WO2019065194A1 - Élément de conversion en longueur d'onde, source lumineuse, particules à corps fluorescents et procédé de production d'élément de conversion en longueur d'onde - Google Patents

Élément de conversion en longueur d'onde, source lumineuse, particules à corps fluorescents et procédé de production d'élément de conversion en longueur d'onde Download PDF

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WO2019065194A1
WO2019065194A1 PCT/JP2018/033524 JP2018033524W WO2019065194A1 WO 2019065194 A1 WO2019065194 A1 WO 2019065194A1 JP 2018033524 W JP2018033524 W JP 2018033524W WO 2019065194 A1 WO2019065194 A1 WO 2019065194A1
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atoms
phosphor particles
wavelength conversion
conversion member
surface layer
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PCT/JP2018/033524
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English (en)
Japanese (ja)
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佑亮 小城原
俊幸 瀧澤
濱田　貴裕
幸彦 杉尾
純久 長崎
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パナソニックＩｐマネジメント株式会社
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/64—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing aluminium
    • 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
    • F21V9/00—Elements for modifying spectral properties, polarisation or intensity of the light emitted, e.g. filters
    • F21V9/08—Elements for modifying spectral properties, polarisation or intensity of the light emitted, e.g. filters for producing coloured light, e.g. monochromatic; for reducing intensity of light
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/20—Filters
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
    • H01L33/50—Wavelength conversion elements

Definitions

  • the present disclosure relates to a wavelength conversion member, a light source, phosphor particles, and a method of manufacturing the wavelength conversion member.
  • the wavelength conversion member has phosphor particles embedded in a matrix.
  • the light of the light emitting element is irradiated to the phosphor particles as excitation light, and light of a wavelength longer than the wavelength of the excitation light is emitted from the phosphor.
  • attempts have been made to increase the brightness and power of the light.
  • Patent Document 1 discloses a wavelength conversion member in which zinc oxide (ZnO) is used as a matrix material.
  • ZnO is an inorganic material having a refractive index close to the refractive index of many phosphors, and also has excellent transparency and high thermal conductivity. According to the wavelength conversion member of Patent Document 1, light scattering at the interface between the phosphor particles and the ZnO matrix can be suppressed, and high light output can be achieved.
  • Patent Document 2 discloses a matrix composed of ZnO polycrystals oriented in the c-axis.
  • the wavelength conversion member of Patent Document 1 has room for improvement from the viewpoint of heat dissipation depending on the phosphor particles used.
  • An object of the present disclosure is to provide a wavelength conversion member having excellent heat dissipation.
  • the wavelength conversion member of the present disclosure includes phosphor particles having a surface layer, and a matrix including zinc oxide and surrounding the phosphor particles, and the surface layer is the phosphor described above at an acceleration voltage of 10.0 kV. It is a part from which composition information can be obtained when performing energy dispersive X-ray analysis of particles, and at least one of the following (a) and (b) is selected from the group:
  • the phosphor particles contain nitride or oxynitride as a main component, and the molar ratio of oxygen atoms to all atoms in the surface layer is 20.0% or more.
  • the phosphor particles contain aluminum, and the molar ratio of aluminum atoms to all atoms in the surface layer is lower than the molar ratio of aluminum atoms to all atoms in the phosphor particles.
  • a wavelength conversion member having excellent heat dissipation can be provided.
  • FIG. 1 is a schematic cross-sectional view of a wavelength conversion member according to an embodiment of the present disclosure.
  • FIG. 2 is a cross-sectional view of the phosphor particle shown in FIG.
  • FIG. 3 is a schematic cross-sectional view of a reflection-type light source using the wavelength conversion member of the present disclosure.
  • FIG. 4 is a schematic cross-sectional view of a transmissive light source using the wavelength conversion member of the present disclosure.
  • FIG. 5 is a schematic configuration diagram of a lighting device using the light source of the present disclosure.
  • FIG. 6A is an energy dispersive X-ray analysis (EDX) spectrum of a conventional phosphor particle made of CaAlSiN 3 : Eu.
  • FIG. EDX energy dispersive X-ray analysis
  • FIG. 6B is a diagram showing an EDX spectrum of a conventional phosphor particle made of CaAlSiN 3 : Eu.
  • 7A shows an EDX spectrum of phosphor particles of sample 1.
  • FIG. 7B is a diagram showing an EDX spectrum of phosphor particles of sample 1.
  • FIG. 8A shows an EDX spectrum of a conventional phosphor particle made of (Ca, Sr) AlSiN 3 : Eu.
  • FIG. 8B is a diagram showing an EDX spectrum of a conventional phosphor particle made of (Ca, Sr) AlSiN 3 : Eu.
  • FIG. 9A is a diagram showing an EDX spectrum of phosphor particles of sample 2.
  • FIG. 9A is a diagram showing an EDX spectrum of phosphor particles of sample 2.
  • FIG. 9B is a diagram showing an EDX spectrum of phosphor particles of sample 2.
  • FIG. 10 is a view showing a scanning electron micrograph of the cross section of the phosphor layer in the wavelength conversion member of Example 1.
  • FIG. 11 is a view showing a scanning electron micrograph of the cross section of the phosphor layer in the wavelength conversion member of Comparative Example 1.
  • the matrix containing zinc oxide can be formed, for example, by crystal growth of zinc oxide.
  • a solution growth method using a solution containing Zn ions can be used for crystal growth of zinc oxide.
  • crystal growth of zinc oxide may be inhibited. At this time, many phosphor particles are exposed to the outside of the matrix. Therefore, there is a problem that a wavelength conversion member having sufficient heat dissipation can not be obtained.
  • elements contained in phosphor particles may be eluted in a solution for crystal growth.
  • the elements eluted in the solution for crystal growth may react with chemical species contained in the solution for crystal growth. This reaction may form a complex oxide containing an element eluted in a solution for crystal growth.
  • the present inventors have found that the elution of elements contained in phosphor particles can be suppressed by treating the surface of the phosphor particles in advance. Furthermore, the present inventors have found that zinc oxide can be easily crystal-grown by suppressing the elution of elements contained in phosphor particles.
  • the wavelength conversion member according to the first aspect of the present disclosure includes phosphor particles having a surface layer, and a matrix that contains zinc oxide and surrounds the phosphor particles.
  • the surface layer is a portion from which information on the composition can be obtained when energy dispersive X-ray analysis of the phosphor particles is performed at an acceleration voltage of 10.0 kV, and it comprises the following (a) and (b) Meet at least one requirement selected from the group.
