by a method of sintering a material for a light reflective substrate, comprising a mixed powder containing RNb 2 O 6 crystal powder and/or R 4 Nb 2 O 9 crystal powder synthesized by, for example, a solid phase reaction, and a glass powder (production method 1).
  • a light reflective substrate wherein the RNb 2 O 6 crystal powder and/or the R 4 Nb 2 O 9 crystal powder is uniformly dispersed in the glass matrix can easily be produced.
  • the light reflective substrate of the present invention can be produced by a method of sintering a material for a light reflective substrate, comprising a mixed powder containing an RO-containing glass powder and Nb 2 O 5 powder, and simultaneously crystallizing RNb 2 O 6 and/or R 4 Nb 2 O 9 (production method 2).
  • production method 2 a process of previously synthesizing RNb 2 O 6 crystal powder and/or R 4 Nb 2 O 9 crystal powder can be omitted, leading to excellent mass productivity.
  • defects are liable to remain in the interface between the glass powder and the crystal powder. This becomes a factor of light absorption, and optical reflectance tends to be decreased.
  • Examples of the glass powder that can be used in the present invention include SiO 2 —B 2 O 3 —Al 2 O 3 glass, and SiO 2 —B 2 O 3 —R′ 2 O (R′ is at least one of Li, Na and K) glass.
  • the SiO 2 —B 2 O 3 —Al 2 O 3 glass preferably contains, in terms of % by mass as a composition, from 30 to 70% of SiO 2 , from 10 to 40% of RO (R is at least one of Mg, Ca, Sr and Ba), from 2 to 20% of B 2 O 3 , and from 2 to 20% of Al 2 O 3 .
  • RO is at least one of Mg, Ca, Sr and Ba
  • the reason for limiting the glass composition as above is as follows.
  • SiO 2 is a component of increasing chemical durability. It is preferable that SiO 2 content is from 30 to 70%, from 40 to 70%, and particularly, from 45 to 60%. When the SiO 2 content is less than 30%, weatherability tends to be remarkably deteriorated. On the other hand, when the SiO 2 content is more than 70%, a glass tends to be difficult to melt.
  • RO is a component for decreasing a liquidus temperature of a glass and adjusting meltability. It is preferable that RO content is from 10 to 40%, from 10 to 30%, and particularly, from 15 to 30%, in total. When the RO content is less than 10%, a melting temperature is too high. On the other hand, when the RO content is more than 40%, devitrification is easy to occur.
  • B 2 O 3 is a component of improving meltability of a glass and decreasing a liquidus temperature. It is preferable that the B 2 O 3 content is from 2 to 20%, from 2 to 15%, and particularly, from 4 to 13%. When the B 2 O 3 content is less than 2%, not only meltability of a glass is deteriorated, but a liquidus temperature is increased, and as a result, devitrification easily occurs when forming a glass. On the other hand, when the B 2 O 3 content is more than 20%, weatherability of a glass tends to be decreased.
  • Al 2 O 3 is a component of improving meltability and weatherability of a glass.
  • the Al 2 O 3 content is from 2 to 20%, and particularly, from 2.5 to 18%.
  • the Al 2 O 3 content is less than 2%, meltability of a glass is easily deteriorated.
  • the Al 2 O 3 content is more than 20%, devitrification easily occurs.
  • the SiO 2 —B 2 O 3 —R′ 2 O (R′ is at least one of Li, Na and K) glass preferably contains, in terms of % by mass as a composition, from 40 to 75% of SiO 2 , from 10 to 30% of B 2 O 3 , and from 0.5 to 20% of R′ 2 O.
  • the reason for limiting the glass composition as above is as follows.
  • SiO 2 is a network former of a glass. It is preferable that the SiO 2 content is from 40 to 75%, and particularly, from 50 to 70%. When the SiO 2 content is less than 40%, vitrification is difficult to occur. On the other hand, when the SiO 2 content is more than 75%, a glass tends to be difficult to melt.
