WO2017073329A1 - 波長変換部材の製造方法 - Google Patents

波長変換部材の製造方法 Download PDF

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WO2017073329A1
WO2017073329A1 PCT/JP2016/080255 JP2016080255W WO2017073329A1 WO 2017073329 A1 WO2017073329 A1 WO 2017073329A1 JP 2016080255 W JP2016080255 W JP 2016080255W WO 2017073329 A1 WO2017073329 A1 WO 2017073329A1
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wavelength conversion
conversion member
producing
glass powder
member according
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PCT/JP2016/080255
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English (en)
French (fr)
Japanese (ja)
Inventor
民雄 安東
忠仁 古山
俊輔 藤田
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日本電気硝子株式会社
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Priority to JP2017547720A priority Critical patent/JPWO2017073329A1/ja
Priority to CN201680061905.7A priority patent/CN108140702A/zh
Priority to KR1020177035955A priority patent/KR20180075434A/ko
Publication of WO2017073329A1 publication Critical patent/WO2017073329A1/ja

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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B11/00—Pressing molten glass or performed glass reheated to equivalent low viscosity without blowing
    • 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
    • C03C12/00—Powdered glass; Bead compositions
    • 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
    • C03C3/00—Glass compositions
    • C03C3/12—Silica-free oxide glass compositions
    • C03C3/16—Silica-free oxide glass compositions containing phosphorus
    • C03C3/19—Silica-free oxide glass compositions containing phosphorus containing boron
    • 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
    • C03C3/00—Glass compositions
    • C03C3/12—Silica-free oxide glass compositions
    • C03C3/16—Silica-free oxide glass compositions containing phosphorus
    • C03C3/21—Silica-free oxide glass compositions containing phosphorus containing titanium, zirconium, vanadium, tungsten or molybdenum
    • 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
    • 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
    • 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
    • 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
    • H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
    • H01L33/502—Wavelength conversion materials
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2933/00—Details relating to devices covered by the group H01L33/00 but not provided for in its subgroups
    • H01L2933/0008—Processes
    • H01L2933/0033—Processes relating to semiconductor body packages
    • H01L2933/0041—Processes relating to semiconductor body packages relating to wavelength conversion elements

Definitions

  • the present invention relates to a method for producing a wavelength conversion member using inorganic nanophosphor particles.
  • Inorganic nanophosphor particles have the property of being easily deteriorated when they come into contact with moisture or oxygen in the atmosphere. For this reason, the inorganic nanophosphor particles are used by being sealed with a resin or the like so as not to contact the external environment.
  • a resin is used as the sealing material, there is a problem that the resin is discolored by heat generated from the inorganic nanophosphor particles when irradiated with excitation light. Further, since the resin is inferior in water resistance and easily penetrates moisture, there is a problem that the inorganic nanophosphor particles are likely to deteriorate over time. Then, using glass excellent in heat resistance and water resistance is examined as a sealing material of inorganic nano fluorescent substance particles (for example, refer to patent documents 4).
  • the inorganic nanophosphor particles When sealing the inorganic nanophosphor particles with glass, it is necessary to perform heat treatment near the yield point (or softening point) of the glass. However, since the inorganic nanophosphor particles have low heat resistance, there is a problem that the luminous efficiency deteriorates due to deterioration during heat treatment.
  • an object of the present invention is to provide a method for producing a wavelength conversion member capable of suppressing thermal degradation of inorganic nanophosphor particles.
  • the method for producing a wavelength conversion member of the present invention is characterized in that a mixture containing glass powder and inorganic nanophosphor particles is sintered by hot pressing using a mold.
  • the softening flow of the glass powder is promoted, and it becomes possible to sinter in an extremely short time. Therefore, the thermal energy applied to the inorganic nanophosphor particles during sealing can be greatly suppressed. As a result, in the present invention, it is possible to remarkably suppress the thermal deterioration of the inorganic nanophosphor particles during the production of the wavelength conversion member. Moreover, according to this invention, a thin wavelength conversion member can be manufactured easily.
  • the method for producing a wavelength conversion member of the present invention it is preferable to heat-press the mixture after drying. If it does in this way, the quantum efficiency of a wavelength conversion member can be raised.