  • the phosphor particles contain nitride or oxynitride as a main component, and the molar ratio of oxygen atoms to all atoms in the surface layer is 20.0% or more.
  • the phosphor particles contain aluminum, and the molar ratio of aluminum atoms to all atoms in the surface layer is lower than the molar ratio of aluminum atoms to all atoms in the phosphor particles.
  • the molar ratio of oxygen atoms to all atoms in the surface layer of phosphor particles is relatively high, or the molar ratio of aluminum atoms to all atoms in the surface layer is relatively low.
  • the wavelength conversion member has excellent heat dissipation.
  • the phosphor particles of the wavelength conversion member according to the first aspect include an alkaline earth metal.
  • the wavelength conversion member can provide light having high luminance and excellent color rendering.
  • the molar ratio of aluminum atoms to all atoms in the surface layer of the wavelength conversion member according to the first or second aspect is 20.0% or less.
  • the wavelength conversion member has excellent heat dissipation.
  • the phosphor particles of the wavelength conversion member according to any one of the first to third aspects contain a nitride or an oxynitride as a main component, and for all atoms in the surface layer.
  • the molar ratio of nitrogen atoms is 20.0% or less.
  • the wavelength conversion member has excellent heat dissipation.
  • the phosphor particles of the wavelength conversion member according to any one of the first to fourth aspects contain silicon, and the molar ratio of oxygen atoms to all atoms in the surface layer; The total of the molar ratio of silicon atoms to all atoms in at least 55.0%.
  • the wavelength conversion member has excellent heat dissipation.
  • the phosphor particles of the wavelength conversion member according to any one of the first to fifth aspects contain the nitride as a main component, and the nitride is CaAlSiN 3 or (Ca , Sr) AlSiN 3 .
  • the wavelength conversion member can provide light having high luminance and excellent color rendering.
  • a light source includes: a light emitting element; and the wavelength conversion member according to any one of the first to sixth aspects disposed on the optical path of light emitted from the light emitting element. It is a thing.
  • the wavelength conversion member has excellent heat dissipation. Therefore, it is possible to easily provide a light source having desired optical characteristics.
  • the method for producing a wavelength conversion member according to the eighth aspect of the present disclosure includes treating the phosphor particles with an acid, and forming a matrix containing zinc oxide so as to surround the phosphor particles.
  • the phosphor particles can be easily surrounded by the matrix. Therefore, the wavelength conversion member which has the outstanding heat dissipation is obtained.
  • the acid is an aqueous acid solution.
  • a wavelength conversion member having excellent heat dissipation can be obtained.
  • the acid is an aqueous nitric acid solution boiling
  • the fluorescent substance particles are treated by bringing the fluorescent substance particles into contact with the aqueous boiling nitric acid solution. According to the tenth aspect, a wavelength conversion member having excellent heat dissipation can be obtained.
  • a matrix is formed by crystal growth of zinc oxide by a solution growth method. According to the eleventh aspect, a wavelength conversion member having excellent heat dissipation can be obtained.
  • the phosphor particle contains an alkaline earth metal.
  • the wavelength conversion member provides light having high luminance and excellent color rendering.
  • the phosphor particles contain nitride as a main component, and the nitride is CaAlSiN 3 or (Ca, Sr). AlSiN is 3.
  • the wavelength conversion member can provide light having high luminance and excellent color rendering.
  • the phosphor particle according to the fourteenth aspect of the present disclosure is a phosphor particle having a surface layer and containing aluminum.
  • the surface layer is a portion from which information on the composition can be obtained when energy dispersive X-ray analysis of the phosphor particles is performed at an acceleration voltage of 10.0 kV.
  • the molar ratio of aluminum atoms to all atoms in the surface layer is lower than the molar ratio of aluminum atoms to all atoms in the phosphor particle.
  • the molar ratio of aluminum atoms to all atoms in the surface layer of phosphor particles is relatively low. According to the phosphor particles, when the wavelength conversion member is manufactured, the phosphor particles are hardly exposed to the outside of the matrix. Therefore, the wavelength conversion member which has the outstanding heat dissipation can be provided.
  • the phosphor particle according to the fourteenth aspect further includes an alkaline earth metal. According to the fifteenth aspect, light having high brightness and excellent color rendering can be obtained.
  • a wavelength conversion member according to a sixteenth aspect of the present disclosure comprises phosphor particles and a matrix containing zinc oxide and surrounding the phosphor particles, and selected from the group consisting of (a) and (b) below: Meet at least one requirement.
  • the molar ratio of oxygen atom to atom is 20.0% or more.
  • the phosphor particles contain aluminum, and the phosphor particles have a molar ratio of aluminum atoms to all atoms obtained by performing energy dispersive X-ray analysis at an acceleration voltage of 10.0 kV. Less than the molar ratio of aluminum atoms to all atoms in the phosphor particles.
  • all phosphor particles of the wavelength conversion member according to the sixteenth aspect obtained by performing energy dispersive X-ray analysis with an acceleration voltage set at 10.0 kV.
  • the molar ratio of aluminum atoms to atoms is 20.0% or less.
  • the phosphor particle of the wavelength conversion member according to the sixteenth or seventeenth aspect contains nitride or oxynitride as a main component, and the acceleration voltage is 10.0 kV for the phosphor particle.
  • the molar ratio of nitrogen atoms to all atoms obtained by setting and performing energy dispersive X-ray analysis is 20.0% or less.
  • phosphor particles of the wavelength conversion member according to any one of the sixteenth to eighteenth aspects include silicon. Then, for the phosphor particles, the molar ratio of oxygen atoms to all atoms obtained by performing energy dispersive X-ray analysis with the acceleration voltage set at 10.0 kV, and the acceleration voltage for the phosphor particles The total with the molar ratio of silicon atoms to all atoms obtained by conducting energy dispersive X-ray analysis set at 10.0 kV is at least 55.0%.
  • the phosphor particles according to the twentieth aspect of the present disclosure are phosphor particles containing aluminum, and are obtained by performing energy dispersive X-ray analysis on phosphor particles while setting an acceleration voltage to 10.0 kV. Also, the molar ratio of aluminum atoms to all atoms is lower than the molar ratio of aluminum atoms to all atoms in the phosphor particle.
  • the wavelength conversion member 100 includes a substrate 10 and a phosphor layer 20.
  • the substrate 10 supports the phosphor layer 20.
  • the phosphor layer 20 is disposed on the substrate 10.
  • the phosphor layer 20 has a matrix 21 and phosphor particles 22.
  • a matrix 21 is present between each particle.