  • B 2 O 3 is a component of improving meltability of a glass. It is preferable that the B 2 O 3 content is from 10 to 30%, and particularly, from 15 to 25%. When the B 2 O 3 content is less than 10%, a glass is difficult to melt. On the other hand, when the B 2 O 3 content is more than 30%, weatherability tends to be decreased.
  • R′ 2 O is a component of improving meltability of a glass.
  • the R′ 2 O content is from 0.5 to 20%, and preferably from 3 to 15%.
  • meltability of a glass tends to be remarkably deteriorated.
  • weatherability is easily decreased.
  • any of the glass composition can contain P 2 O 5 , MgO, ZnO, ZrO 2 , other oxide components, halide components, nitride components, and the like, other than the above components.
  • the SiO 2 —B 2 O 3 —R′ 2 O glass can contain BaO and SrO.
  • the total content of those other components is preferably limited to 20% or less.
  • Average particle diameter D 50 of the glass powder is not particularly limited. However, when the average particle diameter D 50 is too large, optical reflectance and mechanical strength of a light reflective substrate are easily decreased. Therefore, the average particle diameter D 50 is preferably 15 ⁇ m or less, and particularly preferably 7 ⁇ m or less. On the other hand, when the average particle diameter D 50 is too small, production costs are increased. Therefore, the average particle diameter D 50 is preferably 0.5 ⁇ m or more, and particularly preferably 1.5 ⁇ m or more.
  • the light reflective substrate of the present invention can contain a ceramic powder as a filler in order to increase mechanical strength, other than RNb 2 O 6 crystal and R 4 Nb 2 O 9 crystal.
  • a ceramic powder include alumina, quartz, zirconia, titanium oxide, forsterite, cordierite, mullite and zircon. Those can be used alone or as mixtures of two kinds or more thereof.
  • the content of the ceramic powder in the light reflective substrate is from 0.1 to 75% by mass, from 2 to 75% by mass, and particularly, from 20 to 50% by mass.
  • the ceramic powder content is less than 0.1% by mass, an effect of increasing mechanical strength is difficult to achieve.
  • the ceramic powder content is more than 75% by mass, many pores are generated in the light reflective substrate, and mechanical strength is easy to be decreased.
  • the light reflective substrate of the present invention is produced by preforming a raw material powder containing a glass powder (material for light reflective substrate) into various forms such as a plate form, a sheet form and a block form, and then firing.
  • the preforming method various methods can be selected. Examples of the preforming method include a green sheet (tape) forming method, a slip casting method, a screen printing method, a mold pressing method, an aerosol deposition method, a spin coating method, and a die coating method.
  • a green sheet (tape) forming method As the preforming method, various methods can be selected. Examples of the preforming method include a green sheet (tape) forming method, a slip casting method, a screen printing method, a mold pressing method, an aerosol deposition method, a spin coating method, and a die coating method.
  • the green sheet forming method is a method of adding a resin binder, a plasticizer and a solvent to a raw material powder, kneading the resulting mixture to prepare a slurry, and preparing a green sheet (tape) from the slurry using a sheet forming machine such as a doctor blade.
  • This method is in widespread use as a method for producing a ceramic laminated circuit board. According to this method, in producing a ceramic laminated circuit board having optical reflective function by, for example, laminating a green sheet, it is easy to form a circuit in a board, to embed a metal material having high thermal conductivity by forming an electric via-hole, or to form a heat discharge passage by a thermal via-hole.
  • the screen printing method is a method of adding a resin binder and a solvent to an inorganic powder, kneading the resulting mixture to prepare a paste having a certain level of high viscosity, and forming a film on a surface of a substrate using a screen printing machine.
  • a light reflecting portion of a specific pattern can easily be formed on the surface of a substrate.
  • a film having a desired thickness of from about several microns to about several hundred microns can be formed by adjusting viscosity of a paste, thickness of a screen, the number of printing, and the like.
