WO2006005005A2 - Efficient, green-emitting phosphors, and combinations with red-emitting phosphors - Google Patents
Efficient, green-emitting phosphors, and combinations with red-emitting phosphors Download PDFInfo
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- WO2006005005A2 WO2006005005A2 PCT/US2005/023537 US2005023537W WO2006005005A2 WO 2006005005 A2 WO2006005005 A2 WO 2006005005A2 US 2005023537 W US2005023537 W US 2005023537W WO 2006005005 A2 WO2006005005 A2 WO 2006005005A2
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Definitions
- the present invention relates to green-emitting phosphors, to mixtures thereof with red-emitting phosphors, and to white light sources.
- Alkaline earth metal thiogallate phosphors activated with divalent europium are generally blue excited, green emitting phosphors. This type of phosphor can be used as an excellent color converter for LED devices such as white light devices.
- One such phosphor is of stoichiometric formulation (SrGa 2 S 4 :Eu), and was disclosed in Peters, Electrochem. Soc, vol. 119, 1972, p230. This phosphor has a low emission efficiency.
- a non-stoichiometric thiogallate-based phosphor of formula SrGa 2 S 4 :Eu:xGa 2 S 3 was described in US 6,544,438. This phosphor, designated STG, has emission efficiency as high as 90% or higher using a blue light excitation at about 470 nm.
- the LED devices with the phosphor powder typically a thin film of the particulate phosphor needs to be coated on a LED chip so that the phosphor efficiently absorbs the light out of the LED and re-emits light at longer wavelengths.
- the process of applying the phosphor powder onto LED chips involves delivery of given amount of phosphor powders in fluid form, such as a liquid-based slurry or slurry in molten polymer.
- a precise and fast delivery of the phosphor slurry is important.
- the grains of the powder typically have a narrow range of size, typically a size distribution between 4 and 7 micron, or a smaller, narrow range, such as 5 to 6 microns.
- the grains in this size range are suitable for ink-jet application.
- the strontium thiogallate phosphors can be mixed with phosphors that emit at a higher wavelength, meaning photonic lower energy. For example, where an LED produces blue light, partial conversion of this blue light by the two phosphors can create white light.
- a light emitting device comprising: a light output; a light source; and a wavelength transformer located between the light source and the light output, comprising Sri -x3 Ca x3 Ga 2 S 4 :Eu:xGa 2 S 3 wherein x is 0 to about 0.2 (or about 0.0001 to about 0.2), wherein x3 is 0 to 1, and wherein a minor part of the europium component is substituted with praseodymium in an efficiency enhancing amount, the wavelength transformer effective to increase the light at the light output having wavelength from 492 nm to 577 nm.
- a light emitting device comprising: a light output; a light source; and a wavelength transformer located between the light source and the light output, comprising Sr 1-x3 Ca x3 rGa 2 S 4 :Eu:xGa 2 S 3 wherein x is 0 to about 0.2 (or about 0.0001 to about 0.2), wherein x3 is 0 to 1, wherein a minor part of the europium component may be substituted with praseodymium in an efficiency enhancing amount, wherein the median grain size of the phosphor composition is from 2 to 4.5 microns, and wherein the quantum efficiency of the phosphor composition is 85% or more, the wavelength transformer effective to increase the light at the light output having wavelength from 492 nm to 577 nm.
- mixture of two or more phosphors, one of a first emission energy and the second of a lower emission energy comprising: the first phosphor of the formula
- a light emitting device with a light output comprising: a light source; a first wavelength transformer located between the light source and the light output, comprising SrGa 2 S 4 :Eu:xGa 2 S 3 wherein x is 0 to about 0.2 (or about 0.0001 to about 0.2), wherein x3 is 0 to 1, and wherein a minor part of the europium component is substituted with praseodymium in an efficiency enhancing amount; and a second wavelength transformer located between the light source and the light output, comprising Sr x2 Cai -x2 S:Eu , Y wherein x2 is an number from about 0 to 1 (or about 0.3 to about 0.8), and Y is one or more halides in atomic or ionic form.
