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Definitions

• the present invention relates to a phosphor mainly composed of an inorganic compound, a method for producing the same, and a use thereof. More specifically, the application relates to a lighting device and a light-emitting device of an image display device that use the property of the phosphor, that is, the property of emitting fluorescence having a long wavelength of 570 nm or longer.
• Phosphors are used in fluorescent display tubes (VFD), field emission displays (FE D), plasma display panels (PDP), cathode ray tubes (CRT), white light emitting diodes (LEDs), and so on.
• VFD fluorescent display tubes
• FE D field emission displays
• PDP plasma display panels
• CRT cathode ray tubes
• LEDs white light emitting diodes
• the phosphor can be vacuum ultraviolet rays, ultraviolet rays, electron beams, blue light, etc. It is excited by an excitation source with high energy and emits visible light.
• the phosphor is lowered in luminance as a result of being exposed to the excitation source as described above, and there is a need for a phosphor that does not lower in luminance.
• sialon phosphors have been proposed as phosphors with little reduction in luminance, instead of phosphors such as conventional silicate phosphors, phosphate phosphors, aluminate phosphors, and sulfide phosphors.
• This siren phosphor is manufactured by a manufacturing process generally described below. First, silicon nitride (S i 3 N 4 ), aluminum nitride (A1N), calcium carbonate (CaC0 3 ), and europium oxide (Eu 2 0 3 ) are mixed at a predetermined molar ratio and 1 atm (0. IMP a) is produced by baking in a hot press method at 1700 ° C.
• Patent Document 2 discloses this Japanese Patent Application Laid-Open No. 2003-206481 (Patent Document 3), US Pat. No.
• Patent Document 4 discloses MS i 3 N 5 , M 2 Si 4 N 7, M 4 S is "u, M 9 S i U N 23, M 1S S ii 5 0 6 N 32, M 3 S i 18 A 1 12 0 18 N 36, MS i 5 A ⁇ 2 ⁇ 9, M 3 A phosphor that contains Eu and Ce as a host crystal and Si 5 A 1 ON 10 (where M is Ba, Ca, Sr, or a rare earth element) is described. This is a phosphor that emits red light and an LED illumination unit using this phosphor. Among them, as compounds containing S r, S r S i A 1 2 0 3 N 2 : E u2 + and S r 2
• JP 2002- the 322474 Patent Document 5
• luminescent material activated by S r 2 S i 5 N 8 and S r S i 7 N 10 crystal C e is proposed.
• JP 2003-321 675 Patent Document 6) includes L x My N ( 2 / 3x + 4 / 3y) : Z (L is a divalent element such as Ca, Sr , Ba, M is Si, Tetravalent elements such as Ge, Z is an activator such as Eu)
• L is a divalent element such as Ca, Sr , Ba
• M is Si
• Z an activator such as Eu
• Patent Document 7 discloses a light body composed of various L elements, M elements, and Z elements as LxMyN ( 2 / 3x + 4 / 3y) : Z phosphors.
• Patent Document 8 describes a wide range of combinations relating to the LMN: Eu, Z system, but the effect of improving the light emission characteristics when a specific composition or crystal phase is used as a base is shown. It has not been.
• Patent Document 3 4 shown in S r S i A 1 2 0 3 N 2: Eu2 + and S r 2 S i 4 A 1 ON 7: emission brightness of Eu 2+ was not sufficient.
• a white light emitting diode using a combination of a blue light emitting diode element and a blue absorbing yellow light emitting phosphor is known and has been put to practical use in various lighting applications.
• Typical examples are Patent No. 290 O 928 “Light Emitting Diode” (Patent Document 9), Patent No. 2927279 (Patent Document 10) “Light Emitting Diode”, Patent No. 33642 29 (Patent Document 11) “Wavelength Conversion”. Examples include a priming material, a manufacturing method thereof, and a light emitting element.
• the phosphors that are most often used are cerium-activated yttrium anolenium represented by the general formula (Y, Gd) 3 (A 1, Ga) 5 Oi 2 : Ce 3+ ⁇ Ganet phosphor.
• white light-emitting diodes composed of blue light-emitting diode elements and yttrium * aluminum / garnet-based phosphors have the characteristic of pale blue light emission due to the lack of red components, and there is a bias in color rendering. There was a problem.
