WO2009088086A1 - ガラス、発光装置用の被覆材および発光装置 - Google Patents
ガラス、発光装置用の被覆材および発光装置 Download PDFInfo
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- WO2009088086A1 WO2009088086A1 PCT/JP2009/050252 JP2009050252W WO2009088086A1 WO 2009088086 A1 WO2009088086 A1 WO 2009088086A1 JP 2009050252 W JP2009050252 W JP 2009050252W WO 2009088086 A1 WO2009088086 A1 WO 2009088086A1
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- 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
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- 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
-
- 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
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
- C03C8/08—Frit compositions, i.e. in a powdered or comminuted form containing phosphorus
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
- H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L2224/10—Bump connectors; Manufacturing methods related thereto
- H01L2224/15—Structure, shape, material or disposition of the bump connectors after the connecting process
- H01L2224/16—Structure, shape, material or disposition of the bump connectors after the connecting process of an individual bump connector
- H01L2224/161—Disposition
- H01L2224/16151—Disposition the bump connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive
- H01L2224/16221—Disposition the bump connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked
- H01L2224/16225—Disposition the bump connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked the item being non-metallic, e.g. insulating substrate with or without metallisation
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
- H01L2924/15—Details of package parts other than the semiconductor or other solid state devices to be connected
- H01L2924/181—Encapsulation
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier 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 with at least one potential-jump barrier or surface barrier 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
- H01L33/52—Encapsulations
- H01L33/56—Materials, e.g. epoxy or silicone resin
Definitions
- the present invention relates to glass, and more particularly to glass used as a coating material for light emitting devices such as light emitting diode (LED) devices.
- LED light emitting diode
- a glass coating material can be considered as a stable alternative to heat, light and / or moisture in the environment that can alleviate such problems.
- a conventional general glass coating material requires a coating temperature of about 500 ° C. or higher due to restrictions on the softening point of glass.
- high temperature coating treatment is not preferable from the viewpoint of reliability.
- glass that can be coated at a coating temperature of less than 500 ° C. is required.
- Patent Document 1 discloses a P 2 O 5 —SnO-based glass for cathode ray tube (CRT) sealing having a coating temperature of 400 ° C. to 430 ° C.
- Japanese Unexamined Patent Publication No. 7-69672 discloses a P 2 O 5 —SnO-based glass for cathode ray tube (CRT) sealing having a coating temperature of 400 ° C. to 430 ° C.
- Patent Document 1 aims at CRT sealing (sealing between a glass panel and a glass funnel). Therefore, the composition of the glass of Patent Document 1 is determined by placing the highest importance on the strength of the glass. That is, the glass of Patent Document 1 has its glass transition point (Tg) lowered to 250 to 275 ° C., and the glass is intentionally crystallized to obtain its strength. That is, Patent Document 1 attempts to improve strength at the expense of crystallization. Moreover, the composition of the glass of Patent Document 1 is determined on the assumption that the area of a sealing object called CRT is large. Therefore, it is necessary to lower the viscosity at the sealing temperature, and the glass transition point (Tg) is intentionally lowered.
- Tg glass transition point
- the glass of Patent Document 1 is not suitable as a covering material for a small light-emitting device such as an LED device.
- a small light-emitting device such as an LED device.
- crystals that are not a problem with glass as a covering material for large-sized devices reduce light extraction efficiency with glass as a covering material for small-sized devices (particularly, glass as a covering material for light-emitting devices). It can be a fatal problem. That is, in the glass of Patent Document 1, even a slight crystal generated in the glass is small as a coating material, so that the crystal prevents the light emitted from the light emitting device from progressing and reduces the light amount of the light emitting device. .
- the present invention has been made in view of such a background, and an object of the present invention is to provide a glass that can be coated at a coating processing temperature of 400 ° C. or less and is less likely to be deteriorated or altered over a long period of time.
- the present invention in terms of mol% based on oxide, 27% to 33% P 2 O 5 , 50% to 70% SnO, 0-10% ZnO, 0.5% to 5% CaO, 0-5% B 2 O 3 , 0-3% Ga 2 O 3 , 0-3% In 2 O 3 , and 0-3% La 2 O 3 ,
- the glass characterized by including is provided.