- a third wavelength transformer such as described below, or other wavelength transformers, may be added.
- Figures 1 and 2 show light emitting devices.
- Figure 3 illustrates an exemplary layer structure for a near UV emitting semiconductor light source.
- Grains may be single crystals or agglomerations of single-crystal-like components of a phosphor.
- Particles are single crystals or the single-crystal-like components of a phosphor.
- the method of the invention comprises a first phosphor-forming process and a second sizing process.
- the forming process can comprise, for example, the following steps:
- a solution such as in dilute nitric acid
- a soluble strontium or calcium salt such as the nitrate
- a soluble trivalent europium salt such as the nitrate
- a small amount of trivalent praseodymium is added as a soluble salt or mineral (such as Pr 6 Oi 1 ).
- strontium/calcium/europium solution such as neutralizing with ammonium hydroxide
- a sulfate source such as sulfuric acid or ammonium sulfate
- the form of the precipitate is believed to be strontium sulfate particles coated with europium hydroxide.
- the size of the particles within the grains can be adjusted with certain parameters of the precipitation. For example, adding organic solvents to the aqueous medium, such as acetone or ethanol, decreases the polarity of the solvent and leads to a fine powder with smaller particles. Dispersing organic surfactants such as sorbitan monolaurate in the aqueous medium results in very fine particle precipitation. It is believed that smaller particle size allows for high efficiency in smaller grains. Such efficient smaller grain can be achieved with the processes of the invention.
- an acid-soluble gallium salt such as the nitrate.
- metallic gallium can be dissolved in nitric acid (e.g., overnight). As gallium oxide is difficult to convert to the sulfide, its use is less favored.
- a second precipitation is conducted after mixing a suspension of the first Sr/Ca/Eu precipitate with the gallium solution; the gallium solution added to provide an excess x of gallium as in the following formula (assuming strontium:
- the precipitation is conducted by sufficiently neutralizing (e.g., with ammonia) or adding a chaotrophic agent (such as urea).
- sufficiently neutralizing e.g., with ammonia
- a chaotrophic agent such as urea
- a fine powder resulting from the second precipitation is dried, ground and fired in hydrogen sulfide.
- the firing can be in a refractory boat (such as an alumina boat) in a tube furnace. Suitable firing can be, for example, 800 degrees C. for 5 hours.
- a second grinding and firing under hydrogen sulfide step can be applied to assure uniformity.
- a suitable second firing can be, for example, 900 degrees C. for 2 hours.
- X-ray analysis can be used to determine x, as "x" is used in Formula (I).
- Water-miscible (including miscible in the aqueous solvent as finally composed for the Sr/Eu precipitation) solvents for use in the precipitation include, for example, alcohols and ketones.
- the range of x is from one of the following lower endpoints (inclusive) or from one of the following upper endpoints (inclusive).
- the lower endpoints are 0, 0.0001, 0.001, 0.01, 0.02, 0.03, 0.04, 0.05, 0.06, 0.07, 0.08, 0.09, 0.1, 0.11, 0.12, 0.13, 0.14, 0.15, 0.16, 0.17, 0.18 and 0.19.
- the upper endpoints are 0.01, 0.02, 0.03, 0.04, 0.05, 0.06, 0.07, 0.08, 0.09, 0.1, 0.11, 0.12, 0.13, 0.14, 0.15, 0.16, 0.17, 0.18, 0.19 and 0.2.
- the range can be 0.001 to 0.2 or 0.001 to 0.1.
- the range of x3 is from one of the following lower endpoints (inclusive) or from one of the following upper endpoints (inclusive).
- the lower endpoints are 0, 0.0001, 0.001, 0.01, 0.02, 0.03, 0.04, 0.05, 0.06, 0.07, 0.08, 0.09, 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8 and 0.9.