• a white light-emitting diode is investigated by supplementing the red component, which is insufficient in yttrium, aluminum, and gannet phosphors, with another red phosphor by mixing and dispersing the two types of fluorescence #: It was done.
• Examples of such light emitting diodes include JP-A-10-163535 (Patent Document 12) “White Light-Emitting Element”, JP-A 2003-321675 (Patent Document 6) “Nitride Phosphor and its Manufacturing Method” can do.
• Patent Document 12 “White Light-Emitting Element”
• JP-A 2003-321675 Patent Document 6
• Patent Document 6 “Nitride Phosphor and its Manufacturing Method”
• the red phosphor described in Japanese Patent Laid-Open No. 10-163535 contains force dome and has a problem of environmental pollution.
• the red light-emitting phosphors described in JP 2003-321675 typically C ai. 97 Si 5 N 8 : Eu 0.03, do not contain cadmium. Therefore, further improvement in the emission intensity has been desired.
• Patent Document 2 U.S. Pat.No. 66 8 2 663
• Patent Document 3 Japanese Patent Application Laid-Open No. 2003-2 0 6481
• Patent Document 4 US Patent No. 66 7 0 748
• Patent Document 5 Japanese Patent Application Laid-Open No. 2002-3 2 2474
• Patent Document 6 Japanese Patent Laid-Open No. 2003-3 2 1675
• Patent Document 8 Japanese Patent Application Laid-Open No. 2004-1 0 786
• Patent Document 9 Patent No. 2900 9 2 8
• Patent Literature 10 Patent No. 2927 2 7 9
• Patent Document 1 1; Patent No. 3364 2 2 9
• Patent Document 12 Japanese Patent Laid-Open No. 10-166535 Disclosure of Invention
• the present invention is intended to meet such demands, and one of the objects is to provide a chemically stable inorganic phosphor having high luminance orange and red light emission characteristics. Furthermore, another object of the present invention is to provide a lighting apparatus having excellent color rendering properties using such a phosphor and an optical apparatus for an image display device having excellent durability. Means for solving the problem
• the inventors of the present invention are phosphorescent based on a divalent alkaline earth element such as Ca or Sr and an inorganic oxynitride crystal containing A1 and Si as main metal elements.
• the phosphors based on inorganic crystals with a specific composition emit light in orange and red with longer wavelengths than conventional rare earth activated sialon phosphors, and the nitrides reported so far In addition, we have found that it has higher brightness and better chemical stability than red phosphors based on oxynitrides.
• M element that becomes a luminescent ion (where M is one type selected from Mn, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb) Are two or more elements), a divalent A element (where A is one or more elements selected from Mg, Ca, Sr, and Ba), 3 1, and 8
• M is one type selected from Mn, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb
• A is one or more elements selected from Mg, Ca, Sr, and Ba
• the crystalline phase of a specific composition emits light in orange or red with a wavelength of 5700 nm or more
• the present inventors have found that the phosphor is excellent in chemical stability.
• the present invention includes M 13 S i 18 A 1 12 0 18 N 36 , MS i 5 A l 2 ON 9 , M 5 S i 5 A 10 N 10 (M Is completely different from sialons such as C a 1.47 E u 0.03 S i 9 A 1 3 ⁇ 1 ⁇ described in Chapter 1 of Non-Patent Document 2
• a phosphor in which Mn or a rare earth element as an emission center element M is activated in an inorganic matrix crystal changes its emission color and brightness depending on the electronic state around the M element.
• the host crystal is changed; from this, blue, green, yellow, and red emission have been reported.
• the emission color and brightness will be completely different, and it will be regarded as a different phosphor.
• the present invention uses a bivalent, trivalent, tetravalent, and multinary oxynitride as a base crystal, which is different from the conventional ternary nitride of divalent and tetravalent elements.
• a crystal completely different from that of the crystal is used as a host, and fluorescence using such a crystal as a host has not been reported.
• the phosphor based on the composition of the present invention is an excellent phosphor in that it emits red light having a higher luminance than those based on conventional crystals.
• the present inventor has obtained a phosphor exhibiting a high luminance light emission phenomenon in a specific wavelength region by adopting the configuration described in (1) to (14) below. Succeeded in providing.
• (1 5) to (2 4) were successfully used to produce a phosphor having excellent emission characteristics.