- the glass preferably contains 52% to 63% SnO and P 2 O 5 + SnO in a total of 85% to 92% in terms of mol% on the basis of oxide.
- the content of P 2 O 5 is preferably 27% to 30% in terms of mol% based on the oxide.
- the content of CaO is preferably 3% to 5% in terms of mol% based on oxide.
- the present invention is a light emitting device having an optical element disposed on a base substrate and a covering material that covers the optical element, wherein the covering material is made of the glass described above. is there.
- the present invention it is possible to provide a glass that can be coated with a transparent glass at a coating treatment temperature of 400 ° C. or less, and that does not easily deteriorate or deteriorate over a long period.
- a covering material for a light emitting device made of such glass and further a light emitting device having such a covering material.
- the horizontal axis is T (temperature, ° C.), and the vertical axis is Te (thermoelectromotive force, ⁇ V). It is the figure which showed an example of the cross section of the light-emitting device by this invention. It is the figure which showed typically operation at the time of calculating
- the horizontal axis is T (temperature, ° C.), and the vertical axis is Te (thermoelectromotive force, ⁇ V).
- the glass of the present invention is expressed in mol% based on oxide, 27% to 33% P 2 O 5 , 50% to 70% SnO, 0-10% ZnO, 0.5% to 5% CaO, 0-5% B 2 O 3 , 0-3% Ga 2 O 3 , 0-3% In 2 O 3 , and 0-3% La 2 O 3 , It is characterized by including.
- Such a glass according to the present invention can be coated at 400 ° C. or lower.
- the glass according to the present invention has a characteristic that the glass transition temperature (Tg) is about 285 ° C. to 300 ° C. and is relatively high.
- a coating treatment temperature of about 500 ° C. or higher is required due to restrictions on the softening point of the glass.
- each component constituting the light emitting device may be damaged by heat, and the reliability of the device may be impaired.
- conventional glass a P 2 O 5 —SnO-based glass that can be coated at about 400 ° C.
- Tg glass transition temperature
- the glass transition temperature (Tg) of the P 2 O 5 —SnO glass it is necessary to relatively increase the content of P 2 O 5 .
- the chemical stability of the glass decreases. This is because P 2 O 5 easily reacts with moisture in the environment in the vicinity of this composition range.
- the content of P 2 O 5 exceeds 33 mol%, this effect becomes significant.
- the coating material deteriorates and deteriorates over time.
- the covering material is colored (for example, whitened or blackened) due to alteration, the transparency of the covering material is impaired, and the covering material becomes “opaque”.
- the coating material used in the device needs to be sufficiently transparent so as not to interfere with the light emission from the LED element. Therefore, when the above-described “opaque” phenomenon occurs in the covering material, the light output from the LED device is significantly reduced even if the area is small.
- the glass according to the present invention is not only capable of being coated at 400 ° C. or lower, but also has a characteristic that the glass transition temperature (Tg) is relatively high in the range of about 285 ° C. to 300 ° C. .
- Tg glass transition temperature
- the content of P 2 O 5 in the composition is significantly suppressed (33 mol% or less), and a decrease in chemical stability is significantly suppressed. Therefore, deterioration and deterioration of glass due to environmental factors (for example, moisture), and further “opacity” are significantly suppressed. Therefore, in the glass according to the present invention, an effect that appropriate transparency can be maintained over a long period is obtained.
- the glass according to the present invention can be used as a covering material for a light-emitting device that is stable for a long period of time. Further, since the Tg is in the range of about 285 ° C. to 300 ° C., the viscosity is high, and it is optimal as a covering material for a small device.
- FIG. 1 the differential thermal analysis (DTA: Differential Thermal Analysis) result of the glass by this invention is shown.
- DTA Differential Thermal Analysis
- This measurement was obtained by using a 110 mg glass sample and heating the sample from room temperature to 450 ° C. at a heating rate of 10 ° C./min.