- the upper endpoints are 0.01, 0.02, 0.03, 0.04, 0.05, 0.06, 0.07, 0.08, 0.09, 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9 and 1.
- praseodymium When praseodymium is present in the composition, praseodymium substitutes for a minor amount of europium, which amount is effective to enhance the quantum efficiency of the phosphor.
- the amount is for example 0.001 mol percent to 10 mol percent of europium or 0.05 mol percent to 4 mol percent of europium. In certain embodiments, the range of this percentage is from one of the following lower endpoints (inclusive) or from one of the following upper endpoints (inclusive).
- the lower endpoints are 0.001, 0.005, 0.01, 0.02, 0.03, 0.05, 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1.0, 1.2, 1.4, 1.6, 1.8, 2.0, 3.2, 3.4, 3.6, 3.8, 5, 6, 7, 8 and 9mol percent.
- the upper endpoints are 0.005, 0.01, 0.02, 0.03, 0.05, 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1.0, 1.2, 1.4, 1.6, 1.8, 2.0, 3.2, 3.4, 3.6, 3.8, 4.0, 5, 6, 7, 8, 9 and 10 mol percent.
- the range of the median size is from one of the following lower endpoints (inclusive) or from one of the following upper endpoints (inclusive).
- the lower endpoints are 2.0, 2.5, 3.0, 3.5, 4.0, 4.5, 5.0, 5.5, 6.0, 6.5, 7.0, 7.5, 8.0, 8.5, 9.0, 9.5, 10.0, 10.5, 11.0 and 11.5.
- the upper endpoints are 2.5, 3.0, 3.5, 4.0, 4.5, 5.0, 5.5, 6.0, 6.5, 7.0, 7.5, 8.0, 8.5, 9.0, 9.5, 10.0, 10.5, 11.0, 11.5 and 12.0.
- the range of the wavelength of light enhanced by the wavelength transformer is from one of the following lower endpoints (inclusive) or from one of the following upper endpoints (inclusive).
- the lower endpoints are 492, 493, 494,495,496,497,498,499, 500, 501, 502, 503, 504, 505, 506, 507, 508, 509, 510, 511, 512, 513, 514, 515, 516, 517, 518, 519, 520, 521, 522, 523, 524, 525, 526, 527, 528, 529, 530, 531, 532, 533, 534, 535, 536, 537, 538, 539, 540, 541, 542, 543, 544, 545, 546, 547, 548, 549, 550, 551, 552, 553, 554, 555, 556, 557, 558, 559, 560, 56, 562, 563, 564, 5
- the upper endpoints are 493, 494,495,496,497,498,499, 501, 502, 503, 504, 505, 506, 507, 508, 509, 510, 511, 512, 513, 514, 515, 516, 517, 518, 519, 520, 521, 522, 523, 524, 525, 526, 527, 528, 529, 530, 531, 532, 533, 534, 535, 536, 537, 538, 539, 540, 541, 542, 543, 544, 545, 546, 547, 548, 549, 550, 551, 552, 553, 554, 555, 556, 557, 558, 559, 560, 56, 562, 563, 564, 565, 566, 567, 568, 569, 570, 571, 572, 543, 574, 575,576 and 577 nm. [27] In certain embodiments, quantum efficiency
- the present invention is directed to red strontium-calcium sulfide phosphors having the formula
- x2 is a number of from 0 to 1 (such as about 0.3 to 0.8)
- Y is one or more halogens, in either their atomic or ionic forms, and to a method for making them.
- These phosphors have a high quantum efficiency, up to 95%. They are useful to change or convert light from electroluminescent devices to a different emission at various wavelengths.
- the host crystal, Sr x2 Ca 1-x2 S is a solid solution in which the ratio Sr.Ca can be changed arbitrarily.
- the emission spectrum of the material shifts its peak generally between 605 and 670 nm with changes in the strontium to calcium ratio.
- the range of the wavelength of light enhanced by the second wavelength transformer is from one of the following lower endpoints (inclusive) or from one of the following upper endpoints (inclusive).