  • the phosphor particles 22 are embedded in the matrix 21. In other words, the phosphor particles 22 are dispersed in the matrix 21.
  • the phosphor particles 22 are surrounded by a matrix 21.
  • the wavelength conversion member 100 When the wavelength conversion member 100 is irradiated with excitation light having a first wavelength band, the wavelength conversion member 100 converts part of the excitation light into light having a second wavelength band and emits the light.
  • the wavelength conversion member 100 emits light having a wavelength longer than that of the excitation light.
  • the second wavelength band is a band different from the first wavelength band. However, a part of the second wavelength band may overlap the first wavelength band.
  • the light emitted from the wavelength conversion member 100 may include not only the light emitted from the phosphor particles 22 but also the excitation light itself.
  • the substrate 10 has a substrate body 11 and a thin film 12.
  • the thickness of the substrate 10 is, for example, larger than the thickness of the phosphor layer 20.
  • the substrate body 11 is selected from the group consisting of sapphire (Al 2 O 3 ), gallium nitride (GaN), aluminum nitride (AlN), silicon, aluminum, glass, quartz (SiO 2 ), silicon carbide (SiC) and zinc oxide Is made of one material.
  • the substrate body 11 is translucent to, for example, excitation light and light emitted from the phosphor particles 22.
  • the wavelength conversion member 100 can be suitably used for a transmissive light source. If the substrate 10 does not have translucency, the wavelength conversion member 100 can be used for a reflective light source.
  • the substrate body 11 may have a mirror-polished surface.
  • the surface of the substrate main body 11 may be covered with an antireflective film, a dichroic mirror, a metal reflective film, a reflective film, a protective film, or the like.
  • the antireflective film is a film for preventing reflection of excitation light.
  • the dichroic mirror can be constituted by a dielectric multilayer film.
  • the metal reflection film is a film for reflecting light, and is made of a metal material such as silver or aluminum.
  • the reflection increasing film may be constituted by a dielectric multilayer film.
  • the protective film may be a film for physically or chemically protecting these films.
  • the thin film 12 functions as a base layer for forming the phosphor layer 20.
  • the thin film 12 functions as a seed crystal in the crystal growth process of the matrix 21. That is, the thin film 12 is a single crystal thin film or a polycrystalline thin film.
  • the matrix 21 is composed of ZnO single crystal or ZnO polycrystal
  • the thin film 12 may be a ZnO single crystal thin film or a ZnO polycrystal thin film.
  • the substrate body 11 can exhibit the function of a seed crystal, the thin film 12 may be omitted.
  • the matrix 21 made of crystalline ZnO can be formed directly on the substrate body 11.
  • phosphor particles 22 are dispersed in a matrix 21.
  • the phosphor particles 22 are separated from one another. However, the phosphor particles 22 may be in contact with each other.
  • the phosphor particles 22 may be stacked like stone walls.
  • the phosphor particles 22 receive excitation light and emit fluorescence.
  • the phosphor particles 22 are made of a fluorescent material.
  • the phosphor particles 22 contain, for example, an alkaline earth metal.
  • the alkaline earth metal includes at least one selected from the group consisting of Be, Mg, Ca, Sr, Ba and Ra.
  • the phosphor particles 22 may further contain aluminum and may further contain silicon.
  • the phosphor particles 22 may further contain other elements different from alkaline earth metals, aluminum and silicon.
  • the phosphor particles 22 further include, for example, rare earths.
  • the rare earth functions as the luminescent center of the fluorescent material.
  • the rare earth includes, for example, at least one selected from the group consisting of Y, Ce, Eu and Tb.
  • the phosphor particles 22 may contain VO 4 3- as a luminescent center.
  • the phosphor particles 22 may contain at least one selected from the group consisting of nitrides, oxynitrides and oxides.
  • the nitride, oxynitride or oxide may contain an alkaline earth metal, aluminum, silicon, a rare earth or the like.
  • the phosphor particles 22 may contain nitride or oxynitride as a main component.
  • the “main component” means a component contained in the phosphor particles 22 in the largest proportion by weight.
  • the phosphor particles 22 may be substantially made of nitride or oxynitride. “Consisting essentially of” means excluding other components that alter the essential characteristics of the mentioned compound. However, the phosphor particles 22 may contain impurities in addition to the nitride or the oxynitride.
  • the nitrides are, for example, CaAlSiN 3 (CASN), (Ca, Sr) AlSiN 3 (SCASN), SrSi 6 N 8 , (Sr, Ba) YSi 4 N 7 , YSi 4 N 7 , (Ca, Sr, Ba) 2 Si 5 N 8 and at least one selected from the group consisting of CaSiN 2 .
  • the nitride may be CaAlSiN 3 or (Ca, Sr) AlSiN 3 .
  • the wavelength conversion member 100 can provide light having high luminance and excellent color rendering.
  • the oxynitride is, for example, (Sr, Ba) Al 2 Si 3 O 4 N 4 , Ba 3 Si 6 O 12 N 2 , YSiON, LaSiON, SrSi 9 Al 19 ON 31 , SrSiAl 2 O 3 N 2 , SrSi 5 AlO 2 N 7 , BaSi 2 O 2 N 2 , Sr 3 Si 13 Al 3 O 2 N 21 , Sr 5 Si 21 Al 5 O 2 N 35 , (Ca, Sr) Si 2 O 2 N 2 , AlON, M x Si 12- (m + n) Al m + n O n N 16-n ( ⁇ -sialon), Si 6-z Al z O z N 8-z ( ⁇ -sialon) and LaAl (Si 6-z Al z) A) at least one member selected from the group consisting of N 10-z O z (JEM phosphors); In ⁇ -sialon, M contains an element such as Ca.
  • ⁇ -sialon may be Ca x Si 12- (m + n) Al m + n O n N 16-n (Ca- ⁇ -sialon).
  • z satisfies 0 ⁇ z ⁇ 4.2.
  • the oxides are, for example, BaMgAl 10 O 17 , Ca 3 Sc 2 Si 3 O 12 , Ca 3 (Sc, Mg) 2 Si 3 O 12 , CaSc 2 O 4 , Ca (Sc, Mg) 2 O 4 , (Ca , Sr) Sc 2 O 4 , (Sr, Ba) 2 SiO 4 , MgAl 2 O 4 , Mg 2 TiO 4 , 3.5MgO ⁇ 0.5MgF 2 ⁇ GeO 2 , Mg 6 As 2 O 11 , Ca 5 (PO 5 4 ) 3 F, Ca 5 (PO 4 ) 3 (F, Cl), Sr 5 (PO 4 ) 3 F, MgO, CaO, MgGa 2 O 4 , Mg 4 Ta 2 O 9 , CaPO 3 , Ba 2 GdNbO 5 , (Sr, Mg) 2 P 2 O 7 , BaMg 2 Al 16 O 27 , BaMg (SO 4 ) 2 , SrBe 2 Si 2 O
  • the phosphor particles 22 may contain other compounds different from nitrides, oxynitrides and oxides.