- a differential thermal analyzer EXSTAR6000TG / DTA manufactured by Seiko Instruments Inc. was used for the measurement.
- shaft of FIG. 1 shows thermoelectromotive force Te (microvolt)
- a horizontal axis shows temperature T (degreeC).
- the glass also contains 30% P 2 O 5 , 60% SnO, 7% ZnO and 3% CaO, calculated as mol% based on oxide.
- P 2 O 5 is a component that stabilizes the glass and is essential.
- the content of P 2 O 5 is below 27 mol%, there is a possibility that the glass transition temperature (Tg) becomes higher. Further, as described above, there is a possibility that the content of P 2 O 5 is more than 33 mol%, decreases the resistance to environment (particularly moisture).
- the content of P 2 O 5 is particularly preferably 27 mol% to 30 mol%.
- SnO is a component that increases the fluidity of glass and is essential.
- the content of SnO is less than 50 mol%, the softening point becomes too high and the fluidity is deteriorated.
- content of SnO exceeds 70 mol%, vitrification will become difficult.
- the SnO content is 52 mol% to 63 mol% and the total content of P 2 O 5 + SnO is 85 mol% to 92 mol%, the Tg becomes a more preferable range.
- ZnO is not essential, but it has an effect of improving the water resistance of the glass and lowering the coefficient of thermal expansion, so it is preferably added in the range of 0 to 10 mol%. When the content of ZnO exceeds 10 mol%, devitrification tends to precipitate.
- the ZnO content is preferably 1/7 or less of the SnO content. If the ZnO content exceeds 1/7 of the SnO content, the softening point becomes too high and / or crystallization may be promoted.
- CaO is a component that can suppress crystallization of glass and lower the thermal expansion coefficient, and is essential. However, if the CaO content is less than 0.5 mol%, crystallization may not be suppressed. The content is more preferably 1 mol% or more. Moreover, when the content of CaO exceeds 5 mol%, the glass becomes unstable. In particular, 3 mol% to 5 mol% is preferable because a transparent and soft sealing is possible in a wide temperature range.
- B 2 O 3 is not essential, but may be contained up to 5 mol% as a compound that supports crystallization inhibition by CaO. If it exceeds 5 mol%, the refractive index becomes small and the chemical durability such as water resistance may be lowered.
- Ga 2 O 3 may be contained up to 3 mol% in order to improve water resistance and stabilize the glass. If it exceeds 3 mol%, the softening point becomes high and application as a coating material having a temperature of 400 ° C. or less may be difficult. Ga 2 O 3 is preferably 2 mol% or less, and more preferably 1 mol% or less.
- In 2 O 3 may be contained up to 3 mol% in order to improve water resistance and stabilize the glass. When it exceeds 3 mol%, the softening point becomes high and application as a coating material having a coating temperature of 400 ° C. or less becomes difficult.
- the upper limit of the content of In 2 O 3 is preferably 2 mol%, more preferably 1 mol%.
- La 2 O 3 may be contained up to 3 mol% in order to improve water resistance and stabilize the glass. When it exceeds 3 mol%, the softening point becomes high and application as a coating material having a coating temperature of 400 ° C. or less becomes difficult.
- the upper limit of the content of La 2 O 3 is preferably 2 mol%, more preferably 1 mol%.
- the glass of the present invention consists essentially of the above components, but other components such as MgO, SrO, Bi 2 O 3 , Y 2 O 3 , Gd 2 O 3 , and Ce within the range not impairing the object of the present invention. 2 O 3 , CeO 2 , TiO 2 , TeO 2 , Ta 2 O 5 or the like may be added.
- the glass of this invention does not contain PbO substantially.
- the glass of the present invention Li 2 O, Na 2 O , it is preferred not to substantially contain K 2 O, and the like. This is because, when these compounds are present in a significant content in glass, there is a possibility that deterioration due to ion diffusion into the semiconductor element may occur.
- the glass of the present invention MnO, Fe 2 O 3, Co 2 O 3, it is preferred not to substantially contain WO 3 and the like. This is because, when these compounds are present in a significant content in the glass, the transparency of the glass may be impaired due to coloring.