- the lower endpoints are 605,
- the range of x2 is from one of the following lower endpoints (inclusive) or from one of the following upper endpoints (inclusive).
- the lower endpoints are 0.3, 0.35, 0.4, 0.45, 0.5, 0.55, 0.6, 0.65, 0.7 and 0.75.
- the upper endpoints are 0.35, 0.4, 0.45, 0.5, 0.55, 0.6, 0.65, 0.7, 0.75 and 0.8.
- the range of x2 is from one of the following lower endpoints (inclusive) or from one of the following upper endpoints (inclusive).
- the lower endpoints are 0, 0.0001, 0.0005, 0.001, 0.005, 0.01, 0.02, 0.03, 0.04, 0.05, 0.06, 0.07, 0.08, 0.09, 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8 and 0.9.
- the upper endpoints are 0.01, 0.02, 0.03, 0.04, 0.05, 0.06, 0.07, 0.08, 0.09, 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 0.95, 0.97, 0.98, 0.99, 0.995, 0.999, 0.9995, 0.9999 and 1.
- red phosphors are made by a) forming a mixture of the sulfate salts of strontium and calcium; b) adding a solution of europium oxide to the sulfate precipitate; c) firing the solids to a temperature of about 900° C. in a forming gas atmosphere; d) firing to a temperature of about 1000° C. in hydrogen sulfide atmosphere to convert the sulfate to the corresponding sulfide; e) adding an appropriate amount of a halide activator; and f) firing the mixture of step e) to about 1100° C. in nitrogen atmosphere.
- the present phosphors can be efficiently excited by the radiation of a blue light LED or other electroluminescent device to produce a red emission, and can be combined with appropriate phosphors to provide full color white light.
- the present calcium-strontium sulfide phosphors can be made by combining the desired amounts of calcium and strontium sulfates.
- Calcium sulfate can be made by forming a soluble salt solution, such as of calcium carbonate, precipitating the corresponding sulfate salt with sulfuric acid, decanting the liquid, rinsing the sulfate to remove excess acid, and drying the precipitate. [39] After drying, the calcium and strontium sulfate salts are combined with europium oxide as the activator, dissolved in nitric acid. The activator is slurried with the insoluble sulfate salts and the slurry is dried at about 100° C. for from 12-24 hours. [40] The mixture is fired in forming gas at a temperature of about 900° C. and held there for about six hours.
- the solids are then fired in hydrogen sulfide atmosphere to a temperature of about 1000° C. to form the sulfide salts from the sulfate salts.
- the desired amount of halide i.e., fluorine, chlorine, bromine and/or iodine, is added and the temperature increased to about 1100° C in nitrogen. After cooling the phosphor, it can be ground to a powder.
- red-emitting phosphors that can be used with the phosphors of the invention include, without limitation: Y 2 O 2 S: Eu 3+ ,Ce 3+ ; Y 2 O 2 S: Eu 3+ ,Sb 2+ ; Ca 2 MgSi 2 O 7 : Eu 2+ ,Mn 2+ ; Ba 2 Si0 4 :Ce 2+ ,Li + ,Mn 2+ ; SrS:Eu 2+ ,Cr; MgBaP 2 O 7 :Eu 2+ ,Mn 2+ ; CaS:Eu 2+ ,Cr; ZnGa 2 S 4 Mn; 6MgO* As 2 O 5 Mn 4+ .
- Appropriate phosphors for use as the third wavelength transformer shall be recognized by those of skill in the art. These include those described in US Pat. 6,783,700 (which is incorporated by reference herein in its entirety). These further include appropriately selected phosphors of Formula I (with or without substitution with Pr), particularly those described in PCT Appln. WO2004US11927, filed April 15, 2004 (which is incorporated by reference herein in its entirety).
- the range of the wavelength of light enhanced by the wavelength transformer is from one of the following lower endpoints (inclusive) or from one of the following upper endpoints (inclusive).
