KR101270080B1 - High luminescent silicon based nitride phosphors, their fabrication method and light emitting devide comprising such a phosphor - Google Patents

Abstract

The present invention relates to a method for producing a silicon nitride phosphor using a silicon compound phosphor and self-induced pyrolysis reaction, and more particularly, to improve optical properties and significantly improve luminous efficiency, including a high brightness silicon compound phosphor having the following structure: One light-emitting device and LED package.
(Me _{1 - a} Re _a ) Si _x N _y
(Me is an alkaline earth metal, Re is a rare earth metal, Si is a silicon element, N is a nitrogen element, x, y is a real number satisfying 1 <x <20, 1 <y <30, and a replaces Me. The fraction of the activator to be satisfied, where 0 ≦ a ≦ 1.)

Description

High luminescent silicon based nitride phosphors, their fabrication method and light emitting devide comprising such a phosphor}

The present invention relates to a method for producing a silicon nitride phosphor using a silicon compound phosphor and self-induced pyrolysis. In addition, the present invention relates to a light emitting device and an LED package including the phosphor and improving optical characteristics and dramatically improving luminous efficiency.

Phosphors are used in fluorescent display tubes (VFDs), field emission displays (FEDs), plasma display panels (PDPs), cathode ray tubes (CRTs), white light emitting diodes (LEDs), and the like. These phosphors supply energy for excitation to emit light to the phosphor, and are excited by an excitation source having high energy such as vacuum ultraviolet ray, ultraviolet ray, electron beam, blue light, and the like to emit visible light.

Luminescence conversion emitting a white light emitting diode (LED) is a YAG which emits substantially 450㎚ region of blue Ga (In) N light emitting diode and the yellow light having a wavelength: made of a combination of Ce ^{3 +} phosphor. However, such white light emitting diodes have poor color rendering due to the absence of color components (mainly red light components), and thus can be used only within a limited range for general purpose lighting. In order to solve this problem, WO 98/39805 discloses a method of mixing white, green and red phosphors on a blue LED to produce white light by using a method of mixing red, green, and blue colors to produce white light. A method of mixing green and red phosphors in a phosphor-blue LED is disclosed. In response, many three-component or more nitride phosphors have been developed to replace conventional phosphors such as silicates, phosphates, aluminates, borates, sulfides and oxysulfide phosphors. Nitride compounds of urea show high potential as phosphors.

Japanese Laid-Open Patent Publication No. 2003-515665 discloses a phosphor having a composition of M _x Si _y N _z : Eu ⁺² (M is an alkaline earth metal selected from Ca, Sr, and Ba, z = 2 / 3x + 4 / 3y). have. In addition, US Patent Publication No. 2007/0040152 discloses that a phosphor having a composition of M ₂ Si ₅ N ₈ , MSi ₇ N ₁₀ , MSiN _2, and MeAlSiN ₃ (M is Mg, Ca, Sr, Ba, etc.) and substantially free of oxygen is present. Is disclosed.

However, the above methods use alkaline earth metal nitrides and rare earth metal nitrides as raw materials, which makes the manufacturing process difficult, the unit price of the nitrides high, and the problems of storage by air and moisture for the raw materials. The conversion efficiency of the phosphor obtained by the method is not effective and has room for improvement.

Due to these difficulties, the nitride silicate-based phosphors are difficult to produce on an industrial scale, and have disadvantages such as low purity due to the presence of oxygen as an impurity, low fluorescence characteristics due to low purity, and high manufacturing cost. It shows low optical properties.

Japanese Laid-Open Patent No. 2003-515665 (2003.05.07) United States Patent Application Publication No. 2007-0040152 (2007.02.22)

The present invention is to solve the problems of the prior art, is excited by a light source emitted in the near UV spectrum and the blue range to emit visible light, having a light efficiency of 50% or more than the conventional silicon compound compound By providing high brightness silicon compound phosphor, the reaction time is short, the process is simple, and it solves the problems such as high temperature and high pressure heat treatment and the use of plural gases which requires expensive investment cost in mass production. It is an object of the present invention to provide a method for producing a high brightness silicon compound phosphor powder having high properties and purity.

The high brightness silicon compound phosphor according to the present invention has a structure of Formula 1 below.