  • the reason is explained as follows. According to the inventors' investigation, when the inorganic nanophosphor particles and the glass powder are mixed, the water adhering to the surface of the glass powder reacts with the inorganic nanophosphor particles, and the inorganic nanophosphor particles deteriorate, It turned out that it becomes the cause of the quantum efficiency fall of a wavelength conversion member. Therefore, by previously drying the mixture by heating and removing the water adhering to the glass powder surface, it is possible to suppress the degradation of the inorganic nanophosphor particles and improve the quantum efficiency of the wavelength conversion member.
  • the glass powder is dried by heating and then mixed with inorganic nanophosphor particles to obtain a mixture. Also by this method, it is possible to suppress the deterioration of the inorganic nanophosphor particles due to the moisture adhering to the surface of the glass powder, so that the quantum efficiency of the wavelength conversion member can be improved.
  • the temperature during heat drying is preferably 50 to 200 ° C.
  • the pressure at the time of a hot press is 10 kPa / cm ⁇ 2 > or more.
  • the method for producing a wavelength conversion member of the present invention it is preferable to perform heating press at 400 ° C. or lower. If it does in this way, it will become easy to control degradation of inorganic nano fluorescent substance particles at the time of hot press. Note that general inorganic nanophosphor particles (particularly quantum dot phosphors) are deteriorated by heat exceeding 350 ° C. and light emission efficiency is lowered, but the substrate can be fused by a heating press in a relatively short time. Therefore, it is possible to suppress a decrease in the light emission efficiency of the inorganic nanophosphor particles.
  • the heating press time is 0.1 to 10 minutes. If it does in this way, it will become easy to control degradation of inorganic nano fluorescent substance particles at the time of hot press.
  • the yield point of the glass powder is preferably 380 ° C. or lower. If it does in this way, it will become easy to control degradation of inorganic nano fluorescent substance particles at the time of hot press.
  • the glass powder is preferably Sn—P glass powder or Sn—PF glass glass powder. Since Sn-P glass powder and Sn-PF glass powder can easily lower the yield point, sealing at a relatively low temperature is possible.
  • the Sn—P-based glass powder contains 50% to 80% SnO, 15% to 25% P 2 O 5 (however, does not include 25%), and 0 to 3% ZrO 2.
  • the Sn—PF glass glass powder is cation%, Sn 2+ 10 to 90%, P 5+ 10 to 70%, anion%, O 2 ⁇ 30 to 99.99. It is preferable to contain 9% and F ⁇ 0.1 to 70%.
  • the average particle diameter of the glass powder is preferably 0.1 to 100 ⁇ m.
  • the average particle diameter refers to a value (D50) measured according to JIS-R1629.
  • the inorganic nanophosphor particles are made of CdS, CdSe, CdTe, ZnS, ZnSe, ZnTe, InP, GaN, GaAs, GaP, AlN, AlP, AlSb, InN, InAs, and InSb. It is preferably a quantum dot phosphor composed of at least one selected or a composite of two or more of these.
  • the inorganic nanophosphor particles are inorganic particles composed of at least one selected from oxides, nitrides, oxynitrides, sulfides, oxysulfides, rare earth sulfides, aluminate chlorides, and halophosphates. It may be.
  • the wavelength conversion member of the present invention is a plate-like wavelength conversion member made of a sintered body of a mixture containing glass powder and inorganic nanophosphor particles, and has a porous layer at the periphery.
  • the wavelength conversion member when the wavelength conversion member is produced by sealing the inorganic nanophosphor particles in glass, it is possible to suppress thermal degradation of the inorganic nanophosphor particles.
  • Drawing 1 is a typical sectional view showing the manufacturing process of the wavelength conversion member concerning one embodiment of the present invention.
  • a mixture 1 containing glass powder and inorganic nanophosphor particles is prepared.
  • the mixture 1 is preformed into a cylindrical shape, a rectangular parallelepiped shape, or the like by press molding or the like as necessary.
  • the mixture 1 is placed between the upper mold 2a and the lower mold 2b in the mold 2.
  • pressure P is applied to the upper mold 2a to perform heat pressing.
  • the glass powder in the mixture 1 is softened and fluidized and sintered to obtain a plate-like (disc-like, rectangular plate-like) wavelength conversion member 3.
  • the porous layer 3a can be formed in the peripheral part of the wavelength conversion member 3 with manufacturing conditions. It is considered that this is because the peripheral edge of the mixture 1 spreads out in the horizontal direction at the time of hot pressing, so that the press pressure is less likely to be applied than the central portion of the mixture 1. Since the porous layer 3a has high reflection characteristics due to the difference in refractive index between the pores and the glass powder, leakage of light from the peripheral edge of the wavelength conversion member 3 is suppressed. Therefore, when the excitation light is irradiated from the main surface of the wavelength conversion member 3, the light extraction efficiency from the other main surface is easily improved.