- the lower endpoints are 530 nm and the wavelengths to 609 nm (at, for example, 1 nm increments).
- the upper endpoints are 611 nm and the wavelengths to 610 nm (at, for example, 1 nm increments).
- the range can be 530 - 610 nm or 570 - 580 nm.
- the phosphors can be excited by light from a primary source, such as an semiconductor light source emitting in the wavelength of 300-420 nm, or from secondary light such as emissions from other phosphor(s) emitting in the same wavelength range. Where the excitation light is secondary, in relation to the phosphors of the invention, the excitation-induced light is the relevant source light.
- Devices that use the phosphor of the invention can include mirrors, such as dielectric mirrors, to direct light produced by the phosphors to the light output rather than the interior of the device (such as the primary light source).
- the semiconductor light source can, in certain embodiments, emit light of 300 nm or more, or 305 nm or more, or 310 nm or more, and so on in increments of 5 nm to 400 nm or more.
- the semiconductor light source can, in certain embodiments, emit light of 420 nm or less, or 415 nm or less, or 410 nm or less, and so on in increments of 5 nm to 350 nm or less.
- Phosphor particles may be dispersed in the lighting device with a binder or solidifier, dispersant (i.e., light scattering material), filler or the like
- the binder can, for example, be a light curable polymer such as an acrylic resin, an epoxy resin, polycarbonate resin, a silicone resin, glass, quartz and the like.
- the phosphor can be dispersed in the binder by methods known in the art.
- the phosphor can be suspended in a solvent, and the polymer suspended, dissolved or partially dissolved in the solvent, the slurry dispersed on the lighting device, and the solvent evaporated, hi some cases, the phosphor can be suspended in a liquid, pre-cured precursor to the resin, the slurry dispersed, and the polymer cured.
- Curing can be, for example, by heat, UV, or a curing agent (such as a free radical initiator) mixed in the precursor.
- the binder may be liquefied with heat, a slurry formed, and the slurry dispersed and allowed to solidify in situ.
- Dispersants include, for example, titanium oxide, aluminum oxide, barium titanate, silicon dioxide, and the like.
- lighting devices of the invention will use semiconductor light sources such as LEDs to either create excitation energy, or excite another system to provide the excitation energy for the phosphors.
- Devices using the invention can include, for example, white light producing lighting devices, indigo light producing lighting devices, blue light producing lighting devices, green light producing lighting devices, yellow light producing lighting devices, orange light producing lighting devices, pink light producing lighting devices, red light producing lighting devices, or lighting devices with an output chromaticity defined by the line between the chromaticity of a phosphor of the invention and that of one or more second light sources. Headlights or other navigation lights for vehicles can be made with the devices of the invention.
- the devices can be output indicators for small electronic devices such as cell phones and PDAs.
- the lighting devices can also be the backlights of the liquid crystal displays for cell phones, PDAs and laptop computers. Given appropriate power supplies, room lighting can be based on devices of the invention.
- the warmth (i.e., amount of yellow/red chromaticity) of lighting devices can be tuned by selection of the ratio of light from phosphor of the invention to light from a second source.
- Suitable semiconductor light sources are any that create light that excites the phosphors, or that excites a phosphor that in turn excites the phosphors of the invention.
- Such semiconductor light sources can be, for example, Ga-N type semiconductor light sources, In-Al-Ga-N type semiconductor light sources, and the like. In some embodiments, blue or near UV emitting semiconductor light sources are used.
- blue or near UV emitting semiconductor light sources are used.
- a semiconductor light source having a using at least two different phosphors it can be useful to disperse the phosphors separately, and superimpose the phosphor layers instead of dispersing the phosphors together in one matrix. Such layering can be used to obtain a final light emission color by way of a plurality of color conversion processes.
- the light emission process is: absorption of the semiconductor light source light emission by a first phosphor, light emission by the first phosphor, absorption of the light emission of the first phosphor by a second phosphor, and the light emission by the second phosphor.