(Formula 1)

(Me _{1 - a} Re _a ) Si _x N _y

In Formula 1, Me is an alkaline earth metal, and any one or more elements selected from the group consisting of magnesium (Mg), calcium (Ca), strontium (Sr), and barium (Ba), and Re is an active agent for a silicon oxynitride ceramic structure. Lanthanum (La), Cerium (Ce), Praseodymium (Pr), Neodymium (Nd), Samarium (Sm), Eurobium (Eu), Gadolonium (Gd), Terbium (Tb), At least one selected from the group consisting of dysprosium (Dy), holmium (Ho), erbium (Er), tulium (Tm), ytterbium (Yb), and ruthenium (Lu) is an element, and x is 1 to 20 Real number and y is a real number from 1 to 30 represents the fraction of the active agent to replace the alkaline earth metal Me, the range is characterized by 0≤a≤1.

At this time, it is preferable to satisfy 6 ≦ x ≦ 15 and 7 ≦ y ≦ 25.

The silicon compound phosphor is characterized in that the average size of the powder size is at least 3.0㎛ or more, preferably 10.0㎛ or more.

In addition, according to the present invention, the manufacturing method for providing the high-brightness silicon compound phosphor is self-induced heat generation raw materials containing alkaline earth metal halides, rare earth metal oxides, rare earth metal halides, silicon sources, reducing agents, combustion promoters and reactive activators Reaction (Induced exothermic reaction) is characterized in that for producing a high brightness silicon compound phosphor powder.

Specifically, the method for preparing a high brightness silicon compound phosphor powder according to the present invention comprises the steps of: (a) providing a reaction mixture of alkaline earth metal halides, rare earth metal oxides, rare earth metal halides, silicon sources, reducing agents, combustion promoters and reactive activators ;

(b) complexing the reaction mixture under a nitrogen atmosphere in a high pressure reactor, followed by autocombustion reaction for reduction and nitriding reaction; and

(c) washing the product obtained by the reaction of step (b), followed by leaching with an acidic solution.

At this time, in step (b), the reaction mixture, which is a raw material, is locally instantaneously heated and ignited, characterized in that the reduction and nitriding reaction.

The production method according to the present invention does not supply additional heat from the outside, the reduction and nitriding reaction is propagated to the entire raw material by its own heat of synthesis reaction, the reaction is completed by itself, excellent production efficiency and chemical stability and The high purity silicon compound phosphor powder with high purity is produced.

(a) an alkaline earth metal halide in Step is _{MgF 2, CaF 2, SrF 2} , BaF 2, MgCl 2, CaCl 2, SrCl 2, BaCl 2, MgBr 2, CaBr 2, SrBr 2, BaBr 2, MgI 2, CaI ₂ , SrI ₂ , BaI ₂ or a mixture thereof. The alkaline earth metal halide contained in the raw material reacts with the reducing agent in step (b) to cause an exothermic reaction, and forms a high-brightness silicon compound due to the heat generated during the reduction and nitriding reaction.

In the step (a), the rare earth metal oxide is La ₂ O ₃ , CeO ₂ , Pr ₂ O ₃ , Nd ₂ O ₃ , Sm ₂ O ₃ , Eu ₂ O ₃ , Gd ₂ O ₃ , Tb ₂ O ₃ , Dy ₂ O ₃ , Ho ₂ O ₃ , Er ₂ O ₃ , Tm ₂ O ₃ , Yb ₂ O ₃ , Lu ₂ O _3, or a mixture thereof, rare earth metal halides include La ₃ F, LaCl ₃ , CeF ₃ , CeCl ₃ , PrF ₃ , PrCl ₃ , NdF ₃ , NdCl ₂ , NdCl ₃ , SmF ₂ , SmF ₃ , SmCl ₂ , SmCl ₃ , EuF ₂ , EuCl ₂ , GdF ₃ , GdCl ₃ , TbF ₃ , TbCl ₃ , DyF ₃ , DyCl ₃ , HoF ₃ , HoCl ₃ , ErF ₃ , ErCl ₃ , TmF ₃ , TmCl ₃ , YbF ₃ , YbCl ₃ , LuF ₃ , LuCl ₃ or a mixture thereof is not limited thereto.

The rare earth metal oxides and halides contained in the raw material are added to the high brightness silicon compound phosphor as an activator, and are excited when the high brightness silicon compound phosphor receives energy from the outside to serve to emit light.

In the step (b), the silicon source which serves to provide silicon when forming the high-brightness silicon compound compound phosphor by the combustion synthesis reaction is preferably silicon (Si), sodium silicon fluoride (Na ₂ SiF ₄ ), or a mixture thereof. .