  • the phosphor particles 22 are CaF 2 , KMgF 3 , MgS, CaS, SrS, BaS, Ba (F, Cl), BaAlF 5 , SrAlF 5 and (Mg, Ca, Ba) [Pt (CN) 4 ] .nH 2 At least one selected from the group consisting of O may be included.
  • composition formula contains at least one element selected from the plurality of listed elements in the compound Means to For example, the composition formula “(Ca, Sr) AlSiN 3 ” comprehensively shows “CaAlSiN 3 ”, “SrAlSiN 3 ” and “Ca 1 -y Sry AlSiN 3 ”. y satisfies 0 ⁇ y ⁇ 1.
  • composition formula of the compound exemplified as the material of the phosphor particle 22 the description of the light emission center is omitted.
  • composition formula “CaAlSiN 3 ” generically indicates “CaAlSiN 3 : Ce”, “CaAlSiN 3 : Eu”, and the like.
  • the phosphor particles 22 have a surface 25 and an interior 26.
  • the surface layer 25 is a portion from which information on the composition can be obtained when energy dispersive X-ray analysis (EDX) of the phosphor particles 22 is performed at an acceleration voltage of 10.0 kV.
  • EDX energy dispersive X-ray analysis
  • the inside 26 is a portion other than the surface layer 25 in the phosphor particle 22.
  • EDX can measure the elemental composition of the part of the object from the surface of the object to a specific position. Specifically, when the object is measured by EDX, electrons are incident on the object.
  • the elemental composition in the portion of the object from the surface of the object to the penetration depth of electrons incident on the object can be measured. That is, the surface layer 25 of the phosphor particle 22 is the phosphor particle 22 up to the penetration depth of the electrons incident on the phosphor particle 22 when performing EDX from the surface of the phosphor particle 22 by the acceleration voltage of 10.0 kV. It is a part.
  • EDX the relationship between the acceleration voltage V and the penetration depth Rs of electrons incident on the object is expressed by the following equation (1).
  • Rs represents the penetration depth ( ⁇ m) of electrons incident on the object.
  • A shows the average atomic weight (g / mol) of an object.
  • ⁇ indicates the average density (g / cc) of the object.
  • Z represents the average atomic number of the object.
  • V shows acceleration voltage (kV).
  • the acceleration voltage V is constant, the penetration depth Rs of electrons incident on the object changes in accordance with the composition of the object. That is, in FIG. 2, the distance r from the surface of the phosphor particle 22 to the inside 26 changes in accordance with the composition of the phosphor particle 22.
  • the distance r is 0.69 ⁇ m.
  • the surface layer 25 may be a portion of the phosphor particle 22 located at a distance of 0.7 ⁇ m from the surface of the phosphor particle 22.
  • the penetration depth Rs of electrons incident on the object may change depending on the shape of the object. As understood from the equation (1), the penetration depth Rs of electrons incident on the object increases as the acceleration voltage V increases.
  • the temperature around the object when performing EDX is, for example, normal temperature (Japanese Industrial Standard: 20 ° C. ⁇ 15 ° C./JIS Z8703). EDX is performed, for example, under a pressure of 4 Pa or less.
  • the surface layer 25 surrounds the interior 26.
  • the surface layer 25 is in contact with the inside 26.
  • the surface layer 25 has an elemental composition different from that of the inside 26.
  • the phosphor particles 22 contain nitride or oxynitride as a main component, and the molar ratio of oxygen atoms to all atoms in the surface layer 25 is 20.0% or more, (B) The phosphor particles 22 contain aluminum, and the molar ratio of aluminum atoms to all atoms in the surface layer 25 is lower than the molar ratio of aluminum atoms to all atoms in the phosphor particles 22. At least one of the more selected requirements is met.
  • the molar ratio of specific atoms to all atoms in the surface layer 25 is obtained for all of the phosphor particles 22 obtained by performing EDX with the acceleration voltage set to 10.0 kV. It means the molar ratio of a specific atom to an atom.
  • the molar ratio of oxygen atoms to all atoms in the surface layer 25 is higher than, for example, the molar ratio of oxygen atoms to all atoms in the phosphor particle 22.
  • the molar ratio of oxygen atoms to all atoms in the surface layer 25 is, for example, for all the atoms obtained by performing EDX with the accelerating voltage set to a value larger than 10.0 kV for the phosphor particles 22. Higher than the molar ratio of oxygen atoms.
  • the molar ratio of oxygen atoms to all atoms in the surface layer 25 may be in the range of 30.0 to 60.0%, and may be in the range of 39.1 to 48.3%.
  • the penetration depth Rs of electrons incident on the phosphor particles is larger as the acceleration voltage V is larger. That is, the larger the acceleration voltage V of EDX, the more the obtained elemental composition reflects the elemental composition of the entire phosphor particle. Therefore, whether the requirement (b) is satisfied can be determined by the following method. First, with respect to phosphor particles, EDX is performed by setting the acceleration voltage to 10.0 kV. Next, EDX is performed on the phosphor particles by setting the acceleration voltage to 15.0 kV.
  • the molar ratio of aluminum atoms to all atoms, which is obtained by performing EDX at an accelerating voltage of 10.0 kV is defined as X.
  • X is a molar ratio of aluminum atoms to all atoms in the surface layer of phosphor particles.
  • the molar ratio of aluminum atoms to all atoms, which is obtained by performing EDX at an acceleration voltage of 15.0 kV is defined as Y.
  • the value Z of (Y ⁇ X) / X is 0.045 or more, it can be considered that the requirement (b) is satisfied.
  • the value Z may be in the range of 0.126 to 0.222.
  • the method of determining whether requirement (b) is satisfied is not limited to the above method.
  • the molar ratio of aluminum atoms to all atoms in the surface layer 25 is, for example, for the phosphor particles 22, setting the acceleration voltage to a value larger than 10.0 kV and setting EDX to Lower than the molar ratio of aluminum atoms to all atoms obtained by carrying out.
  • the molar ratio of aluminum atoms to all atoms in the surface layer 25 is, for example, 20.0% or less.