- FIG. 3 shows an exemplary layer structure of a semiconductor light source.
- the blue semiconductor light comprises a substrate Sb, for example, a sapphire substrate.
- a buffer layer B an n-type contact layer NCt, an n-type cladding layer NCd, a multi-quantum well active layer MQW, a p-type cladding layer PCd, and a p-type contact layer PCt are formed in that order as nitride semiconductor layers.
- the layers can be formed, for example, by organometallic chemical vapor deposition (MOCVD), on the substrate Sb.
- MOCVD organometallic chemical vapor deposition
- a light-transparent electrode LtE is formed on the whole surface of the p-type contact layer PCt
- a p electrode PEl is formed on a part of the light-transparent electrode LtE
- an n electrode NEl is formed on a part of the n-type contact layer NCt.
- These layers can be formed, for example, by sputtering or vacuum deposition.
- the buffer layer B can be formed of, for example, AlN, and the n-type contact layer NCt can be formed of, for example, GaN.
- the n-type cladding layer NCd can be formed, for example, of AI r Ga 1 -r N wherein 0 ⁇ r ⁇ 1
- the p-type cladding layer PCd can be formed, for example, of AI q Ga 1 - q N wherein 0 ⁇ q ⁇ 1
- the p-type contact layer PCt can be formed, for example, of Al 3 Ga 1-8 N wherein 0 ⁇ s ⁇ 1 and s ⁇ q.
- the band gap of the p-type cladding layer PCd is made larger than the band gap of the n-type cladding layer NCd.
- the n- type cladding layer NCd and the p-type cladding layer PCd each can have a single- composition construction, or can have a construction such that the above-described nitride semiconductor layers having a thickness of not more than 100 angstroms and different from each other in composition are stacked on top of each other so as to provide a superlattice structure.
- the layer thickness is not more than 100 angstroms, the occurrence of cracks or crystal defects in the layer can be prevented.
- the multi-quantum well active layer MQW can be composed of a plurality of PnGaN well layers and a plurality of GaN barrier layers.
- the well layer and the barrier layer can have a thickness of not more than 100 angstroms, preferably 60 to 70 angstroms, so as to constitute a superlattice structure. Since the crystal of InGaN is softer than other aluminum-containing nitride semiconductors, such as AlGaN, the use of InGaN in the layer constituting the active layer MQW can offer an advantage that all the stacked nitride semiconductor layers are less likely to crack.
- the multi-quantum well active layer MQW can also be composed of a plurality of InGaN well layers and a plurality of AlGaN barrier layers.
- the multi-quantum well active layer MQW can be composed of a plurality of AlInGaN well layers and a plurality of AlInGaN barrier layers.
- the band gap energy of the barrier layer can be made larger than the band gap energy of the well layer.
- a reflecting layer can be provided on the substrate Sb side from the multi- quantum well active layer MQW, for example, on the buffer layer B side of the n-type contact layer NCt.
- the reflecting layer can also be provided on the surface of the substrate Sb remote from the multi-quantum well active layer MQW stacked on the substrate Sb.
- the reflecting layer can have a maximum reflectance with respect to light emitted from the active layer MQW and can be formed of, for example, aluminum, or can have a multi-layer structure of thin GaN layers.
- the provision of the reflecting layer permits light emitted from the active layer MQW to be reflected from the reflecting layer, can reduce the internal absorption of light emitted from the active layer MQW, can increase the quantity of light output toward above, and can reduce the incidence of light on the mount for the light source to prevent a deterioration.
- Figure 1 shows a light emitting device 10 with an LED chip 1 powered by leads 2, and having phosphor-containing material 4 secured between the LED chip and the light output 6.
- a reflector 4 can serve to concentrate light output.
- a transparent envelope 5 can isolate the LED and phosphor from the environment and/or provide a lens.
- the lighting device 20 of Figure 2 has multiple LED chips 11, leads 12, subsidiary leads 12', phosphor- containing material 14, and transparent envelope 15.