In step (a), the reducing agent is preferably lithium azide (LiN ₃ ), sodium azide (NaN ₃ ), potassium azide (KN ₃ ) or a mixture thereof. The reducing agent serves to reduce alkaline earth metal oxides and halides and rare earth metal oxides and halides. After the self-induced fever reaction, the reducing agent is converted to LiF, LiCl, NaF, NaCl, KF, KCl, and is removed by washing in step (c).

In step (a), the combustion promoter is ammonium nitrate (NH ₄ NO ₃ ), magnesium nitrate (Mg (NO ₃ ) ₂ ), strontium nitrate (Sr (NO ₃ ) ₂ ), barium nitrate (Ba (NO _{3) 2} ) or mixtures thereof. The combustion accelerator contained in the raw material is decomposed into hydrogen, nitrogen, nitrate gas and alkaline earth metal during the combustion reaction, and generates a large amount of heat through the decomposition reaction to promote the formation reaction of the silicon compound. It plays a role of growing the particles to be more than 탆. In addition, the additional heat supply increases the crystallinity of the phosphor, thereby increasing the luminous efficiency, which is an essential element of the phosphor, by more than 50% compared to the case where no combustion accelerator is added.

In step (a), the reactive agent is ammonium fluoride (NH ₄ F), ammonium chloride (NH ₄ Cl), ammonium carbonate ((NH ₄ ) ₂ CO ₃ ), ammonium bicarbonate (NH ₄ HCO ₃ ) or a mixture thereof It is preferable. The reactive activator contained in the raw material is decomposed into hydrogen, carbon dioxide, and ammonia gas during the self-burning reaction of step (b), so that hydrogen promotes the reduction reaction of alkaline earth metal halides, and ammonia activates the nitriding reaction. After the reaction is completed, the reactive activator is mostly volatilized in gaseous state, and fluorine and chlorine are reacted with metals of the reducing agent (Li, Na, K) during the reaction to convert to LiF, LiCl, NaF, NaCl, KF, KCl, and the above ( removed by washing in step c).

The raw material of step (a) is weighed and mixed so as to have a silicone compound composition represented by Chemical Formula 1, and more preferably, in Formula 1, x and y satisfy 6≤x≤10 and 7≤y≤15. The raw materials are weighed and mixed to form a structure represented by a region forming a silicon compound in phase equilibrium, and the reducing agent and the reactive activator are 1 to 20 moles of reducing agent, 0.01 to 10 based on 1 mole of the alkaline earth metal halide. A mole of reactive agent is weighed and mixed, and the combustion accelerator is weighed and mixed at 0.001 to 0.5 mole based on 1 mole of alkaline earth metal halide.

In step (a), the raw material may be milled, such as a ball mill or a vibrating mill, in order to uniformly mix and adjust the particle size of materials contained in the raw material, wherein the milling is performed at a milling speed and a ball / raw material weight. Process conditions such as proportions, ball size, milling time, and atmosphere are varied and performed under appropriate conditions.

Thereafter, the raw material is loaded into a high-pressure reaction vessel, and localized instantaneous heat ignition of the raw material causes reduction and nitriding of the raw materials, that is, a step of self-inducing exothermic reaction is performed.

In the present invention, the self-induced heating reaction induces an initial synthesis reaction by heating two or more mixed raw materials to a reactionable temperature, and the synthesis reaction propagates itself to the entire raw material by the heat of reaction generated in the locally generated initial synthesis reaction. As this progressing and completion method, it means a synthetic reaction in which the reaction is continued even without applying heat from the outside. When the heat is reached to the ignition temperature by applying heat from the outside to cause the initial reaction, the sample reaches the reaction combustion temperature by the synthesis reaction. Thereafter, when the reaction is completed, the heat of reaction is transferred to the adjacent part, thereby lowering the temperature.

Self-induced heating reaction according to the present invention is difficult to control the process with high reaction temperature and fast reaction rate, but the product required by controlling the process parameters such as the molding density of the reactants, the pressure during the reaction, the particle size of the raw powder, other additives Can be obtained.