  • the yield point of the glass powder is preferably 380 ° C. or lower, 300 ° C. or lower, particularly 200 ° C. or lower. If the yield point of the glass powder is too high, the heating press temperature is increased accordingly, and the inorganic nanophosphor particles are likely to deteriorate.
  • the lower limit of the yield point of the glass powder is not particularly limited, but is practically 100 ° C. or higher, particularly 120 ° C. or higher.
  • the yield point refers to the point at which the test piece showed the maximum elongation in the measurement with the thermal expansion coefficient measurement (TMA) apparatus, that is, the value at which the elongation of the test piece stopped.
  • glass based on Sn and P such as Sn—P glass, Sn—P—B glass, Sn—PF glass, etc. having a low yield point is preferable. Among these, it is preferable to use Sn—PF glass which can easily lower the yield point.
  • Sn—PF glass which can easily lower the yield point.
  • Sn 2+ is a component that improves chemical durability and weather resistance. It also has the effect of lowering the yield point.
  • the Sn 2+ content is preferably 10 to 90%, 20 to 85%, particularly 25 to 82.5%. When the content of Sn 2+ is too small, the above effect is difficult to obtain. On the other hand, when there is too much content of Sn2 + , it will become difficult to vitrify or devitrification resistance will fall easily.
  • P 5+ is a constituent component of the glass skeleton. Moreover, it has the effect of increasing the light transmittance. It also has the effect of suppressing devitrification and lowering the yield point.
  • the content of P 5+ is preferably 10 to 70%, 15 to 60%, particularly preferably 20 to 50%. When there is too little content of P5 + , the said effect will become difficult to be acquired. On the other hand, when the content of P 5+ is too large, the content of Sn 2+ is relatively low, the weather resistance tends to lower.
  • the content of P 5+ and Sn 2+ is preferably 50% or more, 70.5% or more, 75% or more, 80% or more, and particularly preferably 85% or more. When the content of P 5+ and Sn 2+ is too small, devitrification resistance and mechanical strength tends to decrease.
  • the upper limit of the content of P 5+ and Sn 2+ is not particularly limited and may be 100%. However, when other components are contained, they are 99.9% or less, 99% or less, 95% or less, and further 90%. % Or less.
  • the following components can be contained as the cationic component.
  • B 3+ , Zn 2+ , Si 4+ and Al 3+ are components of the glass skeleton, and have a particularly large effect of improving chemical durability.
  • the content of B 3+ + Zn 2+ + Si 4+ + Al 3+ is preferably 0 to 50%, 0 to 30%, 0.1 to 25%, 0.5 to 20%, particularly preferably 0.75 to 15%.
  • the content of B 3+ + Zn 2+ + Si 4+ + Al 3+ is too large, the devitrification resistance tends to decrease. Moreover, Sn metal etc. precipitate with a raise of melting temperature, and light transmittance becomes easy to fall. Also, the yield point tends to rise. From the viewpoint of improving the weather resistance, it is preferable to contain 0.1% or more of B 3+ + Zn 2+ + Si 4+ + Al 3+ .
  • the preferable content range of each component of B 3+ , Zn 2+ , Si 4+ and Al 3+ is as follows.
  • B 3+ is a component constituting the glass skeleton. Moreover, there exists an effect which improves a weather resistance, and especially the effect which suppresses that components, such as P5 + in glass, elute selectively into water is large.
  • the content of B 3+ is preferably 0 to 50%, 0.1 to 45%, particularly preferably 0.5 to 40%. When there is too much content of B3 + , there exists a tendency for devitrification resistance and a light transmittance to fall.
  • Zn 2+ is a component that acts as a flux. Moreover, there exists an effect which improves a weather resistance, suppresses the elution of the glass component in various washing
  • Si 4+ is a component constituting a glass skeleton. Moreover, there exists an effect which improves a weather resistance, and especially the effect which suppresses that components, such as P5 + in glass, elute selectively into water is large.
  • the content of Si 4+ is preferably 0 to 20%, particularly preferably 0.1 to 15%. When the content of Si 4+ is too large, the yield point tends to be high. In addition, striae and bubbles due to undissolved are likely to remain in the glass.