- the upper limit of the thermal expansion coefficient ( ⁇ ) of the glass of the present invention is preferably 130 ⁇ 10 ⁇ 7 / ° C., more preferably 128 ⁇ 10 ⁇ 7 / ° C.
- the lower limit of the thermal expansion coefficient ( ⁇ ) is preferably 110 ⁇ 10 ⁇ 7 / ° C., more preferably 115 ⁇ 10 ⁇ 7 / ° C.
- Tg glass transition temperature
- the thermal expansion coefficient ( ⁇ ) exceeds 130 ⁇ 10 ⁇ 7 / ° C.
- the element is brought into contact with the glass light emitting element in the process of cooling the element to room temperature or in the subsequent process. There is a risk of cracking starting from the part.
- the glass according to the present invention having the above composition can be used as a coating material for a light emitting device having a glass coating portion.
- a coating material for a light emitting device having a glass coating portion can be used as a coating material for a light emitting device having a glass coating portion.
- the configuration of the light-emitting device in which the glass of the present invention is applied as a coating material will be described taking an LED device as an example. It is obvious that the glass according to the present invention can be applied as a coating material for other light emitting devices.
- FIG. 2 schematically shows an example of a cross-sectional view of the LED device 1 according to the present invention.
- the LED device 1 includes a base substrate 120, a light emitting unit 100 placed on the base substrate 120, and a covering unit 110 that covers the light emitting unit 100.
- a plurality of wirings 130 are formed on the surface of the base substrate 120 on the side where the light emitting unit 100 is placed.
- the base substrate 120 is composed of a substrate made of an inorganic material such as rectangular alumina having a purity of 98.0% to 99.5% and a thickness of 0.2 mm to 1.2 mm, for example.
- the wirings 130a and 130b formed on the surface of the base substrate 120 may be gold wirings formed of, for example, a gold paste.
- the LED element 102 is, for example, an LED that emits ultraviolet light or blue light having a wavelength of 360 to 480 nm, and is an LED having a quantum well structure (InGaN-based LED) using InGaN in which In is added to GaN as a light-emitting layer. May be. However, it goes without saying that LEDs having specifications other than this may be used.
- the thermal expansion coefficient of the element substrate 101 is, for example, 70 ⁇ 10 ⁇ 7 to 90 ⁇ 10 ⁇ 7 / ° C. Normally, sapphire having a thermal expansion coefficient of about 80 ⁇ 10 ⁇ 7 / ° C. is used as the material for the element substrate 101.
- the covering portion 110 is composed of a covering material 115, and the covering material 115 is composed of glass having the above-described composition.
- the covering material 115 covering the light emitting unit 100 can be installed at a covering processing temperature of 400 ° C. or lower. Therefore, the thermal damage of each part which comprises the light-emitting device 1 can be suppressed significantly.
- the glass transition temperature (Tg) of this coating material is in the range of 285 ° C. to 300 ° C. Accordingly, the deterioration and deterioration due to moisture in the environment and the progress of “opacity”, which can be a problem in “conventional glass”, are significantly suppressed. Accordingly, a light emitting device that exhibits a stable light output over a long period of time can be provided.
- Example 1 Prepare a glass (glass according to Example 1) containing 30% P 2 O 5 , 60% SnO, 7% ZnO and 3% CaO, calculated as mol% on oxide basis, in the following manner: did.
- an orthophosphoric acid aqueous solution (containing 85 mass% H 3 PO 4 ) was added to the slurry to prepare a mixed solution.
- the normal phosphoric acid aqueous solution was injected little by little in a state where the slurry was agitated so as not to cause bumping of moisture.
- the obtained mixed solution was poured into a stainless steel bat provided with a “Teflon” (registered trademark) sheet. The vat was kept at 200 ° C. for 3 hours with sufficient ventilation, and dried to obtain a cookie-like solid having a weight of 200 g.
- each powder and the normal phosphoric acid aqueous solution were weighed so that each component contained in the finally obtained solid (200 g) had the aforementioned molar concentration.