- Semiconductor light source-based white light devices can be used, for example, in a self-emission type display for displaying a predetermined pattern or graphic design on a display portion of an audio system, a household appliance, a measuring instrument, a medical appliance, and the like. Such semiconductor light source-based light devices can also be used, for example, as light sources of a back-light for LCD displays, a printer head, a facsimile, a copying apparatus, and the like.
- Ga solution 28.72 gram of gallium metal was dissolved in 200 mL concentrated nitric acid. The solution was warmed until the nitric acid fumed (and the preparation turns to brownish). The solution was cooled to room temperature and set overnight. After this overnight setting, the solution was clear greenish. The solution was heated until it turned yellow and then clear. Deionized water was added to make a 500 mL solution. The pH was. adjusted to pH 2.02 with ammonium hydroxide (approximately 40 mL), and then deionized water was added to 600 mL.
- Ga(OH) 3 The Ga solution prepared in step 4 was added to the suspension from step 3, and the pH adjusted to pH 7.0. The suspension was stirred for 17 hours at room temperature, then set for two hours. A product of white fine powder was filtered out.
- the powder was rinsed with acetone, then stirred with 1400 mL acetone for 1 hour at 50°C prior to another filtration to recover the powder.
- the powder was dried.
- the powder was ball milled for 5 hours, filtered and dried overnight.
- the powder was fired at 800°C for 5 hours in H 2 S gas. After being cooled down to room temperature, the powder was ground (can be ball milled) for 40 minutes.
- the phosphor was again fired at 900°C for 2 hours in H 2 S gas.
- the X-ray powder diffraction data of this sample showed the co-existence of two crystalline phases, one is SrGa 2 S 4 , and the other is Ga 2 S 3 .
- the grain size was measured on a Horiba CAPA-700 Grain Analyzer to be between 1 and 8.5 micron with a median size of 4.66 micron.
- the quantum efficiency was measured at 89% using the emission band at 537 nm with 450 nm excitation.
- Ga solution 57.17 grams of metal gallium was dissolved in 400 mL concentrated nitric acid. The solution was warmed until the nitric acid fumed (turned brownish). After the solution was cooled to room temperature and set overnight, the solution was transparent greenish. The solution was heated until it turned yellow and then clear. Deionized water was added to make a 1000 mL solution. The pH was adjusted to pH 1.2 with ammonium hydroxide (approximately 80 mL), then deionized water was added to 1200 mL.
- step 5 The Ga solution made in step 4 was added to the suspension obtained in step 3 while vigorously stirring. Ethyl alcohol was added to the suspension to a total volume of 3.4 L. The pH was adjusted to pH7.0. The suspension was stirred for two hours and then allowed to settle overnight. The supernatant was decanted and the powder filtered out. The powder was rinsed with acetone several times. The powder was dried at 55 0 C overnight.
- the powder was ball milled in acetone with alumina balls for 5 hours, then filtered and dried overnight.
- the powder was fired precursor at 800 0 C for 5 hour in H 2 S.
- the fired phosphor product was ground.
- Ga solution 57.54 gram of gallium metal was dissolved in 400 mL concentrated nitric acid. The solution was warmed until the nitric acid fumed (turned to brownish). The solution was cooled to room temperature and set overnight. After this setting, the solution was clear greenish. The solution was heated until it turned yellow and then clear. Deionized water was added to make a 1000 mL. The pH was adjusted to pH 2.02 with ammonium hydroxide (approximately 80 mL). Then deionized water was added to 1200 mL.
- Ga(OH) 3 The Ga solution prepared in step 4 was added into the suspension from step 3, and the pH adjusted to pH 7.0. The suspension was stirred for 2 hours at room temperature, then set for 15 hours. A white colored fine powder was recovered by filtration.
- the powder was rinsed with acetone, filtered, mixed with 1400 mL acetone for 1 hour at 50°C, and filtered again. The powder was dried.