  • average optical reflectance at a wavelength of from 400 to 800 nm of the light reflective substrate of the present invention is 80% or more, 85% or more, and particularly, 88% or more.
  • a light-permeable functional layer can be provided on a surface of the light reflective substrate of the present invention.
  • a protective coating against scratches, stain and chemical corrosion, and a functional layer having a function as a wavelength filter, optical diffusion or an interference layer can be further formed while maintaining optical reflective function on the surface of the light reflective substrate.
  • the functional layer is not particularly limited, and conventional materials such as glasses such as silicate glass; metal oxides such as silica, alumina, zirconia, tantalum oxide and niobium oxide; and resins such as polymethyl methacrylate, polycarbonate and polyacrylate can be used.
  • glasses such as silicate glass
  • metal oxides such as silica, alumina, zirconia, tantalum oxide and niobium oxide
  • resins such as polymethyl methacrylate, polycarbonate and polyacrylate can be used.
  • Light reflective substrate of each of Examples and Comparative Examples was produced as follows.
  • Raw materials were formulated so as to obtain glasses having compositions shown in Tables 1 and 2, and melted in an electric furnace kept at from 1,400 to 1,600° C. for 2 hours.
  • the molten glass obtained was poured in water-cooled rollers to obtain a film-shaped glass.
  • the content of RNb 2 O 6 crystal and R 4 Nb 2 O 9 crystal in the light reflective substrate obtained was calculated based on peak intensity by powder X-ray diffraction.
  • Optical reflectance of the light reflective substrate obtained was measured. The results are shown in Tables 1 and 2. The optical reflectance was evaluated by average optical reflectance at a wavelength of from 400 to 800 nm measured by spectrophotometer.
  • the light reflective substrates of Examples 1 to 8 contain RNb 2 O 6 crystal or R 4 Nb 2 O 9 crystal, having high refractive index, and therefore had high reflectance of 82% or more.
  • the light reflective substrates of Comparative Examples 1 to 3 had low optical reflectance of from 72 to 78%.
  • the light reflective substrate of the present invention has very high optical reflectance, and is therefore suitable for uses as a light reflective substrate used in displays such as LED package and organic EL, automotive lighting, general lighting and the like.

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  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Optics & Photonics (AREA)
  • General Physics & Mathematics (AREA)
  • Dispersion Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Ceramic Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Glass Compositions (AREA)
  • Optical Elements Other Than Lenses (AREA)
  • Led Device Packages (AREA)

Abstract

An object of the present invention is to provide a light reflective substrate capable of achieving high optical reflectance even though fine particles are not used as a material, and a light emitting device using the same. The light reflective substrate according to the present invention comprises: a glass matrix; and RNb2O6 crystal and/or R4Nb2O9 crystal (R is at least one of Mg, Ca, Sr and Ba) in the glass matrix.

Description

    TECHNICAL FIELD
  • The present invention relates to a light reflective substrate having high optical reflectivity and a light emitting device using the same.
    • BACKGROUND ART
  • LED and an organic EL device consume less electricity, and recently attract the attention as a new lighting device. In a device for lighting, a substrate and a package material, having high optical reflectance are required in order to effectively utilize light emitted from a luminous body. For example, alumina ceramic having relatively high optical reflectance, or a substrate having provided on the alumina ceramic an light reflective film comprising a metal has been used as the conventional package material of LED element. However, optical reflectance of a substrate and a package material is required to be further improved in order to obtain sufficient quantity of light as automotive lighting, display lighting and general lighting.
  • To achieve the above object, Patent Document 1 describes a light reflective substrate obtained by sintering a mixture of a glass powder and a ceramic powder, as a substrate having relatively high optical reflectivity. Specifically, the light reflective substrate described in Patent Document 1 comprises glass-ceramic containing a glass powder and a ceramic powder, wherein in a cross-section of the glass-ceramic, an area occupied by particles having a particle diameter of from 0.3 to 1 μm of the ceramic particles is from 10 to 70%. Thus, in Patent Document 1, high optical reflectivity is achieved by containing a large amount of ceramic particles having very fine particle size in the substrate.