  • the molar ratio of aluminum atoms to all atoms in the surface layer 25 may be 15.0% or less.
  • the molar ratio of aluminum atoms to all atoms in the surface layer 25 may be in the range of 2.7 to 13.5%.
  • the surface layer 25 may not contain an aluminum atom.
  • the molar ratio of aluminum atoms to all atoms in the surface layer 25 is lower than, for example, the molar ratio of oxygen atoms to all atoms in the surface layer 25.
  • the molar ratio of nitrogen atoms to all atoms in the surface layer 25 is, for example, the molar ratio of nitrogen atoms to all atoms in the phosphor particles 22 Lower than.
  • the molar ratio of nitrogen atoms to all atoms in the surface layer 25 is, for example, for all the atoms obtained by performing EDX with the accelerating voltage set to a value larger than 10.0 kV for the phosphor particles 22. Lower than the molar ratio of nitrogen atoms.
  • the molar ratio of nitrogen atoms to all atoms in the surface layer 25 is, for example, 20.0% or less.
  • the molar ratio of nitrogen atoms to all atoms in the surface layer 25 may be 15.0% or less.
  • the molar ratio of nitrogen atoms to all atoms in the surface layer 25 may be in the range of 4.5 to 12.3%.
  • the surface layer 25 may not contain a nitrogen atom.
  • the molar ratio of nitrogen atoms to all atoms in the surface layer 25 is lower than, for example, the molar ratio of oxygen atoms to all atoms in the surface layer 25.
  • the molar ratio of silicon atoms to all atoms in the surface layer 25 is higher than, for example, the molar ratio of silicon atoms to all atoms in the phosphor particles 22.
  • the molar ratio of silicon atoms to all the atoms in the surface layer 25 is, for example, for all the atoms obtained by performing EDX with the accelerating voltage set to a value larger than 10.0 kV for the phosphor particles 22. Higher than the molar ratio of silicon atoms.
  • the molar ratio of silicon atoms to all atoms in the surface layer 25 is, for example, 20.0% or more.
  • the molar ratio of silicon atoms to all atoms in the surface layer 25 may be in the range of 35.0 to 55.0%.
  • the molar ratio of silicon atoms to all atoms in the surface layer 25 is higher than the molar ratio of aluminum atoms to all atoms in the surface layer 25.
  • the molar ratio of silicon atoms to all atoms in the surface layer 25 is higher than the molar ratio of nitrogen atoms to all atoms in the surface layer 25.
  • the total of the molar ratio of oxygen atoms to all atoms in the surface layer 25 and the molar ratio of silicon atoms to all atoms in the surface layer 25 is, for example, 55.0% or more.
  • the sum of the molar ratio of oxygen atoms to all atoms in the surface layer 25 and the molar ratio of silicon atoms to all atoms in the surface layer 25 may be in the range of 66.6 to 92.3%.
  • the surface layer 25 may be substantially composed of oxygen atoms and silicon atoms.
  • the molar ratio of the alkaline earth metal to all atoms in the surface layer 25 is lower than, for example, the molar ratio of the alkaline earth metal to all atoms in the phosphor particle 22.
  • the molar ratio of the alkaline earth metal to all the atoms in the surface layer 25 is, for example, all of the phosphor particles 22 obtained by performing EDX with the acceleration voltage set to a value larger than 10.0 kV. Lower than the molar ratio of alkaline earth metal to atom.
  • the molar ratio of alkaline earth metal to all atoms in the surface layer 25 is, for example, 10.0% or less.
  • the molar ratio of the alkaline earth metal to all atoms in the surface layer 25 may be 3.0% or less.
  • the surface layer 25 may not contain an alkaline earth metal.
  • the average particle size of the phosphor particles 22 is, for example, larger than 1.4 ⁇ m.
  • the average particle diameter of the phosphor particles 22 is, for example, 50 ⁇ m or less.
  • the average particle size of the phosphor particles 22 can be identified, for example, by the following method. First, the cross section of the wavelength conversion member 100 is observed with a scanning electron microscope. In the obtained electron microscope image, the area of a specific phosphor particle 22 is calculated by image processing. The diameter of a circle having the same area as the calculated area is regarded as the particle size (diameter of the particle) of that specific phosphor particle 22.
  • the particle diameter of an arbitrary number (for example, 50) of phosphor particles 22 is calculated, and the average value of the calculated values is regarded as the average particle diameter of phosphor particles 22.
  • the method of measuring the average particle diameter is not limited to the method described above.
  • the average particle diameter of the phosphor particles 22 is a particle diameter (median diameter or D50) corresponding to 50% of the cumulative volume percentage in the particle size distribution measured by the laser diffraction / scattering type particle diameter / particle size distribution measuring apparatus. Good.
  • the shape of the phosphor particles 22 is not limited.
  • the shape of the phosphor particles 22 may be spherical, scaly, or fibrous.
  • the matrix 21 contains ZnO.
  • ZnO is suitable as the material of the matrix 21 in terms of transparency and thermal conductivity.
  • ZnO has high thermal conductivity. Therefore, when ZnO is used as the material of the matrix 21, the heat of the phosphor layer 20 can be easily dissipated to the outside (mainly the substrate 10).
  • the matrix 21 may contain ZnO as a main component.
  • the matrix 21 may be substantially made of ZnO. However, the matrix 21 may contain impurities in addition to ZnO.
  • ZnO as a material of the matrix 21 is a single crystal of ZnO or a polycrystalline of ZnO.
  • ZnO has a wurtzite crystal structure.
  • the matrix 21 is formed by crystal growth, the matrix 21 has, for example, a crystal structure corresponding to the crystal structure of the thin film 12. That is, when the polycrystal of ZnO oriented to the c axis is used as the thin film 12, the matrix 21 has the polycrystal of ZnO oriented to the c axis.
  • the “c-axis oriented ZnO” means that a plane parallel to the main surface (the surface having the largest area) of the substrate 10 is the c-plane.
  • the ZnO polycrystal oriented in the c-axis contains a plurality of columnar crystal grains oriented in the c-axis. There are few crystal grain boundaries in the c-axis direction in ZnO polycrystalline oriented in the c-axis. “The columnar crystal grains are oriented in the c-axis” means that the growth of ZnO in the c-axis direction is faster than the growth of ZnO in the a-axis direction, and longitudinally elongated ZnO crystal grains are formed on the substrate 10 Means to The c-axis of the ZnO crystal grain is parallel to the normal direction of the substrate 10.
  • ZnO is a c-axis oriented crystal
  • XRD measurement (2 ⁇ / ⁇ scan).