- the obtained solid substance was put in a quartz crucible, and after placing a quartz lid on the upper part of the crucible, the crucible was held at 1100 ° C. for 40 minutes to dissolve the solid substance.
- the crucible was taken out from the furnace only once during the melting process, the lid was removed, and stirring was performed using a quartz rod. Thereafter, the crucible was covered again, and the crucible was returned to the furnace. After the melting process at 1100 ° C. for 40 minutes was completed, the crucible was removed from the furnace. Furthermore, in order to form the melt into plate-like glass, the molten glass in the crucible was poured into a carbon mold. Thereafter, the glass taken out from the carbon mold was placed in another electric furnace maintained at 315 ° C., held in this electric furnace for 1 hour, and then cooled to room temperature over 12 hours.
- the glass according to Example 1 was obtained through these steps.
- an orthophosphoric acid solution was used as a raw material for P 2 O 5 contained in the glass.
- powder raw materials such as zinc phosphate, tin phosphate, calcium phosphate, and aluminum phosphate can be used instead of the regular phosphate solution.
- the mixing step of the slurry and the powder can be omitted.
- Example 3 A glass containing 30% P 2 O 5 , 60% SnO, 9% ZnO, and 1% CaO, calculated in mol% on an oxide basis, in the same manner as in Example 1 (according to Example 3 Glass) was prepared.
- Example 4 30% P 2 O 5 , 60% SnO, 6% ZnO, 3% CaO, and 1% B 2 O 3 , calculated as mol% on oxide basis, in the same manner as Example 1. (A glass according to Example 4) was prepared.
- Example 5 30% P 2 O 5 , 62% SnO, 4% ZnO, 3% CaO, and 1% B 2 O 3 , calculated as mol% on oxide basis, in the same manner as Example 1. (A glass according to Example 5) was prepared.
- Example 6 In a manner similar to Example 1, calculated as mol% on oxide basis, 30% P 2 O 5 , 60% SnO, 8.5% ZnO, 0.5% CaO, and 1% A glass containing B 2 O 3 (glass according to Example 6) was prepared.
- Example 7 A glass containing 30% P 2 O 5 , 60% SnO, 9.5% ZnO, and 0.5% CaO, calculated in mol% on oxide basis, in the same manner as in Example 1 A glass according to Example 7) was prepared.
- Example 8 A glass containing 32% P 2 O 5 , 58% SnO, 8% ZnO, and 2% CaO, calculated in mol% on an oxide basis, in the same manner as in Example 1 (according to Example 8 Glass) was prepared.
- Example 9 In the same manner as in Example 1, calculated as mol% based on oxide, 30% P 2 O 5 , 60% SnO, 9.5% ZnO, and 0.5% B 2 O 3 A glass containing (glass according to Example 9) was prepared.
- the glass transition temperature (Tg) was calculated by the operation as shown in FIG. 3 from the measurement result of the differential thermal analysis. First, a straight line L1 is drawn so as to coincide with a flat portion in a region on a lower temperature side than a temperature at which an endothermic peak A on the lower temperature side occurs. Next, a straight line L2 is drawn so as to coincide with the curved portion after the inflection point B of the endothermic peak A. The intersection C of the two straight lines thus obtained was defined as the glass transition temperature (Tg).
- Example 4 and Example 6 After processing the glass of Example 4 and Example 6 so that the thickness was about 1.5 mm, both surfaces were mirror-polished. Then, this glass was cut
- Alumina base substrate with gold wiring pattern (dimensions: 14 mm long x 14 mm wide x 1 mm thick) and LED element (Toyoda Gosei Co., Ltd .: E1C60-0B011-03) with connection bumps prepared did.
- This LED element was mounted on a base substrate in a flip chip format.