  • Al 3+ is a component capable of constituting a glass skeleton together with Si 4+ and B 3+ . Moreover, there exists an effect which improves a weather resistance, and especially the effect which suppresses that components, such as P5 + in glass, elute selectively into water is large.
  • the content of Al 3+ is preferably 0 to 20%, particularly preferably 0.1 to 15%. When there is too much content of Al3 + , there exists a tendency for devitrification resistance and a light transmittance to fall. Further, the melting temperature is increased, and striae and bubbles due to undissolution are likely to remain in the glass.
  • Mg 2+ , Ca 2+ , Sr 2+ and Ba 2+ are components that act as fluxes. Moreover, there exists an effect which improves a weather resistance, suppresses the elution of the glass component in various washing
  • Li + is a component having the greatest effect of lowering the yield point among alkali metal oxides.
  • Li + has a strong phase separation property, if its content is too large, the devitrification resistance tends to decrease.
  • Li + tends to reduce chemical durability and light transmittance. Accordingly, the Li + content is preferably 0 to 10%, 0 to 5%, 0 to 1%, particularly preferably 0 to 0.1%.
  • Na + has the effect of lowering the yield point in the same manner as Li + .
  • the Na + content is preferably 0 to 10%, 0 to 5%, 0 to 1%, particularly preferably 0 to 0.1%.
  • K + also has the effect of lowering the yield point in the same way as Li + .
  • the content of K 2 O is preferably 0 to 10%, 0 to 5%, 0 to 1%, particularly 0 to 0.1%.
  • Li + , Na + and K + are preferably 0 to 10%, 0 to 5%, 0 to 1%, particularly preferably 0 to 0.1%.
  • La 3+ , Gd 3+ , Ta 5+ , W 6+ , Nb 5+ , Ti 4+ , Y 3+ , Yb 3+ , Ge 4+ , Te 4+ , Bi 3+ and Zr 4+ are contained up to 10%. Can be made.
  • Rare earth components such as Ce 4+ , Pr 3+ , Nd 3+ , Eu 3+ , Tb 3+ and Er 3+ , Fe 3+ , Ni 2+ and Co 2+ are components that reduce the light transmittance. Therefore, the content of these components is preferably 0.1% or less, and more preferably not contained.
  • F ⁇ which is an anionic component has an effect of lowering the yield point and an effect of increasing the light transmittance. However, if the content is too large, the volatility at the time of melting becomes high and striae easily occurs. Further, the devitrification resistance is likely to be lowered.
  • the content of F ⁇ is preferably 0.1 to 70%, 1 to 67.5%, 5 to 65%, 2 to 60%, particularly preferably 10 to 60%.
  • examples of the raw material for introducing F ⁇ include fluorides such as La, Gd, Ta, W, Nb, Y, Yb, Ge, Mg, Ca, Sr, and Ba.
  • Sn-P-based glasses include, as mol%, SnO 50 to 80%, P 2 O 5 15 to 25% (however, 25% is not included), ZrO 2 0 to 3%, Al 2 O 3 0 to 10 %, B 2 O 3 0-10%, Li 2 O 0-10%, Na 2 O 0-10%, K 2 O 0-10%, Li 2 O + Na 2 O + K 2 O 0-10%, MgO 0- 10%, CaO 0-3%, SrO 0-2.5%, BaO 0-2%, MgO + CaO + SrO + BaO 0-11% and ZrO 2 + Al 2 O 3 + MgO 0-10%, SnO / P 2 O 5 Examples thereof include 1.6 to 4.8.
  • the average particle diameter of the glass powder is preferably 0.1 to 100 ⁇ m, 0.5 to 50 ⁇ m, particularly 1 to 20 ⁇ m. If the average particle diameter of the glass powder is too small, bubbles may be generated during the hot pressing, and the mechanical strength of the obtained wavelength conversion member may be reduced. In addition, the degree of light scattering in the wavelength conversion member increases, and if it becomes overscattered, the light emission efficiency may be reduced. On the other hand, when the average particle diameter of the glass powder is too large, the inorganic nanophosphor particles are difficult to be uniformly dispersed in the glass matrix, and as a result, the light emission efficiency of the obtained wavelength conversion member may be reduced.
  • Inorganic nanophosphor particles include CdS, CdSe, CdTe, ZnS, ZnSe, ZnTe, etc. as II-VI group compounds, InP, GaN, GaAs, GaP, AlN, AlP, AlSb, InN, InAs as III-V compounds.