    • CITATION LIST Patent Document
  • Patent Document 1: JP-A-2007-121613
    • SUMMARY OF THE INVENTION Problems to be Solved by the Invention
  • Light reflective substrate is obtained by, for example, forming a mixture of a glass powder and a ceramic powder into a slurry, forming the slurry into a green sheet, and firing the green sheet obtained. However, when a large amount of fine particles is contained in a substrate as in the light reflective substrate described in Patent Document 1, problems on production occur such that fluidity of the powder is deteriorated, and forming of a green sheet becomes difficult to be conducted.
  • The present invention has been made in view of the above circumstances, and has an object to provide a light reflective substrate capable of achieving high optical reflectance even though fine particles are not used as a material, and a light emitting device using the same.
    • Means for Solving the Problems
  • The present inventors found that high optical reflectance can easily be realized by containing specific crystals having high refractive index characteristics in a glass matrix, and proposes the finding as the present invention.
  • That is, the present invention relates a light reflective substrate comprising: a glass matrix; and RNb2O6 crystal and/or R4Nb2O9 crystal (R is at least one of Mg, Ca, Sr and Ba) in the glass matrix.
  • Refractive index of RNb2O6 crystal and R4Nb2O9 crystal is from 2.07 to 2.20, and those crystals have very high refractive index as compared with that of the other conventional oxide crystals. On the other hand, a refractive index of a glass generally used as a light reflective substrate is generally from 1.5 to 1.6, and therefore, refractive index difference between a glass phase and a crystal phase can be increased. As a result, light reflectance on a surface of a light reflective substrate can remarkably be improved.
  • Secondly, the light reflective substrate of the present invention is characterized that R is Ca.
  • Thirdly, the light reflective substrate of the present invention is characterized that the content of RNb2O6 crystal and/or R4Nb2O9 crystal is 0.3% by mass or more.
  • Fourthly, the light reflective substrate of the present invention is characterized to comprise a sintered body of a mixed powder containing a glass powder and RNb2O6 crystal and/or R4Nb2O9 crystal powders.
  • According to the constitution, a light reflective substrate wherein RNb2O6 crystal powder and/or R4Nb2O9 crystal powder is uniformly dispersed in a glass matrix can easily be produced.
  • Fifthly, the light reflective substrate of the present invention is characterized to comprise a sintered body of a mixed powder containing a glass powder containing at least RO as a composition, and an Nb2O5 powder.
  • According to the constitution, a glass powder and an Nb2O5 powder are reacted to each other to crystallize RNb2O6 and/or R4Nb2O9. As a result, light-absorbing defects are difficult to be foamed in an interface between those crystals and the glass matrix. Therefore, light scattering can be enhanced, and as a result, optical reflectance can be enhanced.
  • Sixthly, the light reflective substrate of the present invention is characterized to further comprise at least one ceramic powder selected from alumina, quartz, zirconia, titanium oxide, forsterite, cordierite, mullite and zircon.
  • According to the constitution, mechanical strength of the light reflective substrate can further be improved.
  • Seventhly, the light reflective substrate of the present invention is characterized that the content of the ceramic powder is from 0.1 to 75% by mass.
  • Eighthly, the light reflective substrate of the present invention is characterized to have average optical reflectance at a wavelength of from 400 to 800 nm of 80% or more.
  • Ninthly, the present invention relates to a light emitting device using any one of the light reflective substrate described above.
  • Tenthly, the present invention relates to a light reflective substrate material, comprising a mixed powder containing a glass powder, and RNb2O6 crystal powder and/or R4Nb2O9 crystal powder (R is at least one of Mg, Ca, Sr and Ba).