  • ZnO is a crystal with c-axis orientation It can be determined that there is.
  • the phosphor layer 20 may further have filler particles.
  • filler particles are dispersed in the matrix 21. When the filler particles are irradiated with excitation light, the filler particles do not emit fluorescent light or emit only fluorescent light of negligible intensity.
  • the material, shape and addition amount of the filler particles are appropriately adjusted according to the required chromaticity.
  • the filler particles are, for example, inorganic particles, and typically contain metal oxides.
  • the filler particles may consist essentially of metal oxides. Many of the metal oxides are suitable as filler particle materials because they are chemically stable and emit little fluorescence.
  • the filler particles include at least one selected from Al 2 O 3 particles, SiO 2 particles, and TiO 2 particles.
  • the average particle size of the filler particles is, for example, in the range of 0.1 to 20 ⁇ m.
  • the average particle size of the filler particles is smaller than, for example, the average particle size of the phosphor particles 22.
  • the ratio (D2 / D1) of the average particle diameter D2 of the filler particles to the average particle diameter D1 of the phosphor particles 22 is, for example, in the range of 0.01 to 0.90.
  • the average particle size of the filler particles can be measured by the same method as the average particle size of the phosphor particles 22.
  • the shape of the filler particles may be spherical, scaly, or fibrous.
  • the volume of the phosphor particles 22 is defined as V1.
  • the volume of the filler particles is defined as V2. At this time, the value of V2 / (V1 + V2) is, for example, in the range of 0.1 to 0.9.
  • phosphor particles 22 are produced.
  • conventional phosphor particles are prepared.
  • Conventional phosphor particles are treated with acid.
  • some elements contained in the surface layer of the conventional phosphor particles are removed.
  • the elements remaining on the surface layer of the phosphor particles are oxidized by the acid. Therefore, the molar ratio of oxygen atoms to all atoms in the surface layer is increased.
  • phosphor particles 22 are obtained.
  • a commercially available thing can be used as a conventional fluorescent substance particle.
  • the acid is not particularly limited as long as the phosphor particles 22 can be produced.
  • the acid may be a strong acid.
  • the acid is, for example, an aqueous acid solution.
  • the concentration of the acid in the aqueous acid solution is, for example, in the range of 0.1 to 20.0 mol / L.
  • the acid may be a boiling aqueous nitric acid solution.
  • the phosphor particles 22 can be produced by bringing the conventional phosphor particles into contact with a boiling nitric acid aqueous solution.
  • the concentration of nitric acid in the aqueous solution of boiling nitric acid is, for example, 15.6 mol / L.
  • the boiling nitric acid aqueous solution may be in contact with the entire surface of the conventional phosphor particles. At this time, the surface layer 25 of the obtained phosphor particles 22 has a uniform elemental composition.
  • the atmospheric pressure at which the conventional phosphor particles and the boiled nitric acid aqueous solution are brought into contact with each other is, for example, 1 atm.
  • the time for which the conventional phosphor particles and the boiling nitric acid aqueous solution are brought into contact with each other is, for example, in the range of 5 to 300 minutes.
  • the substrate 10 is prepared.
  • a crystalline ZnO thin film is formed on the substrate body 11 as the thin film 12.
  • vapor phase film forming methods such as vapor deposition method, electron beam vapor deposition method, reactive plasma vapor deposition method, ion assisted vapor deposition method, sputtering method, pulse laser deposition method and the like are used.
  • the thin film 12 may be formed by the following method. First, a sol containing a precursor such as zinc alkoxide is prepared. The sol is applied to the substrate body 11 by a printing method to form a coating film. Next, the thin film 12 is obtained by heat-treating the coating film.
  • the thin film 12 may be a ZnO single crystal thin film or a ZnO polycrystalline thin film.
  • a layer containing phosphor particles 22 is formed on the substrate 10 (on the thin film 12).
  • a dispersion containing phosphor particles 22 is prepared.
  • the substrate 10 is placed in the dispersion and the phosphor particles 22 are deposited on the substrate 10 using electrophoresis.
  • the layer containing the phosphor particles 22 can be formed on the substrate 10.
  • a layer containing the phosphor particles 22 can also be formed on the substrate 10 using a coating solution containing the phosphor particles 22 by a thin film forming method such as a printing method.
  • a matrix 21 is formed between the plurality of phosphor particles 22.
  • a solution growth method using a solution containing Zn ions can be used.
  • Solution growth methods include chemical bath deposition under atmospheric pressure, hydrothermal synthesis under superatmospheric pressure, electrolytic deposition with voltage or current applied ( electrochemical deposition) and the like are used.
  • a solution for crystal growth for example, an aqueous solution of zinc nitrate containing hexamethylenetetramine is used.
  • a crystalline matrix 21 is epitaxially grown on the thin film 12. Thus, the phosphor layer 20 is obtained.
  • elements contained in phosphor particles may be eluted in a solution for crystal growth.
  • metals having a higher ionization tendency than Zn elute into a solution for crystal growth.
  • metals having a larger ionization tendency than Zn include alkaline earth metals, aluminum and the like.
  • the elements eluted in the solution for crystal growth may react with chemical species contained in the solution for crystal growth. This reaction may form a complex oxide containing an element eluted in a solution for crystal growth.
  • the surface layer 25 of the phosphor particles 22 has an elemental composition different from that of the inside 26.
  • the elemental composition of the interior 26 is almost the same as the elemental composition of the conventional phosphor particles before being treated with acid.
  • the molar ratio of oxygen atoms to all atoms in the surface layer 25 of the phosphor particles 22 is relatively high, or the molar ratio of aluminum atoms to all atoms in the surface layer 25 is relatively low. Therefore, when the phosphor particles 22 come in contact with the solution for crystal growth, the metal contained in the phosphor particles 22 hardly elutes in the solution for crystal growth. That is, in the phosphor particles 22, the surface layer 25 functions as a passive state.
  • the metal contained in the phosphor particles 22 hardly elutes in the solution for crystal growth, the formation of the complex oxide can be suppressed. At this time, zinc oxide can be easily crystal-grown. Therefore, the phosphor particles 22 can be easily surrounded by the matrix 21. Thereby, the wavelength conversion member 100 which has the outstanding heat dissipation is obtained.
  • the light source 200 of the present embodiment includes the wavelength conversion member 100 and the light emitting element 51.
  • the light emitting element 51 emits excitation light.
  • the wavelength conversion member 100 is disposed on the optical path of the excitation light emitted from the light emitting element 51.