  • quantum dot phosphors such as InSb. These can be used alone or in admixture of two or more. Or you may use the composite_body
  • inorganic nanophosphor particles include oxides, nitrides, oxynitrides, sulfides, oxysulfides, rare earth sulfides, aluminate chlorides, halophosphates, and the like. What consists of inorganic particles can also be used. These can be used alone or in admixture of two or more.
  • the average particle diameter of the inorganic nanophosphor particles is not particularly limited, but is usually 100 nm or less, 50 nm or less, particularly 1 to 30 nm, 1 to 15 nm, or even about 1.5 to 12 nm.
  • the luminous efficiency of the wavelength conversion member 3 varies depending on the type and content of the inorganic nanophosphor particles dispersed in the glass matrix and the thickness of the wavelength conversion member 3. If you want to increase luminous efficiency, adjust the wavelength conversion member 3 by reducing the thickness of the wavelength conversion member 3 to increase the transmittance of fluorescence or excitation light, or increasing the content of inorganic nanophosphor particles to increase the amount of fluorescence. That's fine. However, if the content of the inorganic nanophosphor particles is too large, it becomes difficult to sinter, the porosity increases, and it becomes difficult to efficiently irradiate the inorganic nanophosphor particles with the excitation light, or the wavelength conversion member 3. There arises a problem that the mechanical strength of the steel tends to decrease.
  • the content of the inorganic nanophosphor particles in the wavelength conversion member 3 is preferably adjusted as appropriate within the range of 0.01 to 30% by mass, 0.05 to 10% by mass, and particularly 0.08 to 5% by mass.
  • the mixture 1 may contain a light diffusing material such as alumina or silica up to 30% by mass in total.
  • Pressure during the heating press 10 kPa / cm 2 or more, 12 kPa / cm 2 or more, and particularly preferably 15 kPa / cm 2 or more. If the pressure of the hot press is too low, the glass powder tends to be insufficiently sintered or difficult to sinter in a short time. On the other hand, the upper limit of the pressure of the heat press is not particularly limited, hardly even further effect can be obtained too high, because it leads to energy loss, 400 kPa / cm 2 or less, 100 kPa / cm 2 or less, in particular 50 kPa / cm 2 or less Preferably there is.
  • the temperature of the heating press is preferably within the yield point ⁇ 50 ° C. of the glass powder.
  • the temperature of the hot press is preferably 380 ° C. or lower, 300 ° C. or lower, 200 ° C. or lower, particularly 180 ° C. or lower. If the temperature of the heating press is too high, the inorganic nanophosphor particles are deteriorated, or the inorganic nanophosphor particles and the glass powder react to easily decrease the light emission efficiency. On the other hand, if the temperature of the hot press is too low, the glass powder is not sufficiently sintered and the porosity of the wavelength conversion member 3 tends to increase. As a result, light scattering in the wavelength conversion member 3 becomes stronger, and the extraction efficiency of fluorescence (or excitation light) tends to be reduced. Therefore, it is preferable that the temperature of a hot press is 130 degreeC or more.
  • the heating press time is preferably 0.1 to 10 minutes, 0.3 to 5 minutes, 0.4 to 3 minutes, particularly 0.5 to 2 minutes. If the time for the heating press is too short, the glass powder tends to be insufficiently sintered. On the other hand, if the heating press time is too long, the inorganic nanophosphor particles tend to deteriorate.
  • the atmosphere of the heating press may be an air atmosphere, but in order to suppress problems such as glass powder modification, inorganic nanophosphor particle deactivation, and deterioration due to oxidation of the mold, reduced pressure atmosphere or inert atmosphere, especially running cost In consideration of the above, a nitrogen atmosphere is preferable.
  • the mixture 1 is heated and dried before being heated and pressed (drying method 1), or the glass powder is previously heated and dried and then mixed with inorganic nanophosphor particles to obtain the mixture 1 (drying method 2). ), It is possible to suppress the deterioration of the inorganic nanophosphor particles due to the water adhering to the glass powder surface. As a result, the quantum efficiency of the wavelength conversion member 3 can be improved. In the drying method 2, even if the glass powder is heated and dried to remove the water once, the water tends to be reattached in the step of mixing with the inorganic nanophosphor particles.
  • the drying method 1 is preferable because once the mixture 1 is produced, it is dried by heating and is directly subjected to a heating press, so that it is difficult for moisture to reattach to the glass powder.