  • Eleventhly, the present invention relates to a light reflective substrate material, comprising a mixed powder containing a glass powder containing at least RO (R is at least one of Mg, Ca, Sr and Ba) as a composition, and Nb2O5 powder.
  • Twelfthly, the light reflective substrate material of the present invention is characterized that the R is Ca.
  • Thirteenthly, the present invention relates to a green sheet for a light reflective substrate, using any one of the light reflective substrate material above.
    • MODE FOR CARRYING OUT THE INVENTION
  • The light reflective substrate according to the present invention comprises: a glass matrix; and RNb2O6 crystal and/or R4Nb2O9 crystal (R is at least one of Mg, Ca, Sr and Ba) in the glass matrix.
  • It is preferable that total content of RNb2O6 crystal and R4Nb2O9 crystal in the light reflective substrate is 0.3% by mass or more, 1.0% by mass or more, and particularly, 1.5% by mass or more. When the content of RNb2O6 crystal and R4Nb2O9 crystal is less than 0.3% by mass, sufficient optical reflectance is difficult to be obtained. On the other hand, the upper limit is not particularly limited. However, excessively large content of RNb2O6 crystal and R4Nb2O9 crystal is not preferred from the standpoint of production costs. Therefore, it is preferable that the content of RNb2O6 crystal and R4Nb2O9 crystal is 30% by mass or less, 20% by mass or less, and particularly, 10% by mass or less.
  • Particle diameter of RNb2O6 crystal and R4Nb2O9 crystal is not particularly limited. However, good optical reflectance can be obtained even at short wavelength in the vicinity of, for example, 400 nm with decreasing the particle diameter. On the other hand, an interface between the crystals and a glass matrix is decreased with increasing the crystal particle diameter, resulting in decrease in optical reflectance. From the standpoint of this, it is preferable that the crystal particle diameter is 10 μm or less, 5 μm or less, and particularly, 1 μm or less. As described before, in the case that the crystal particle diameter is small, fluidity of a powder is deteriorated, and green sheet forming tends to be difficult. Therefore, special attention is needed such that the crystal content is not excessive.
  • The light reflective substrate of the present invention can be produced by a method of sintering a material for a light reflective substrate, comprising a mixed powder containing RNb2O6 crystal powder and/or R4Nb2O9 crystal powder synthesized by, for example, a solid phase reaction, and a glass powder (production method 1). According to the method, a light reflective substrate wherein the RNb2O6 crystal powder and/or the R4Nb2O9 crystal powder is uniformly dispersed in the glass matrix can easily be produced.
  • Alternatively, the light reflective substrate of the present invention can be produced by a method of sintering a material for a light reflective substrate, comprising a mixed powder containing an RO-containing glass powder and Nb2O5 powder, and simultaneously crystallizing RNb2O6 and/or R4Nb2O9 (production method 2). Particularly, according to the production method 2, a process of previously synthesizing RNb2O6 crystal powder and/or R4Nb2O9 crystal powder can be omitted, leading to excellent mass productivity. Furthermore, in the production method 1, defects are liable to remain in the interface between the glass powder and the crystal powder. This becomes a factor of light absorption, and optical reflectance tends to be decreased.
  • However, in the production method 2, light-absorbable defects are difficult to be formed in the interface between a glass matrix and crystal particles. Therefore light scattering can be enhanced, and as a result, optical reflectance can be enhanced.
  • Examples of the glass powder that can be used in the present invention include SiO2—B2O3—Al2O3 glass, and SiO2—B2O3—R′2O (R′ is at least one of Li, Na and K) glass.
  • The SiO2—B2O3—Al2O3 glass preferably contains, in terms of % by mass as a composition, from 30 to 70% of SiO2, from 10 to 40% of RO (R is at least one of Mg, Ca, Sr and Ba), from 2 to 20% of B2O3, and from 2 to 20% of Al2O3.
  • The reason for limiting the glass composition as above is as follows.