  • the phosphor layer 20 of the wavelength conversion member 100 is located between the light emitting element 51 and the substrate 10 of the wavelength conversion member 100.
  • the light source 200 is a reflective light source.
  • the light emitting element 51 is typically a semiconductor light emitting element.
  • the semiconductor light emitting element is, for example, a light emitting diode (LED), a super luminescent diode (SLD) or a laser diode (LD).
  • the light emitting element 51 may be configured by one LD or may be configured by a plurality of LDs.
  • the plurality of LDs may be optically coupled.
  • the light emitting element 51 emits, for example, blue-violet light.
  • blue-violet light is light having a peak wavelength in the range of 380-420 nm.
  • the light source 200 further includes an optical system 50.
  • the optical system 50 may be located on the optical path of the excitation light emitted from the light emitting element 51.
  • the optical system 50 includes optical components such as a lens, a mirror, and an optical fiber.
  • the light source 210 of the present embodiment includes the wavelength conversion member 100 and the light emitting element 51.
  • the light emitting element 51 faces the substrate 10 of the wavelength conversion member 100.
  • the light of the light emitting element 51 passes through the substrate 10 and reaches the phosphor layer 20.
  • the light source 210 is a transmissive light source.
  • the illumination device 300 of the present embodiment includes a light source 200 and an optical component 55.
  • the optical component 55 is a component for guiding light emitted from the light source 200 to the front, and more specifically, is a reflector.
  • the optical component 55 has, for example, a metal film of Al, Ag or the like or an Al film in which a protective film is formed on the surface.
  • a filter 56 may be provided in front of the light source 200. The filter 56 absorbs or scatters the blue light so that the coherent blue light from the light emitting element of the light source 200 does not go out directly.
  • the lighting device 300 may be a so-called reflector type or a projector type.
  • the lighting device 300 is, for example, a headlamp for a vehicle.
  • [Phosphor particles] (Sample 1) First, conventional phosphor particles (made by DENKA) made of CaAlSiN 3 : Eu were prepared. The phosphor particles were added to the boiling aqueous nitric acid solution. The concentration of nitric acid in the aqueous nitric acid solution was 15.6 mol / L. Next, the boiling nitric acid aqueous solution was stirred for 30 minutes. The phosphor particles were removed from the aqueous nitric acid solution. Thus, phosphor particles of sample 1 were obtained. The average particle size (median diameter) of the phosphor particles of sample 1 was 12.3 ⁇ m.
  • Example 2 By the same method as Sample 1 except that the conventional phosphor particles (made by DENKA) made of (Ca, Sr) AlSiN 3 : Eu were used instead of the conventional phosphor particles made of CaAlSiN 3 : Eu , And phosphor particles of sample 2 were obtained.
  • the average particle size (median diameter) of the phosphor particles of sample 2 was 10.7 ⁇ m.
  • the vertical axes in FIG. 6A, FIG. 6B, and FIGS. 7A to 9B shown below indicate signal intensities.
  • the unit of the vertical axis is an arbitrary unit.
  • the elemental composition was calculated based on the obtained spectrum.
  • the relationship between the accelerating voltage and the elemental composition is shown in Table 1.
  • EDX of Measurement Example 2 was performed by the same method as Measurement Example 1 except that the phosphor particles of Sample 1 were used instead of the conventional phosphor particles made of CaAlSiN 3 : Eu.
  • the EDX spectra obtained when the accelerating voltage is 5.0 kV and 10.0 kV are shown in FIGS. 7A and 7B, respectively.
  • the elemental composition was calculated based on the obtained spectrum. The relationship between the accelerating voltage and the elemental composition is shown in Table 1.
  • Measurement example 3 Measurement Example 3 by the same method as Measurement Example 1 except that the conventional phosphor particles made of (Ca, Sr) AlSiN 3 : Eu were used instead of the conventional phosphor particles made of CaAlSiN 3 : Eu Did the EDX.
  • the EDX spectra obtained when the accelerating voltage is 5.0 kV and 10.0 kV are shown in FIGS. 8A and 8B, respectively.
  • the elemental composition was calculated based on the obtained spectrum. The relationship between the accelerating voltage and the elemental composition is shown in Table 2.
  • EDX of Measurement Example 4 was performed by the same method as that of Measurement Example 1 except that the phosphor particles of Sample 2 were used instead of the conventional phosphor particles made of CaAlSiN 3 : Eu.
  • the EDX spectra obtained when the accelerating voltage is 5.0 kV and 10.0 kV are shown in FIGS. 9A and 9B, respectively.
  • the elemental composition was calculated based on the obtained spectrum. The relationship between the accelerating voltage and the elemental composition is shown in Table 2.
  • the elemental composition of the phosphor particles obtained when the acceleration voltage is set to 10.0 kV corresponds to the elemental composition in the surface layer of the phosphor particles.
  • the part where information on the composition is obtained when EDX of the phosphor particles is performed at an acceleration voltage of 5.0 kV may be expressed as “the outermost layer”.
  • the outermost layer of the phosphor particles corresponds to a part of the surface of the phosphor particles.
  • the elemental composition in the outermost layer of the phosphor particle reflects the elemental composition in the vicinity of the surface of the phosphor particle more than the elemental composition in the surface layer of the phosphor particle.
  • oxygen atoms were detected in the surface layer of the conventional phosphor particle made of CaAlSiN 3 : Eu.
  • the molar ratio (28.4%) of oxygen atoms in the outermost layer of the phosphor particles largely exceeded the molar ratio (18.1%) of oxygen atoms in the surface layer of the phosphor particles.
  • calcium atoms were not detected in the outermost layer of the conventional phosphor particles made of CaAlSiN 3 : Eu. From the above, it is presumed that an oxide film formed by natural oxidation of phosphor particles is present on the surface of a conventional phosphor particle made of CaAlSiN 3 : Eu.
  • the elemental composition in the surface layer of the phosphor particles was changed.
  • the elemental composition inside the phosphor particles hardly changes. That is, the elemental composition of the entire phosphor particles of Samples 1 and 2 is almost the same as the elemental composition of the entire conventional phosphor particles before treatment.
  • the elemental composition of the whole conventional phosphor particle is almost the same as the elemental composition in the surface layer of the conventional phosphor particle. Therefore, the elemental composition of the entire phosphor particles of Samples 1 and 2 is also almost the same as the elemental composition of the surface layer of the conventional phosphor particle before the treatment.
  • the molar ratio of oxygen atoms to all atoms in the surface layer of a conventional phosphor particle made of CaAlSiN 3 : Eu was 18.1%.