  • the denseness becomes high, and therefore, moisture is less likely to enter the mixture 1 during subsequent heating and drying.
  • the heating temperature is preferably 50 to 200 ° C., 80 to 150 ° C., particularly preferably 100 to 130 ° C. If the heating temperature is too low, the above effect is difficult to obtain. On the other hand, when heating temperature is too high, inorganic nano fluorescent substance particles will deteriorate and the quantum efficiency of wavelength conversion member 3 will fall easily.
  • the heating time is preferably 1 to 30 hours, 2 to 20 hours, particularly 3 to 10 hours. If the heating time is too short, it is difficult to obtain the above effect. On the other hand, if the heating time is too long, the inorganic nanophosphor particles are deteriorated, and the quantum efficiency of the wavelength conversion member 3 tends to be lowered.
  • the atmosphere during heat drying is preferably a vacuum atmosphere or an inert atmosphere such as nitrogen in order to suppress the deterioration of the inorganic nanophosphor particles.
  • the thickness of the wavelength conversion member 3 is preferably 0.03 to 1 mm, 0.05 to 0.5 mm, particularly 0.1 to 0.3 mm. If the thickness of the wavelength conversion member 3 is too small, the mechanical strength tends to be inferior. On the other hand, when the thickness of the wavelength conversion member 3 is too large, the sintering time becomes long and the inorganic nanophosphor particles are easily deteriorated. Alternatively, the sintering tends to be insufficient.
  • the wavelength conversion member 3 can be used as a light emitting device by combining with an excitation light source such as LED or LD.
  • Example 1 SnO, a SnF 2, P 2 O 5 as starting materials, by cationic%, Sn 2+ 56.3%, P 5+ 43.8%, by anionic%, F - 24.8%, O 2- 75.2%
  • the batch prepared so as to contain the solution was put into a quartz beaker and melted at 680 ° C. for 5 minutes in an electric furnace in a nitrogen atmosphere.
  • the obtained mixture was placed on a lower die of a tungsten carbide press die, and another tungsten carbide press die was placed thereon, and preheated at 150 ° C. for 5 minutes in a nitrogen atmosphere. Then, it heat-pressed for 1 minute with the pressure of 14 kPa / cm ⁇ 2 > with 150 degreeC. Thereby, a plate-like wavelength conversion member was obtained. With respect to the obtained wavelength conversion member, the light emission quantum efficiency was measured and found to be 40%. In addition, the light emission quantum efficiency points out the value calculated by the following formula, and measured using the absolute PL quantum yield apparatus made from Hamamatsu Photonics. A quartz plate was used as a reference.
  • Luminescence quantum efficiency ⁇ (number of photons emitted from the sample as luminescence) / (number of photons absorbed from the sample) ⁇ ⁇ 100 (%)
  • Example 2 A wavelength conversion member was produced in the same manner as in Example 1 except that the temperature of the preheating and the heating press was 180 ° C. With respect to the obtained wavelength conversion member, the light emission quantum efficiency was measured and found to be 38%.
  • Example 3 A wavelength conversion member was produced in the same manner as in Example 1 except that the temperature of the preheating and the heating press was 200 ° C. The obtained wavelength conversion member was measured for luminescence quantum efficiency and found to be 30%.
  • Example 1 After adding and mixing the dispersion liquid of inorganic nano fluorescent substance particles with respect to glass powder, by performing a drying process on the conditions described in Table 1, the mixture of glass powder and inorganic nano fluorescent substance particles is obtained. Obtained. The obtained mixture was heated and pressed in the same manner as in Example 1 to obtain a plate-like wavelength conversion member. Table 1 shows the results of measuring the quantum efficiency of the obtained wavelength conversion member. The quantum efficiency was expressed as a relative value with the quantum efficiency of the wavelength conversion member of Example 1 being 100.

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PCT/JP2016/080255 2015-10-27 2016-10-12 波長変換部材の製造方法 WO2017073329A1 (ja)

Priority Applications (3)

Application Number Priority Date Filing Date Title
JP2017547720A JPWO2017073329A1 (ja) 2015-10-27 2016-10-12 波長変換部材の製造方法
CN201680061905.7A CN108140702A (zh) 2015-10-27 2016-10-12 波长变换部件的制造方法
KR1020177035955A KR20180075434A (ko) 2015-10-27 2016-10-12 파장 변환 부재의 제조 방법

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