• a 2 Si 5-xA 1 x O x N 8 - x (where A is a mixture of one or more elements selected from Mg, Ca, Sr, or B a, X is a value of 0.05 or more and 0.8 or less, and the metal element M (where M is Mn, Ce, Nd, Sm, Eu, Tb, Dy, Ho, Er, Tm, 1.
• the inorganic compound is composed of Sr a C ab Si 5 -xA 1 xO x N 8 -x : Eu y , and the a and b values are
• the conductive inorganic substance is an oxide, oxynitride, nitride, or a mixture thereof containing one or more elements selected from Zn, Ga, In, and Sn.
• the phosphor according to item (1 1) characterized in that
• a composition comprising M, A, S i, A 1, 0, N, which is a mixture of metal compounds and fired (where M is Mn, Ce, Nd, Sm, Eu, Tb , Dy, Ho, Er, Tm, Yb, one or more elements selected from Ab, and A is one or more elements selected from Mg, Ca, Sr, Ba
• M is Mn, Ce, Nd, Sm, Eu, Tb , Dy, Ho, Er, Tm, Yb
• A is one or more elements selected from Mg, Ca, Sr, Ba
• the possible raw material mixture is calcined in a nitrogen atmosphere at a pressure of 0. IMP a or more and 10 OMP a or less in a temperature range of 1200 ° C or more and 2200 ⁇ or less, (1) to (14)
• the method for producing a phosphor according to any one of the items.
• the mixture of metal compounds is M metal, oxide, carbonate, nitride, fluoride, chloride or oxynitride and A metal, oxide, carbonate, nitride, fluoride,
• the phosphor powder after firing, the phosphor powder after pulverization treatment, or the phosphor powder after particle size adjustment is heat-treated at a temperature of 1000 ° C. or higher and lower than a firing temperature.
• the product is characterized by reducing the content of the glass phase, second phase, or impurity phase contained in the product by washing the product with a solvent comprising an aqueous solution of water or acid after firing.
• the method for producing a phosphor according to any one of items (15) to (21).
• a lighting fixture comprising a light emitting source and a phosphor, wherein the phosphor according to any one of claims 1 to (14) is used.
• the light emitting source is an LED that emits light having a wavelength of 330 to 420 nm
• the phosphor according to any one of claims 1 to 14 and the excitation light of 330 to 420 nm are used to generate 420 nm.
• a blue phosphor having an emission peak at a wavelength of 500 nm or less and a green phosphor having an emission peak at a wavelength of 500 nm or more and 570 nm or less by excitation light of 330 to 420 nm, red
• the lighting apparatus according to any one of (25) or (26), characterized in that green light and blue light are mixed to emit white light.
• the light-emitting light source is an LED that emits light having a wavelength of 420 to 500 nm, and the phosphor according to any one of claims 1 to 14 and excitation light of 420 to 500 nm is 500 nm or more.
• the light emitting light source is an LED that emits light having a wavelength of 420 to 500 nm, and the phosphor according to any one of claims 1 to 14 and the excitation light of 420 to 500 nm is 550 nm or more.
• An image display device comprising an excitation source and a phosphor, wherein at least the phosphor described in any one of (1) to (14) is used.
• the image display device is any one of a fluorescent display tube (VFD), a field emission display (FED), a plasma display panel (PDP), and a cathode ray tube (CRT).
• VFD fluorescent display tube
• FED field emission display
• PDP plasma display panel
• CRT cathode ray tube
• Item 15 The image display device according to any one of items (33) to (33). The invention's effect
• the phosphor of the present invention contains a divalent alkaline earth element, A 1, S ⁇ ⁇ , oxygen and nitrogen-containing primary oxynitride as main components, thereby enabling conventional sialon and oxynitride fluorescence. It emits light at a higher wavelength than the body and is excellent as an orange or red phosphor. Even when exposed to an excitation source, this phosphor provides a useful phosphor that is suitably used for VFD, FED, PDP, CRT, white LED, etc. without lowering the luminance.
• FIG. 1 is a diagram showing an X-ray diffraction chart of a phosphor (Example 1).
• Fig. 2 shows the X-ray diffraction chart of the phosphor (Comparative Example 2).
• Fig. 3 shows the emission and excitation spectra of the phosphor (Example 1).
• FIG. 4 Schematic diagram of a lighting fixture (LED lighting fixture) according to the present invention.