The raw material of step (a) is compressed by applying a molding pressure of 0.001 ~ 1t. When a molding pressure of 0.01t or less is applied, the molded body may be easily broken due to a low pressure, and when a molding pressure of 1t or more is applied, the molded body may not be easily ignited, and thus, the molded body may be molded at a pressure in the above range and loaded in a high pressure reaction vessel. After the high pressure reaction vessel is purged with nitrogen gas, the self-induced exothermic reaction is performed in a nitrogen gas atmosphere of 1 to 100 atm, preferably in a nitrogen gas atmosphere of 1 to 50 atm.

In order to trigger localized instantaneous heating and ignition of the self-induced heating reaction, the raw material may be ignited by applying a voltage to a coil-type heating element. The part ignited locally by the heating element in the raw material generates heat of reaction by the reaction, and the reaction combustion temperature rises to 1000 ° C or higher. At this time, a synthetic high temperature reaction occurs in the heated portion, and the heat generated by the reaction is transferred to another adjacent raw material portion to bring the temperature there to the ignition temperature. The part where the reaction is completed no longer generates its own heat of reaction, and there is no heat supply from the outside, so it is naturally cooled at a high speed, so that a separate cooling time is unnecessary and the reaction is completed in a short time.

Since the powders produced by the reaction of step (b) are agglomerated with each other, the step of physically pulverizing them may be performed, which may use a conventional ball mill, roll mill, or the like.

The reaction product of step (b) contains a product other than silicon oxynitride by a reducing agent, a reactive agent, or the like added to the raw material, and the washing and washing steps for removing the reaction product are performed.

The washing is performed by mixing and stirring distilled water with the reaction product (meaning the reaction product before or after grinding) of step (b), and separating and recovering the solid phase through solid-liquid separation using filtration. The step may be performed one or more times.

The washing step is performed by mixing and stirring an acid solution having a pH of 1 to 3 with the washed powder and then separating and recovering the powder, and may be repeated one or more times as in the washing step. The acid solution is a solution of hydrochloric acid, sulfuric acid, hydrofluoric acid, nitric acid or a mixed acid thereof.

The high brightness silicon compound phosphor is prepared by the method of preparing a high brightness silicon compound phosphor using the above-described self-induced heating reaction of the present invention. The average particle size of the powder is 3.0 µm or more, the apparent specific gravity is 1.0-1.5 g / cc, and the purity is high. Has the advantage of producing a high purity high brightness silicon compound phosphor having 99% or more.

The manufacturing method according to the present invention emits light having a wavelength of 300 to 500 nm, and locally heats and ignites only a part of a reactant so that the autogenous combustion reaction occurs at a high temperature with the heat generated by the reaction, thereby improving the thermal efficiency of the synthesis reaction process. Excellent, the impurities are vaporized, it is possible to provide a high-brightness silicon compound phosphor having a very high purity of the reaction yield, it provides a lighting fixture comprising the same. In addition, compared to the existing manufacturing process, the process is simple, the productivity is excellent, and the economical cost can be greatly reduced, and it is chemically very stable, so it can be applied to other phosphors (lower than 10% PL value) at 200 ℃ during the reflow test. Compared to this, the light efficiency shows less than 3%, which is very excellent.

Figure 1 shows a scanning electron micrograph of the high brightness silicon compound powder prepared in Example 1 of the present invention.
Figure 2 shows a scanning electron micrograph of the high brightness silicon compound powder prepared in Example 2 of the present invention.
Figure 3 shows the X-ray diffraction results of the high brightness silicon compound powder prepared in Example 1 of the present invention.
Figure 4 shows the X-ray diffraction results of the high brightness silicon compound powder prepared in Example 2 of the present invention.
Figure 5 shows the emission spectrum of the high brightness silicon compound powder prepared in Example 1 of the present invention.
Figure 6 shows the emission spectrum of the high brightness silicon compound powder prepared in Example 2 of the present invention.
Figure 7 shows the LED package spectrum of the high brightness silicon compound powder prepared in Example 2 of the present invention.

Hereinafter, the present invention will be described in detail by way of examples.

However, the following examples are illustrative of the present invention, and the contents of the present invention are not limited by the following examples.