  • SiO2 is a component of increasing chemical durability. It is preferable that SiO2 content is from 30 to 70%, from 40 to 70%, and particularly, from 45 to 60%. When the SiO2 content is less than 30%, weatherability tends to be remarkably deteriorated. On the other hand, when the SiO2 content is more than 70%, a glass tends to be difficult to melt.
  • RO is a component for decreasing a liquidus temperature of a glass and adjusting meltability. It is preferable that RO content is from 10 to 40%, from 10 to 30%, and particularly, from 15 to 30%, in total. When the RO content is less than 10%, a melting temperature is too high. On the other hand, when the RO content is more than 40%, devitrification is easy to occur.
  • Preferable range of the content of each component of RO is as follows. That is, it is preferable that CaO content is from 10 to 40%, from 10 to 30%, and particularly, from 15 to 30%. It is preferable that the content of each of MgO, SrO and BaO is from 10 to 40%, from 10 to 30%, and particularly, from 15 to 20%.
  • B2O3 is a component of improving meltability of a glass and decreasing a liquidus temperature. It is preferable that the B2O3 content is from 2 to 20%, from 2 to 15%, and particularly, from 4 to 13%. When the B2O3 content is less than 2%, not only meltability of a glass is deteriorated, but a liquidus temperature is increased, and as a result, devitrification easily occurs when forming a glass. On the other hand, when the B2O3 content is more than 20%, weatherability of a glass tends to be decreased.
  • Al2O3 is a component of improving meltability and weatherability of a glass.
  • It is preferable that the Al2O3 content is from 2 to 20%, and particularly, from 2.5 to 18%. When the Al2O3 content is less than 2%, meltability of a glass is easily deteriorated. On the other hand, when the Al2O3 content is more than 20%, devitrification easily occurs.
  • The SiO2—B2O3—R′2O (R′ is at least one of Li, Na and K) glass preferably contains, in terms of % by mass as a composition, from 40 to 75% of SiO2, from 10 to 30% of B2O3, and from 0.5 to 20% of R′2O.
  • The reason for limiting the glass composition as above is as follows.
  • SiO2 is a network former of a glass. It is preferable that the SiO2 content is from 40 to 75%, and particularly, from 50 to 70%. When the SiO2 content is less than 40%, vitrification is difficult to occur. On the other hand, when the SiO2 content is more than 75%, a glass tends to be difficult to melt.
  • B2O3 is a component of improving meltability of a glass. It is preferable that the B2O3 content is from 10 to 30%, and particularly, from 15 to 25%. When the B2O3 content is less than 10%, a glass is difficult to melt. On the other hand, when the B2O3 content is more than 30%, weatherability tends to be decreased.
  • R′2O is a component of improving meltability of a glass. The R′2O content is from 0.5 to 20%, and preferably from 3 to 15%. When the R′2O content is less than 0.5%, meltability of a glass tends to be remarkably deteriorated. On the other hand, when the R′2O content is more than 20%, weatherability is easily decreased.
  • Any of the glass composition can contain P2O5, MgO, ZnO, ZrO2, other oxide components, halide components, nitride components, and the like, other than the above components. Furthermore, the SiO2—B2O3—R′2O glass can contain BaO and SrO. However, the total content of those other components is preferably limited to 20% or less.
  • Average particle diameter D50 of the glass powder is not particularly limited. However, when the average particle diameter D50 is too large, optical reflectance and mechanical strength of a light reflective substrate are easily decreased. Therefore, the average particle diameter D50 is preferably 15 μm or less, and particularly preferably 7 μm or less. On the other hand, when the average particle diameter D50 is too small, production costs are increased. Therefore, the average particle diameter D50 is preferably 0.5 μm or more, and particularly preferably 1.5 μm or more.