• Figure 6 A diagram showing the luminous spectrum of a lighting fixture.
• Fig. 7 Schematic of the lighting fixture (LED lighting fixture) according to the present invention.
• Fig. 8 Schematic diagram of an image display device (plasma display panel) according to the present invention. Explanation of symbols
• the phosphor of the present invention is a composition containing at least an activating element, a divalent alkaline earth element A, A1, Si, nitrogen, and oxygen.
• M is one or more elements selected from Mn, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, and Yb.
• A can include one or more elements selected from Mg, Ca, Sr, and Ba. With these constituent elements, a phosphor that emits light in the orange or red region can be obtained.
• the host crystal constituting the phosphor of the present invention is represented by A 2 Si 5- xA 1 xOxNs-x (where is a value of 0.05 or more and 0.8 or less).
• 8 is a substitutional solid solution in which a part of N is substituted with 0 and has a crystal structure similar to that of the A 2 Si 5 N. 8 crystal.
• a 2 Si 5-xA 1 x O x N 8 - x has not been reported so far in the form of a solid solution of A 1 and O. Is a crystal newly synthesized in the present invention.
• metal element ⁇ (where ⁇ is Mn, Ce, Nd, Sm, Eu, Tb, Dy, Ho, Er, Tm, When one element or two or more elements selected from Yb are dissolved, the phosphor emits orange or red light.
• the solid solution of A 1 and oxygen increases the chemical stability of the A 2 Si 5 N 8 crystal and improves the durability of the phosphor.
• substitution amount X is less than 0 ⁇ 05, the chemical stability is less effective.
• it is greater than 0.8, the crystal structure becomes unstable, and the brightness of the phosphor decreases. For this reason, the range of X should be between 0.05 and 0.8.
• a composition having a value in this range is preferable.
• a 2 S i 5- ⁇ 1 ⁇ ⁇ ⁇ ⁇ 8 - ⁇ the base of the phosphor, has the same crystal structure as A 2 S i 5 N 8 (where A is Mg, Ca, S r, or Ba)
• the composition has a small solid solution and only the lattice constant changes. Therefore, the inorganic compound of the present invention can be identified by X-ray diffraction.
• a 2 - y S i 5- x A 1 xOxNs-x a M y.
• the y value which is the content of soot in the entire inorganic compound, is in the range of 0.001 to 0.5, and a high-luminance phosphor can be obtained. If it is less than 0.001 atomic%, the luminance decreases because the amount of atoms involved in light emission is small, and if it exceeds 5 atomic%, the luminance decreases due to concentration quenching.
• elements with particularly high luminance are Ca and Sr. Since phosphors using these materials have different emission colors, they should be selected according to the application.
• Eu is used as the metal element M, light emission characteristics having a peak in the range of 570 to 650 nm can be obtained, and therefore, it is preferable as a red phosphor for illumination use.
• the combination of A and M, which has a particularly high brightness is C a 2 Si 5 N 8 where A is C a and M is Eu: £ ⁇ 1, 8 is 3 r, and M is Eu S r 2 S i 5 N 8 : Eu.
• C a and S r should be mixed.
• impurities contained in the inorganic compound be as small as possible.
• impurity elements such as Fe, Co, and Ni impede light emission, it is recommended to select the raw material powder and control the synthesis process so that the total of these elements is 500 ppm or less. .
• components serving A 2 S i 5- ⁇ 1 ⁇ ⁇ ⁇ ⁇ 8 of the oxynitride - chi: M y composition comprise as much as possible in high purity, if possible It is desirable that it is composed of a single phase, but it can also be composed of a mixture with other crystal phases or amorphous phases as long as the characteristics do not deteriorate.
• a 2 S i 5 - x A l x O x N 8 - x: the content of M y composition is desired to be 10 mass% or more to obtain a high luminance. More preferably, the luminance is remarkably improved at 50% by mass or more.
• the main component is such that the content of the A 2 Si 5 -x A and O x N 8 -My composition is at least 10% by mass or more.
• a 2 S 15- ⁇ 1 xOxNs -x the content of M y composition subjected to X-ray diffraction, can be obtained by multi-phase analysis of the Rietveld method. The easy easy manner, by using the X-ray diffraction results, A 2 S i 5- ⁇ 1 ⁇ ⁇ ⁇ 8 - ⁇ : the content from the ratio of the height of the strongest line of M y composition crystals and other crystals Can be sought.