- the LED element was placed in an electric furnace with the covering material sample placed on the flip-chip mounted LED element, and the temperature was increased from room temperature to 400 ° C. at a rate of 100 ° C. per minute. After the temperature reached 400 ° C., the LED element was held at the same temperature for 2 minutes to soften and flow the glass plate. Thereby, the LED element was covered with glass, and the LED device was formed. Thereafter, the LED device was cooled to room temperature at a rate of 100 ° C. per minute. After reaching room temperature, the LED device was taken out of the furnace and the state of the covering material was visually observed. As a result, no bubbles were observed on the surface and inside of the glass.
- the glass of the present invention can be used for coating and / or sealing of LED elements used for backlight light sources for liquid crystal panels, general lighting, and headlights for automobiles. It should be noted that the entire content of the specification, claims, drawings and abstract of Japanese Patent Application No. 2008-003553 filed on January 10, 2008 is cited herein as the disclosure of the specification of the present invention. Incorporated.
Abstract
Description
また、特許文献1のガラスは、CRTという封止対象物の面積が大きいものを想定して組成を決定している。そのため、封止温度での粘性を下げる必要があり、意図的に、ガラス転移点(Tg)を下げている。
27%~33%のP2O5、
50%~70%のSnO、
0~10%のZnO、
0.5%~5%のCaO、
0~5%のB2O3、
0~3%のGa2O3、
0~3%のIn2O3、および
0~3%のLa2O3、
を含むことを特徴とするガラスが提供される。
さらに、P2O5の含有量は、酸化物基準のmol%表示で、27%~30%であることが好ましい。
また、CaOの含有量は、酸化物基準のmol%表示で、3%~5%であることが好ましい。
100 発光部
101 素子用基板
102 LED素子
103 正極
104 負極
110 被覆部
115 被覆材
120 ベース基板
130a、130b 配線。
27%~33%のP2O5、
50%~70%のSnO、
0~10%のZnO、
0.5%~5%のCaO、
0~5%のB2O3、
0~3%のGa2O3、
0~3%のIn2O3、および
0~3%のLa2O3、
を含むことを特徴とする。
また本発明によるガラスは、長期間安定な発光装置の被覆材として使用することができる。また、Tgがほぼ285℃~300℃の範囲のため、粘性率も高くなり、小型装置の被覆材として最適である。
表1を用いて、実施例及び比較例について説明する。表中の例1~例8は、実施例であり、例9は比較例である。
以下の方法で、酸化物基準のmol%で計算して、30%のP2O5、60%のSnO、7%のZnOおよび3%のCaOを含むガラス(例1に係るガラス)を調製した。
例1と同様の方法により、酸化物基準のmol%で計算して、30%のP2O5、60%のSnO、5%のZnO、および5%のCaOを含むガラス(例2に係るガラス)を調製した。
例1と同様の方法により、酸化物基準のmol%で計算して、30%のP2O5、60%のSnO、9%のZnO、および1%のCaOを含むガラス(例3に係るガラス)を調製した。
例1と同様の方法により、酸化物基準のmol%で計算して、30%のP2O5、60%のSnO、6%のZnO、3%のCaO、および1%のB2O3を含むガラス(例4に係るガラス)を調製した。
例1と同様の方法により、酸化物基準のmol%で計算して、30%のP2O5、62%のSnO、4%のZnO、3%のCaO、および1%のB2O3を含むガラス(例5に係るガラス)を調製した。
例1と同様の方法により、酸化物基準のmol%で計算して、30%のP2O5、60%のSnO、8.5%のZnO、0.5%のCaO、および1%のB2O3を含むガラス(例6に係るガラス)を調製した。