- the powder was fired at 800°C for 5 hours in H 2 S gas. After being cooled to room temperature, the powder was ground (or can be ball milled) for 40 minutes.
- the phosphor was again fired at 900°C for 2 hours in H 2 S gas.
- the X-ray powder diffraction data of this phosphor sample showed the co ⁇ existence of two crystalline phases, one is SrGa 2 S 4 , and the other is Ga 2 S 3 .
- the grain size was measured on a Horiba CAPA-700 Grain Analyzer to be between 1 and 12 micron with median size of 6.8 micron.
- the quantum efficiency was measured as 88% using the emission band at 537 nm with 450 nm excitation.
- the suspension was allowed to settle for 30 minutes. A portion of the powder settled while another portion of the powder remained suspended.
- the suspension was transferred to another container, while the settled portion was isolated as a larger-sized portion.
- a weighed amount of STG phosphor with median particle size of 10.5 micron is suspended in acetone. The suspension is then placed into an alumina milling jar containing 1 A inch (0.635 cm) glass balls. Milling then proceeded for 40 minutes. After milling, the powder was dried at 55 0 C. The particles size was measured to be 7.2 micron (median). The quantum efficiency of the milled sample was 39%, while the quantum efficiency of the unmilled sample was 91%. Annealing of the milled phosphor at 500 0 C for 2 hours recovered partly the emission efficiency to 45%.
- a halide dopant such as ammonium chloride was added and fired in a quartz tube, placed in a reverse quartz tube and the temperature increased to 1100° C. at a rate of 207min in nitrogen for about one hour.
- the solids were ground with a mortar and pestle, sieved through a 100 mesh screen and stored under dry conditions.
- FIG. 1 of US 2003/0132433 is a graph of emission intensity versus wavelength for the phosphor.
- the excitation spectrum labeled "A" is shown on the left.
- the emission color changes from yellow to deep red as the strontiumicalcium ratio changes from a ratio of about 10 to 0.1.
- the excitation spectra changes its maximum position to longer wavelength as the calcium content increases.
- the peak labeled "2" is a phosphor having a Sr:Ca ratio of 0.75:0.25.
- the peak labeled "3" is a phosphor having a Sr:Ca ratio of 0.50:0.50.
- the peak labeled "4" is a phosphor having a Sr:Ca ratio of 0.25:0.75.
- the peak labeled "5" is a phosphor having a Sr:Ca ratio of 0.20:0.80.
- Example 6 The procedure of Example 6 was followed to make a phosphor having the formula Sr o . 75 Cao. 25 :Eu o .o 75 Cl.
- FIG. 2 (of US 2003/0132433) is a graph of emission intensity versus wavelength for this phosphor.
- the spectra curve labeled "1" is for a phosphor having a chloride content of 1.5%.
- the spectra curve labeled "2" is for a phosphor having a chloride content of 0.5%.
- the spectra curve labeled "3" is for a phosphor having no chloride. It can be seen that the emission intensity decreases as the chloride content decreases.
Abstract
Description
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- 2005-07-05 EP EP05800911A patent/EP1769050B1/en not_active Not-in-force
- 2005-07-05 KR KR1020077002838A patent/KR101209488B1/en active IP Right Grant
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Cited By (3)
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WO2013112915A1 (en) * | 2012-01-25 | 2013-08-01 | General Hydroponics, Inc. | Compositions, devices and methods for optimizing photosynthetically active radiation |
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Also Published As
Publication number | Publication date |
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US20060012287A1 (en) | 2006-01-19 |
EP1769050B1 (en) | 2013-01-16 |
KR20070030949A (en) | 2007-03-16 |
KR101209488B1 (en) | 2012-12-07 |
WO2006005005A3 (en) | 2006-12-28 |
EP1769050A2 (en) | 2007-04-04 |
US7427366B2 (en) | 2008-09-23 |
EP1769050A4 (en) | 2011-12-07 |
JP2008506011A (en) | 2008-02-28 |
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