• conductivity can be imparted to the phosphor by mixing an inorganic substance having conductivity.
• an inorganic substance having conductivity an oxide, an oxynitride, a nitride, or a mixture thereof containing one or more elements selected from Zn, Al, 'Ga, In, and Sn can be used.
• the phosphor of the present invention develops red, but if it is necessary to mix with other colors such as yellow, green, and blue, inorganic phosphors that develop these colors can be mixed as necessary. .
• the phosphor of the present invention has an excitation spectrum and a fluorescence spectrum that differ depending on the composition, and can be set to have various emission spectra by appropriately selecting and combining them.
• the mode may be set to the spectrum required based on the application.
• the phosphor of the present invention obtained as described above has a broad excitation range from electron beams, X-rays, and ultraviolet to visible light compared to ordinary oxide phosphors and existing sialons: 3 ⁇ 4 phosphors. In addition, it emits orange or red light of 570 nm or more, and in particular, it exhibits a red color from 6 O 0 nm to 70 nm in a specific composition. (X on the CIE chromaticity coordinates Y) indicates red emission in the range of 0.4 5 ⁇ x 0.7. Due to the above light emission characteristics, it is suitable for lighting equipment and image display devices.
• the phosphor of the present invention does not define a production method, but a phosphor having high luminance can be produced by the following method.
• a high-luminance phosphor can be obtained by firing in the temperature range of 0 0 to 2 2 0 0 C.
• the mixed powder of the metal compound may be fired in a state where the packing density is maintained at a bulk density of 40% or less.
• the bulk density is the volume filling rate of the powder, and is a value obtained by dividing the ratio of mass to volume when filling a certain container by the theoretical density of the metal compound.
• a boron nitride sintered body is suitable because of its low reactivity with metal compounds. Firing with the bulk density kept at 40% or less is because the reaction product grows in a free space when the material powder is baked in a free space around the raw material powder. This is because crystals with few surface defects can be synthesized because of less contact.
• the obtained mixture of metal compounds is placed in an inert atmosphere containing nitrogen.
• a phosphor is synthesized by firing in a temperature range of 1200 C to 2200.
• ⁇ is a metal resistance heating resistance heating method or a graphite resistance heating method because the firing temperature is a high temperature and the firing atmosphere is an inert atmosphere containing nitrogen.
• An electric furnace using carbon is preferred.
• a sintering method in which mechanical pressure is not applied from the outside such as an atmospheric pressure sintering method or a gas pressure sintering method, is preferable because firing is performed while maintaining a high bulk density.
• the powder aggregate obtained by firing is firmly fixed, it is ground with a powder mill normally used in factories such as a ball mill and a jet mill. Grind until the average particle size is 20 m or less.
• the average particle size is 0.1 111 or more and 5 111 or less.
• the average particle size exceeds 20 im, the fluidity of the powder and the dispersibility in the resin are deteriorated, and when the light emitting device is formed in combination with the light emitting element, the light emission intensity becomes uneven depending on the part.
• the thickness is less than 0.1 m, the amount of defects on the phosphor powder surface increases, and the emission intensity decreases depending on the phosphor composition.
• the phosphor powder after firing, the phosphor powder after powdering, or the phosphor powder after particle size adjustment is heat-treated at a temperature of 1 000 ° C or more and below the firing temperature, it was introduced to the surface at the time of pulverization, etc.
• the phosphor of the present invention exhibits higher luminance than the conventional sialon phosphor, and there is little decrease in the luminance of the phosphor when exposed to an excitation source.
• the lighting fixture of the present invention is configured using at least a light emitting light source and the phosphor of the present invention.
• Lighting equipment includes LED lighting equipment and fluorescent lamps.
• An LED illuminator can be manufactured by a known method such as described in JP-A-5-152609, JP-A-7-99345, and Japanese Patent No. 292 7279 using the purple light of the present invention. it can. In this case, it is desirable that the light source emits light with a wavelength of 330-500 nm.
• an ultraviolet (or purple) LED light emitting element of 330 to 420 nm or a blue light of 420-500 nm: LED light emitting element is preferable.
• Some of these light-emitting elements are made of nitride semiconductors such as GaN and InGaN.
• the light-emitting element can be a light-emitting light source that emits light of a predetermined wavelength. It can be.