例1と同様の方法により、酸化物基準のmol%で計算して、30%のP2O5、60%のSnO、9.5%のZnO、および0.5%のCaOを含むガラス(例7に係るガラス)を調製した。
例1と同様の方法により、酸化物基準のmol%で計算して、32%のP2O5、58%のSnO、8%のZnO、および2%のCaOを含むガラス(例8に係るガラス)を調製した。
例1と同様の方法により、酸化物基準のmol%で計算して、30%のP2O5、60%のSnO、9.5%のZnO、および0.5%のB2O3を含むガラス(例9に係るガラス)を調製した。
前述の各例に係るガラスのサンプルを用いて、ガラス転移温度(Tg)を測定した。転移温度の測定には、示差熱分析装置(セイコーインスツル社製示差熱分析装置EXSTAR6000TG/DTA)を用いた。粉末状に加工したサンプル110mgを白金パンに充填し、これを室温から500℃まで、10℃/分の昇温速度で昇温した。
各サンプルを直径5mm、長さ20mmの円柱状に加工して試料を作製した。この試料を10℃/分の昇温速度で250℃まで昇温し、熱膨張計(ブルカーエイエックスエス社製水平示差検出式熱膨張計TD5010)を用いて、各温度での膨張係数を測定した。100~250℃での値を25℃刻みで求め、その平均値を熱膨張係数αとした。
各サンプル(200g)を1100℃で溶融させた状態で、カーボン製の型に注入し、サンプルが固化するまでの間に、ガラス内部に結晶析出が生じるかどうかを目視で観察した。
各サンプルを赤外線集光炉で加熱温度を360℃、370℃、380℃、390℃、400℃にして封止を行った。各温度での封止の状況を観察した。表1中の封止温度における「○」は「透明でありかつ軟化した」を意味し、「※1」は「透明であったが軟化しなかった」を意味し、「※2」は「白濁しており軟化しなかった」を意味し、「※3」は「軟化はしたが白濁していた」を意味している。
例5および例8のサンプルを恒温恒湿槽に入れ、80℃80%RH下で保持し、約1000時間耐候性試験を行った。その後、460nmでの分光透過率を測定し、50%以上であったものを「○」とし、50%未満であったものを「△」とした。
なお、表1中、「-」は、測定、評価などが未実施であることを意味する。
次に、実際に本発明によるガラスを用いて、LED素子の被覆処理を行い、本発明によるガラスの被覆材としての適性を評価した。
なお、2008年1月10日に出願された日本特許出願2008-003553号の明細書、特許請求の範囲、図面及び要約書の全内容をここに引用し、本発明の明細書の開示として、取り入れるものである。
Claims (7)
- 酸化物基準のmol%表示で、
27%~33%のP2O5、
50%~70%のSnO、
0~10%のZnO、
0.5%~5%のCaO、
0~5%のB2O3、
0~3%のGa2O3、
0~3%のIn2O3、および
0~3%のLa2O3、
を含むことを特徴とするガラス。 - 酸化物基準のmol%表示で、52%~63%のSnO、および
P2O5+SnOの合計で85%~92%を含む請求項1に記載のガラス。 - P2O5の含有量は、酸化物基準のmol%表示で、27%~30%である請求項1または2に記載のガラス。
- CaOの含有量は、酸化物基準のmol%表示で、3%~5%である請求項1~3のいずれか1項に記載のガラス。
- 請求項1~4のいずれか1項に記載のガラスで構成された発光装置用の被覆材。
- ベース基板上に配置された光学素子と、該光学素子を被覆する被覆材とを有する発光装置であって、
前記被覆材は、請求項1~4のいずれか1項に記載のガラスで構成されていることを特徴とする発光装置。 - 前記光学素子が、発光ダイオード(LED)であることを特徴とする請求項6に記載の発光装置。
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EP09701328A EP2228350A4 (en) | 2008-01-10 | 2009-01-09 | GLASS, COATING MATERIAL FOR LIGHT-EMITTING DEVICE, AND LIGHT-EMITTING DEVICE |
CN2009801021360A CN101910081B (zh) | 2008-01-10 | 2009-01-09 | 玻璃、发光装置用被覆材料及发光装置 |
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Also Published As
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EP2228350A1 (en) | 2010-09-15 |
CN101910081A (zh) | 2010-12-08 |
US20100252858A1 (en) | 2010-10-07 |
JP5458893B2 (ja) | 2014-04-02 |
CN101910081B (zh) | 2012-10-10 |
KR20100103455A (ko) | 2010-09-27 |
JPWO2009088086A1 (ja) | 2011-05-26 |
EP2228350A4 (en) | 2010-12-29 |
US8203169B2 (en) | 2012-06-19 |
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