  • The light reflective substrate of the present invention can contain a ceramic powder as a filler in order to increase mechanical strength, other than RNb2O6 crystal and R4Nb2O9 crystal. Examples of the ceramic powder include alumina, quartz, zirconia, titanium oxide, forsterite, cordierite, mullite and zircon. Those can be used alone or as mixtures of two kinds or more thereof.
  • It is preferable that the content of the ceramic powder in the light reflective substrate is from 0.1 to 75% by mass, from 2 to 75% by mass, and particularly, from 20 to 50% by mass. When the ceramic powder content is less than 0.1% by mass, an effect of increasing mechanical strength is difficult to achieve. On the other hand, when the ceramic powder content is more than 75% by mass, many pores are generated in the light reflective substrate, and mechanical strength is easy to be decreased.
  • The light reflective substrate of the present invention is produced by preforming a raw material powder containing a glass powder (material for light reflective substrate) into various forms such as a plate form, a sheet form and a block form, and then firing.
  • As the preforming method, various methods can be selected. Examples of the preforming method include a green sheet (tape) forming method, a slip casting method, a screen printing method, a mold pressing method, an aerosol deposition method, a spin coating method, and a die coating method.
  • The green sheet forming method is a method of adding a resin binder, a plasticizer and a solvent to a raw material powder, kneading the resulting mixture to prepare a slurry, and preparing a green sheet (tape) from the slurry using a sheet forming machine such as a doctor blade. This method is in widespread use as a method for producing a ceramic laminated circuit board. According to this method, in producing a ceramic laminated circuit board having optical reflective function by, for example, laminating a green sheet, it is easy to form a circuit in a board, to embed a metal material having high thermal conductivity by forming an electric via-hole, or to form a heat discharge passage by a thermal via-hole.
  • The screen printing method is a method of adding a resin binder and a solvent to an inorganic powder, kneading the resulting mixture to prepare a paste having a certain level of high viscosity, and forming a film on a surface of a substrate using a screen printing machine. According to this method, a light reflecting portion of a specific pattern can easily be formed on the surface of a substrate. Furthermore, a film having a desired thickness of from about several microns to about several hundred microns can be formed by adjusting viscosity of a paste, thickness of a screen, the number of printing, and the like.
  • It is preferable that average optical reflectance at a wavelength of from 400 to 800 nm of the light reflective substrate of the present invention is 80% or more, 85% or more, and particularly, 88% or more.
  • A light-permeable functional layer can be provided on a surface of the light reflective substrate of the present invention. For example, a protective coating against scratches, stain and chemical corrosion, and a functional layer having a function as a wavelength filter, optical diffusion or an interference layer can be further formed while maintaining optical reflective function on the surface of the light reflective substrate.
  • The functional layer is not particularly limited, and conventional materials such as glasses such as silicate glass; metal oxides such as silica, alumina, zirconia, tantalum oxide and niobium oxide; and resins such as polymethyl methacrylate, polycarbonate and polyacrylate can be used.
    • EXAMPLES
  • The present invention is described below by reference to Examples. However, the invention is not construed as being limited to those Examples.
  • Tables 1 and 2 show Examples and Comparative Examples.