• a lighting fixture that emits a desired color can be configured by using it together with a phosphor having other light emission characteristics.
• the green phosphor and the phosphor of the present invention are combinations of the green phosphor and the phosphor of the present invention.
• a blue LED light emitting element of 420 to 5 O 0 nm is combined with a yellow phosphor excited at this wavelength and having an emission peak at a wavelength of 550 nm to 600 nm and the phosphor of the present invention.
• a yellow phosphor as described in Japanese Patent No. 2927279 (Y, Gd) 2 ( A 1, Ga) 5 0 12: Ce Ya JP 20 02-363554 Fei one described Saiaron: the E u Can be mentioned.
• the image display device of the present invention is composed of at least an excitation source and the phosphor of the present invention, and includes a fluorescent display tube (VFD), a field emission display (FED :), a plasma display panel (PDP), and a cathode ray tube (CRT). ) and so on.
• VFD fluorescent display tube
• FED field emission display
• PDP plasma display panel
• CRT cathode ray tube
• the phosphor of the present invention emits light by excitation with vacuum ultraviolet rays of 100 to 190 nm, ultraviolet rays of 190 to 380 nm, electron beams, etc., and a combination of these excitation sources and the phosphor of the present invention. By combining them, it is possible to configure the image display device as described above.
• the raw material powder has an average particle size of 0.5iim, oxygen content of 0.93% by weight, template content of 92%, nitride nitride powder, specific surface area of 3.3 m ⁇ g, oxygen content of 0.79%
• Aluminum nitride powder, aluminum oxide powder with a specific surface area of 13.6 m2 / g, nitrogen nitride powder, and single-pium nitride powder synthesized by nitriding metal single-pium in Ammoni: were used.
• Composition formula E u cool S r 0 .i32 3 A 10.0333 S ⁇ o.sOo.osssNo.s Table 1 shows the parameters of the design composition and Table 2 shows the mixed composition of the raw material powder).
• the powder weighing, mixing, and molding steps were all performed in a glove box capable of maintaining a nitrogen atmosphere with a moisture content of 1 ppm or less and oxygen of 1 ppm or less.
• This mixed powder was placed in a boron nitride crucible and set in a graphite resistance heating type electric furnace.
• the firing atmosphere was evacuated with a diffusion pump, heated at a rate of 5001 per hour from room temperature to 800, introduced nitrogen with a purity of 99.999 volume% at 800, and a pressure of 0.5 MP.
• the temperature was raised to 1700 at 500 per hour and held at 1700 ° C for 2 hours.
• the fired body thus obtained was coarsely powdered, and then powdered by hand using a crucible made of a nitrided silicon sintered body and a mortar, and passed through a 30-m sieve. When the particle size distribution was measured, the average particle size was 8 m.
• the synthesized compound was pulverized using an agate mortar, and powder X-ray diffraction measurement using Cu Cu ⁇ : line was performed. The resulting chart is shown in FIG 1, FIG 2 Chiya one Bok of S r 2 S i 5 N 8 for comparison (synthesized in Comparative Example 2).
• the synthesized inorganic compound was confirmed to be only the lattice constant is the same crystal ⁇ as S r 2 S i 5 N 8 has changed, is a solid solution of S r 2 S Ns. Further, S r 2 S i 5 - x A 1 x O x N 8-x crystal phase other than was detected. As a result of irradiating this powder with a lamp that emits light with a wavelength of 365 nm, it emits red light Confirmed to do. The emission spectrum and excitation spectrum (Fig. 3) of this powder were measured using a fluorescence spectrophotometer.
• the composition formula Eu 0. 001 S r 0 .i32 3 A 10.1333S i ⁇ .2 ⁇ ⁇ 333 ⁇ compound represented by 4 (parameter design compositions in Table 1 Isseki, Table 2 shows the mixed composition of the raw material powders.) 32.6 wt%, 6% by weight of each of the nitride nitride powder, the aluminum nitride powder, the aluminum oxide powder, the strontium nitride powder, and the europium nitride powder. 347 wt%, 15. 79 wt%, 44.7 wt%, 0.58 wt% were weighed and mixed with an agate pestle and mortar for 30 minutes.
• the raw material powder is a nitride nitride powder having an average particle size of 0.5 m, an oxygen content of 0.93 wt%, an ⁇ content of 9 2%, a specific surface area of 3.3 m2 / g, and an oxygen content of 0.79.