Example 1

Strontium chloride (SrCl ₂ , large gold), eurobium oxide (Eu ₂ O ₃ , Alfa Aesar), silicon (Si, trielectrochemical), sodium azide (NaN ₃ , large gold), ammonium nitrate (NH ₄ NO ₃ , trielectric chemistry) and ammonium chloride (NH ₄ Cl, trielectric chemistry) powders were weighed in a molar ratio of 0.925: 0.075: 7: 3: 0.2: 1, and then the zirconia balls were mixed at a weight ratio of 1/2 of the raw material. Mix for 24 hours with a push. The mixture was placed in a high-purity alumina refractory container, laminated at 5 Mpa, pressurized to 5 Mpa, and then placed in a reactor, followed by three purging steps of charging and evacuating nitrogen gas, followed by filling and maintaining the inside of the reactor with 50 atm of nitrogen gas. A portion of the stacked raw materials were ignited using a hot wire to cause a rotating reaction to synthesize a powder. The synthesized powder was washed three times, and then mixed with HCl solution of pH 1, stirred for 2 hours, and then separated and recovered to wash the powder. Thereafter, the recovered powder was dried at 100 ° C. for 2 hours to prepare a high brightness silicon compound powder.

About the high brightness silicon compound powder obtained at the said process, the chemical composition analysis by the X-ray diffraction analysis and the particle shape by the electron microscope were observed.

In addition, in order to evaluate the fluorescence characteristics of the obtained high luminance silicon compound powder, an excitation spectrum at a detection wavelength of 520 to 560 nm and a light emission spectrum at an excitation wavelength of 450 nm were measured using a fluorescence measuring apparatus (FP-6500 manufactured by JASCO Corporation). Measured.

Example 2

Calcium Chloride (CaCl ₂ , Large Gold), Eurobium Oxide (Eu ₂ O ₃ , Alfa Aesar), Silicon (Si, Trielectrochemical), Sodium Azide (NaN ₃ , Large Gold), Ammonium Nitrate (NH ₄ NO ₃ , trielectric chemistry), ammonium chloride (NH ₄ Cl, trielectric chemistry) powder of a high-brightness silicone compound in the same manner as in Example 1 except that the powder was weighed and mixed in a molar ratio of 1.925: 0.075: 10: 5: 0.1: 1 Powder was prepared.

1 is a scanning electron micrograph of a high brightness silicon compound powder prepared in Example 1 of the present invention, Figure 2 is a scanning electron micrograph of a high brightness silicon nitride compound powder in Example 2 of the present invention, the present invention It can be seen that the high-brightness silicon compound powder having an average particle size of 3.0 μm or more is prepared by the method of preparing the same. In addition, as shown in Figures 1 and 2, the synthesized powder can be confirmed that there is little aggregation between the particles.

FIG. 3 is an X-ray diffraction result of the high brightness silicon compound powder prepared in Example 1, and FIG. 4 is a diagram showing an X-ray diffraction result of the high brightness silicon compound powder prepared in Example 2, and does not contain impurities. It can be seen that the high-brightness silicon compound of the crystalline pure SrSi ₇ N ₁₀ phase and CaSi ₁₀ N ₁₄ phase was prepared. In addition, Table 1 below shows the XRF results of the high brightness silicon compound powders prepared in Examples 1 and 2, indicating that a high brightness silicon compound phosphor according to the present invention was prepared.

5 is a view showing an emission spectrum of the high brightness silicon compound powder prepared in Example 1 of the present invention, Figure 6 is a view showing an emission spectrum of the high brightness silicon compound powder in Example 2 of the present invention.

The optical properties of the LED package applied to the high-brightness silicon compound powder prepared in Example 2 according to the present invention on a 50 to 452.5 nm blue chip were compared. At this time, the composition ratio of the main component, the curing agent, the green phosphor, and the silicon compound phosphor on the blue chip was SSN-26 (B) to which the high luminance silicon phosphor of Example 2 according to the present invention was applied at a ratio of 10: 10: 1.3: 0.65. , BR102C of the sample to be compared was 10: 10: 1.3: 1.3.

As shown in the above table, when comparing the sample to be compared with the powder prepared by the present invention, the same color coordinates are realized by adding only about 50% of the powder prepared by the present invention to the comparative sample, and the light emission of the LED product It can be seen that the strength is the same. Therefore, the product containing the phosphor according to the present invention can be confirmed that the cost savings by the weight ratio during mass production is remarkable.

7 is a view showing the LED package spectrum of the high-brightness silicon compound powder prepared in Example 2 of the present invention, the composition ratio of the main body, the curing agent, the green phosphor (GR), the silicon compound phosphor on the blue chip, respectively, in the present invention G + SSN-26 (B) to which the high-brightness silicon phosphor of Example 2 was applied was 10: 10: 1.3: 0.65, and the BR102C of the sample to be compared was 10: 10: 1.3: 1.3.