  • TABLE 1
    Example Comparative Example
    1 2 3 4 1 2 3
    Glass powder SiO2 55 40 50 60 55 40 50
    composition Al2O3 14 10 14 10
    (% by mass) B2O3 6 15 20 25 6 15 20
    MgO 2 2
    CaO 23 30 23 30
    BaO 5 5
    ZnO 3 5 3 5
    Li2O 2 6 2
    Na2O 2 5 9 2 5
    K2O 3 5 3 5
    TiO2 2 2
    ZrO2 2 2
    P2O5 1 1
    Raw material Glass 68.4 96 57 61 70 75 60
    powder powder
    composition CaNb2O6 2
    (% by mass) Ca4Nb2O9 3 2
    Nb2O5 1.6 4
    Alumina 30 30
    Zirconia 40 40
    Mullite 35
    Quartz 25
    High refractive index CaNb2O6 CaNb2O6 Ca4Nb2O9 CaNb2O6 None None None
    crystal (2) (5) (3) (2)
    *( ) means content Ca4Nb2O9
    (% by mass) (2)
    Optical reflectance (%) 90 88 82 90 78 75 72
  • TABLE 2
    Example
    5 6 7 8
    Glass powder SiO2 50 50 55 58
    composition Al2O3 14 5 4
    (% by mass) B2O3 11 10 15 25
    MgO 10
    CaO 15 20
    SrO 7 4
    BaO 6 10
    Li2O 2 4
    Na2O 2 5 5
    K2O 3 5
    TiO2 2
    ZrO2 2
    P2O5 1
    Raw material Glass 67 96 77 76
    powder powder
    composition CaNb2O6 2
    (% by mass) Ca4Nb2O9 3 2
    Nb2O5 3 4
    Alumina 30
    Zirconia 20
    Mullite
    Quartz 20
    High refractive index MgNb2O6 (1) CaNb2O6 (2) Ca4Nb2O9 (3) CaNb2O6 (2)
    crystal CaNb2O6 (2) SrNb2O6 (1) BaNb2O6 (1) Ca4Nb2O9 (2)
    *( ) means content BaNb2O6 (1) SrNb2O6 (1)
    (% by mass)
    Optical reflectivity (%) 91 89 85 91
  • Light reflective substrate of each of Examples and Comparative Examples was produced as follows. Raw materials were formulated so as to obtain glasses having compositions shown in Tables 1 and 2, and melted in an electric furnace kept at from 1,400 to 1,600° C. for 2 hours. The molten glass obtained was poured in water-cooled rollers to obtain a film-shaped glass. The glass film was pulverized with alumina ball mill to obtain a glass powder (average particle diameter D50=3 μm).
  • Various inorganic powders were mixed with the glass powder in proportions shown in Tables 1 and 2. The resulting mixed powder was press molded with a mold having a diameter of 20 mm to prepare columnar pellets. The pellets were fired at 950° C. for 2 hours to obtain a light reflective substrate.
  • The content of RNb2O6 crystal and R4Nb2O9 crystal in the light reflective substrate obtained was calculated based on peak intensity by powder X-ray diffraction.
  • Optical reflectance of the light reflective substrate obtained was measured. The results are shown in Tables 1 and 2. The optical reflectance was evaluated by average optical reflectance at a wavelength of from 400 to 800 nm measured by spectrophotometer.
  • As shown in Tables 1 and 2, the light reflective substrates of Examples 1 to 8 contain RNb2O6 crystal or R4Nb2O9 crystal, having high refractive index, and therefore had high reflectance of 82% or more. On the other hand, the light reflective substrates of Comparative Examples 1 to 3 had low optical reflectance of from 72 to 78%.
  • Although the present invention has been described in detail and by reference to the specific embodiments, it is apparent to one skilled in the art that various changes or modifications can be made without departing the spirit and scope of the present invention.
  • This application is based on Japanese Patent Application No. 2010-041461 filed Feb. 26, 2010 and Japanese Patent Application No. 2011-28031 filed Feb. 14, 2011, the disclosures of which are incorporated herein by reference in their entities.
    • INDUSTRIAL APPLICABILITY
  • The light reflective substrate of the present invention has very high optical reflectance, and is therefore suitable for uses as a light reflective substrate used in displays such as LED package and organic EL, automotive lighting, general lighting and the like.

Claims (5)

1-10. (canceled)
11. A light reflective substrate material, comprising a mixed powder containing a glass powder containing at least RO (R is at least one of Mg, Ca, Sr and Ba) as a composition, and Nb2O5 powder.
12. The light reflective substrate material according to claim 11, wherein the R is Ca.
13. A green sheet for a light reflective substrate, using the light reflective substrate material according to claim 12.
14. A green sheet for a light reflective substrate, using the light reflective substrate material according to claim 11.
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