• Luminium powder, aluminum oxide powder with a specific surface area of 13.6 ms / g, magnesium silicide powder, strontium nitride powder, calcium nitride powder, palycum nitride powder, and single-mouthed palladium powder synthesized by nitriding metal europium in ammonia was used.
• the emission wavelength is 6 37 nm, which is a preferable value as a phosphor for illumination and image display devices, and is a practically excellent composition.
• this inorganic compound was measured by X-ray diffraction, it was confirmed that it was a solid solution having the same crystal structure as Sr 2 Si 5 N 8 .
• Tables 1 to 3 The results of Examples and Comparative Examples are summarized in Tables 1 to 3 below.
• Table 1 shows the parameters of the design composition of each example 1-10.
• Table 2 shows the composition of the raw material powders of Examples 1 to 10 in each example. .
• Table 3 shows the peak wavelength and peak intensity of the excitation and emission spectra of Examples 1 to 10.
• Example 8 52.1 0.635 1.58 0 0 45.06 0 0.58
• a phosphor (/ 3 sialon: Eu) having the following composition was synthesized by the following procedure. First, in order to obtain a compound represented by the composition formula EU0.00296S i 0.41395A 1 ⁇ .01334 ⁇ .0044 ⁇ 0.56528, 94.77% by weight, respectively, of nitride silicon powder, aluminum nitride powder and europium oxide powder, 2. The mixture was mixed to 68 wt% and 2.556 wt%, placed in a boron nitride crucible, and baked at 1900 in nitrogen gas of IMP a for 8 hours.
• the obtained powder was an inorganic compound in which Eu was dissolved in ⁇ 1 sialon, and was a green phosphor as shown in the excitation emission spectrum of FIG. ..
• the so-called gun-type white light-emitting diode lamp (1) shown in Fig. 5 was manufactured.
• the lower electrode of the blue light-emitting diode element (4) is electrically connected to the bottom surface of the recess by the conductive best, and the upper electrode and the other lead wire (3) are the gold wire (5) Is electrically connected.
• As the phosphor a first phosphor and a second phosphor were mixed.
• the first phosphor is 3-sialon: Eu synthesized in this example.
• the second phosphor is the phosphor synthesized in Example 1.
• a mixture of the first phosphor and the second phosphor (7) is dispersed in the resin and mounted in the vicinity of the light-emitting diode element (4). Disperse this phosphor
• the first resin (6) is transparent and covers the entire blue light emitting diode element (4).
• the leading end portion of the lead wire including the concave portion, the blue light emitting diode element, and the first resin in which the phosphor is dispersed are sealed with a transparent second resin (8).
• the transparent second resin (8) has a substantially cylindrical shape as a whole, and has a lens-shaped curved surface at the tip, which is commonly called a shell type.
• the mixing ratio of the first phosphor powder and the second phosphor powder is 5 to 1, and the mixed powder is mixed with an epoxy resin at a concentration of 35% by weight, and an appropriate amount thereof is dropped using a dispenser.
• the first resin (6) in which the phosphor mixture (7) was dispersed was formed.
• Figure 6 shows the emission spectrum of this white light-emitting diode.
• a manufacturing procedure of the gun type white light emitting diode of the first embodiment will be described.
• a blue light emitting diode element (4) is die-bonded to the element mounting recess on one of the pair of lead wires (2) using a conductive best, and the lead wire and the blue light emitting diode are bonded together.
• the lower electrode of the diode is electrically connected and the blue light emitting diode (4) is fixed.
• the upper electrode of the blue light-emitting diode element (4) and the other lead wire are wire-bonded and electrically connected.
• a green first phosphor powder and a red second phosphor powder are mixed in advance at a mixing ratio of 5 to 2, and this mixed phosphor powder is mixed with an epoxy resin at a concentration of 35% by weight.
• Example 12 An appropriate amount of this is coated with a dispenser so as to cover the blue light emitting diode element in the concave portion, and cured to form the first resin portion (6). Finally, the tip of the lead wire including the recess, the blue light emitting diode, and the entire first resin in which the phosphor is dispersed are sealed with the second resin by a casting method.
• the same epoxy resin is used for both the first resin and the second resin.