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed embodiments, but, on the contrary, Various modifications and variations are possible in light of the above teachings.

Accordingly, the spirit of the present invention should not be construed as being limited to the embodiments described, and all of the equivalents or equivalents of the claims, as well as the following claims, belong to the scope of the present invention .

Claims (15)

delete delete delete delete (a) providing a reaction mixture of alkaline earth metal halides, rare earth metal oxides, rare earth metal halides, silicon sources, reducing agents, combustion promoters and reactive activators;
(b) complexing the reaction mixture under a nitrogen atmosphere in a high pressure reactor, followed by autocombustion reaction for reduction and nitriding reaction; and
(c) washing the product obtained by the reaction of step (b) and then leaching it into an acidic solution. 6. The method of claim 5,
The reaction mixture is a method for producing a high-brightness silicon compound phosphor powder containing 1 to 20 moles of reducing agent, 0.01 to 10 moles of reactive activator and 0.001 to 0.5 moles of combustion accelerator with respect to 1 mole of alkaline earth metal halide. The method of claim 5,
The alkaline earth metal halide is _{MgF 2, CaF 2, SrF 2} , BaF 2, MgCl 2, CaCl 2, SrCl 2, BaCl 2, MgBr 2, CaBr 2, SrBr 2, BaBr 2, MgI 2, CaI 2, SrI 2 , BaI ₂ or a mixture of high brightness silicon compound phosphor powder using a self-induced heating reaction, characterized in that. The method of claim 5,
The rare earth metal oxide is La ₂ O ₃ , CeO ₂ , Pr ₂ O ₃ , Nd ₂ O ₃ , Sm ₂ O ₃ , Eu ₂ O ₃ , Gd ₂ O ₃ , Tb ₂ O ₃ , Dy ₂ O ₃ , Ho ₂ O ₃ , Er ₂ O ₃ , Tm ₂ O ₃ , Yb ₂ O ₃ , Lu ₂ O _3, or mixtures thereof, rare earth metal halides include La ₃ F, LaCl ₃ , CeF ₃ , CeCl ₃ , PrF ₃ , PrCl ₃ , NdF ₃ , NdCl ₂ , NdCl ₃ , SmF ₂ , SmF ₃ , SmCl ₂ , SmCl ₃ , EuF ₂ , EuCl ₂ , GdF ₃ , GdCl ₃ , TbF ₃ , TbCl ₃ , DyF ₃ , DyCl ₃ , HoF ₃ , A method for producing a high brightness silicon compound phosphor powder which is HoCl ₃ , ErF ₃ , ErCl ₃ , TmF ₃ , TmCl ₃ , YbF ₃ , YbCl ₃ , LuF ₃ , LuCl ₃ or a mixture thereof. The method of claim 5,
The silicon source is silicon (Si), Natri silicon fluoride (Na ₂ SiF ₄ ) or a mixture of high brightness silicon compound phosphor powder. The method of claim 5,
The reducing agent is a lithium azide (LiN ₃ ), sodium azide (NaN ₃ ), potassium azide (KN ₃ ) or a mixture thereof, a method for producing a high brightness silicon compound phosphor powder. The method of claim 5,
The combustion promoter may be ammonium nitrate (NH ₄ NO ₃ ), magnesium nitrate (Mg (NO ₃ ) ₂ ), strontium nitrate (Sr (NO ₃ ) ₂ ), barium nitrate (Ba (NO ₃ ) ₂ ) or Mixtures thereof, and the activator is ammonium fluoride (NH ₄ F), ammonium chloride (NH ₄ Cl), ammonium carbonate ((NH ₄ ) ₂ CO ₃ ), ammonium bicarbonate (NH ₄ HCO ₃ ), or a mixture thereof. Method for producing a silicon compound phosphor powder. The method of claim 5,
The nitrogen pressure of the step (b) is 0.5 ~ 10 MPa method for producing a high brightness silicon compound phosphor powder. An LED package comprising a light emitting device comprising a high brightness silicon compound phosphor powder prepared by the method of claim 5. The method of claim 13,
The LED package includes applying the high brightness silicon compound phosphor powder on a blue chip. The method of claim 13,
The LED package includes applying a yellow phosphor and the high brightness silicon compound phosphor powder on a blue chip.

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