  • the molar ratio of oxygen atoms to all atoms in the surface layer of the phosphor particle of sample 1 was 39.1%. That is, by treating the phosphor particles with an acid, the molar ratio of oxygen atoms to all atoms in the surface layer was increased.
  • the molar ratio of oxygen atoms to all atoms (39.1%) in the surface layer of the phosphor particles of sample 1 is the molar ratio of oxygen atoms to all atoms in the phosphor particles of sample 1 (about 18.1% Higher than).
  • the molar ratio of aluminum atoms to all atoms in the surface layer of a conventional phosphor particle made of CaAlSiN 3 : Eu was 25.0%.
  • the molar ratio of aluminum atoms to all the atoms in the surface layer of the phosphor particles of sample 1 was 13.5%. That is, by treating the phosphor particles with an acid, the molar ratio of aluminum atoms to all atoms in the surface layer was reduced.
  • the molar ratio of aluminum atoms to all atoms (13.5%) in the surface layer of the phosphor particles of sample 1 is the molar ratio of aluminum atoms to all atoms in the phosphor particles of sample 1 (about 25.0% Lower than).
  • the molar ratio of aluminum atoms to all atoms (25.0%) in the surface layer of a conventional phosphor particle made of CaAlSiN 3 : Eu is the molar ratio of silicon atoms to all atoms in the surface layer of the phosphor particle It was higher than (16.2%).
  • the molar ratio (13.5%) of aluminum atoms to all atoms in the surface layer of the phosphor particles of sample 1 is the molar ratio of silicon atoms to all atoms in the surface layer of the phosphor particles Lower than 27.5%). That is, by treating the phosphor particles with an acid, the magnitude relationship between the molar ratio of aluminum atoms to all atoms in the surface layer and the molar ratio of silicon atoms to all atoms in the surface layer changed.
  • the molar ratio of oxygen atoms to all atoms in the surface layer of the conventional phosphor particles made of (Ca, Sr) AlSiN 3 : Eu was 19.2%.
  • the molar ratio of oxygen atoms to all the atoms in the surface layer of the phosphor particles of sample 2 was 48.3%.
  • the molar ratio of oxygen atoms to all atoms (48.3%) in the surface layer of the phosphor particles of sample 2 is the molar ratio of oxygen atoms to all atoms in the phosphor particles of sample 2 It was higher than (about 19.2%).
  • the molar ratio of aluminum atoms to all atoms in the surface layer of a conventional phosphor particle made of (Ca, Sr) AlSiN 3 : Eu was 21.4%.
  • the molar ratio of aluminum atoms to all the atoms in the surface layer of the phosphor particles of sample 2 was 2.7%.
  • the molar ratio of aluminum atoms to all atoms (2.7%) in the surface layer of the phosphor particles of sample 2 is the molar ratio of aluminum atoms to all atoms in the phosphor particles of sample 2 Lower than (about 21.4%).
  • Example 1 The wavelength conversion member provided with the phosphor particles of Sample 1 was produced by the following method. First, a crystalline ZnO thin film was formed on the substrate body. As a substrate body, an Ag mirror with a protective film (manufactured by Keihin Light Film Industry Co., Ltd.) was used. The phosphor particles of sample 1 were placed on the ZnO thin film. Next, a crystalline ZnO matrix was produced on the ZnO thin film by a solution growth method. As a solution for crystal growth, an aqueous solution of zinc nitrate containing hexamethylenetetramine was used. The concentration of hexamethylenetetramine in the aqueous solution was 0.10 mol / L. The concentration of zinc nitrate in the aqueous solution was 0.10 mol / L. Thus, the wavelength conversion member of Example 1 was obtained.
  • a crystalline ZnO thin film was formed on the substrate body.
  • an Ag mirror with a protective film manufactured by Keihin Light Film
  • Comparative example 1 A wavelength conversion member of Comparative Example 1 was obtained by the same method as Example 1, except that the conventional phosphor particles made of CaAlSiN 3 : Eu were used instead of the phosphor particles of Sample 1.
  • the wavelength conversion member of the present disclosure can be used, for example, as a light source in a general illumination device such as a ceiling light.
  • the wavelength conversion member of this indication can be utilized for the light source in special illuminating devices, such as a spotlight, illumination for stadiums, and illumination for studios, for example.
  • the wavelength conversion member of this indication can be utilized for the light source in the illuminating devices for vehicles, such as a headlamp, for example.
  • the wavelength conversion member of this indication can be utilized for the light source in projection apparatuses, such as a projector and a head-up display, for example.
  • the wavelength conversion member of the present disclosure can be used, for example, as a light source for medical or industrial endoscope light; an imaging device such as a digital camera, a cellular phone, or a smartphone.
  • the wavelength conversion member of the present disclosure is, for example, a light source in a monitor for a personal computer (PC), a notebook personal computer, a television, a portable information terminal (PDX), a smartphone, a tablet PC, a liquid crystal display device such as a mobile phone, It can be used. That is, the wavelength conversion member of the present disclosure is industrially useful.
  • the method of manufacturing the light source, the phosphor particle, and the wavelength conversion member of the present disclosure is also industrially useful.

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Abstract

L'invention concerne un élément de conversion en longueur d'onde qui présente des propriétés supérieures de dissipation de la chaleur. L'élément de conversion en longueur d'onde (100) selon la présente invention comprend une matrice (21) et des particules à corps fluorescents (22) ayant chacune une couche de surface. La couche de surface est une partie à partir de laquelle sont obtenues des informations concernant la composition par spectroscopie par rayons X à dispersion d'énergie des particules à corps fluorescents (22) à une tension d'accélération de 10,0 kV. L'élément de conversion en longueur d'onde (100) satisfait à au moins une exigence choisie dans le groupe constitué par : (a) les particules à corps fluorescents (22) contiennent un nitrure ou un nitrure d'acide utilisé comme constituant principal, et le rapport molaire entre les atomes d'oxygène et l'ensemble des atomes dans la couche de surface est supérieur ou égal à 20,0 % ; et (b) les particules à corps fluorescents (22) contiennent de l'aluminium, et le rapport molaire entre les atomes d'aluminium et l'ensemble des atomes dans la couche de surface est inférieur au rapport molaire entre les atomes d'aluminium et l'ensemble des atomes dans les particules à corps fluorescents (22).
PCT/JP2018/033524 2017-09-28 2018-09-11 Élément de conversion en longueur d'onde, source lumineuse, particules à corps fluorescents et procédé de production d'élément de conversion en longueur d'onde WO2019065194A1 (fr)

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