• other resins such as a silicone resin or a transparent material such as glass may be used. It is preferable to select a material with as little deterioration by ultraviolet light as possible.
• Example 12 An appropriate amount of this is coated with a dispenser so as to cover the blue light emitting diode element in the concave portion, and cured to form the first resin portion (6).
• a chip-type white light-emitting diode lamp (21) for board mounting was manufactured.
• Figure 7 shows the composition.
• Two lead wires (22, 23) are fixed to a white alumina ceramic substrate (29) with high visible light reflectivity, and one end of the wires is located in the middle of the substrate, and the other end is in each case. It is an electrode that goes out and is soldered when mounted on an electric board.
• One of the lead wires (22) has a blue light-emitting diode element diode element (24) placed on one end of the lead wire so as to be in the center of the substrate. It is fixed.
• the lower electrode of the blue light-emitting diode element (24) and the lower lead wire are electrically connected by a conductive pace ⁇ , and the upper electrode and the other lead wire (23) are connected by a gold wire (25). Electrically connected.
• a mixture of the first resin and the second phosphor (27) is dispersed in the resin and mounted in the vicinity of the light emitting diode element.
• the first resin (26) in which the phosphor is dispersed is transparent and covers the entire blue light emitting diode element (24).
• a wall surface member (30) having a shape with a hole in the center is fixed on the ceramic substrate. As shown in FIG.
• the wall member (30) has a hole in the center for accommodating the first resin (26) in which the blue light emitting diode element (24) and the phosphor (27) are dispersed.
• the part facing the center is a slope. This slope is a reflection surface for extracting light forward, and the curved surface shape of the slope is determined in consideration of the light reflection direction.
• at least the surface constituting the reflective surface is a surface with high visible light reflectivity with white or metallic luster.
• the wall member was made of white silicone resin (30).
• the hole in the center of the wall member forms a recess as the final shape of the chip-type light-emitting diode lamp.
• the first light-emitting diode (24) and phosphor (27) are dispersed.
• a transparent second resin (28) is filled so as to seal all of the resin (26).
• the same epoxy resin was used for the first resin (26) and the second resin (28).
• the mixing ratio of the first phosphor and the second phosphor, the achieved chromaticity, etc. are substantially the same as in the first embodiment.
• the manufacturing procedure is substantially the same as the manufacturing procedure of the first embodiment, except for the portion for fixing the lead wires (22, 23) and the wall member (30) to the alumina ceramic substrate (29).
• a lighting device of FIG. 5 as a light emitting device using a blue LED of 450 nm, the phosphor of Example 1 of the present invention, Ca 0. 75 Eu
• Example 15 An illumination device having a configuration different from the above composition is shown.
• a 38 Onm ultraviolet LED was used as the light emitting element.
• the phosphor of Example 1 of the present invention, the blue phosphor (BaMgA 1 10 ⁇ 7 : Eu), and the green phosphor (B aM g A 1 10 ⁇ 17 : Eu, M n) is dispersed in the resin layer and covered with the ultraviolet LED.
• the LED emits light at 380 nm, and this light excites the red, green, and blue phosphors to emit red, green, and blue light. It was confirmed that these lights function as a lighting device that emits white light when mixed.
• Example 15 a design example of an image display device using the phosphor of the present invention will be described.
• FIG. 8 is a schematic diagram of the principle of a plasma display panel as an image display device.
• the red phosphor, the green phosphor (Zn 2 S i 0 4 : Mn), and the blue phosphor (BaMgA 1 10 O 17 : Eu) of Example 1 of the present invention are respectively provided in the cells 34, 35, 36. It is applied to the inner surface.
• the electrodes 37, 38, 39, and 40 are energized, vacuum ultraviolet rays are generated by Xe discharge in the cell, which excites the phosphor and emits red, green, and blue visible light. It was observed from the outside through the dielectric layer 42 and the glass substrate 45, and was found to function as an image display.
• the nitride phosphor of the present invention exhibits light emission at a wavelength higher than that of the conventional sialic acid oxynitride phosphor, is excellent as a red phosphor, and further exhibits the brightness of the phosphor when exposed to an excitation source. It is a nitride phosphor suitable for use in VFD, FED, PDP, CRT, white LED, etc. because of its low degradation. In the future, it can be expected to contribute greatly to industrial development by being used greatly in the design of materials for various display devices.

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• 2004
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• 2005
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