CN1318540C - Blue light-excitated white phosphor powder for LED and production method thereof - Google Patents

Blue light-excitated white phosphor powder for LED and production method thereof Download PDF

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CN1318540C
CN1318540C CN 02130949 CN02130949A CN1318540C CN 1318540 C CN1318540 C CN 1318540C CN 02130949 CN02130949 CN 02130949 CN 02130949 A CN02130949 A CN 02130949A CN 1318540 C CN1318540 C CN 1318540C
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phosphor
lt
blue light
white led
flux
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CN1482208A (en
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庄卫东
张书生
黄小卫
何华强
赵春雷
鱼志坚
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北京有色金属研究总院<Del/>
有研稀土新材料股份有限公司
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Abstract

本发明涉及一种蓝光激发的白色LED用荧光粉及其制造方法,该荧光粉的结构式为:R The present invention relates to a white LED with a fluorescent powder and method for producing a blue light excitation, the formula of this phosphor is: R

Description

一种蓝光激发的白色LED用荧光粉及其制造方法 White LED with a phosphor and method for manufacturing a blue light excitation

技术领域 FIELD

本发明涉及一种蓝光激发的白色LED用荧光粉及其制造方法。 The present invention relates to a white LED with a fluorescent powder and method for producing a blue light excitation.

背景技术 Background technique

在蓝色LED芯片上涂敷高效的可被蓝光有效激发而发射黄光的荧光粉,即可得到白色LED。 Coating efficiency may be blue light efficiently excited in the blue LED chip and emits yellow phosphor, to obtain a white LED. 白色LED光源的研究成功,为LED在普通照明中的应用创造了条件。 Successful research white LED light source, to create the conditions for the application of LED lighting in general in. 其特点是具有小电流,在室温下即可得到足够的亮度,发光响应快,性能稳定,寿命长,体积小,经久耐用,抗冲击等优点,因此在普通照明、指示灯、信号等领域有广泛的应用,根据有关专家预测在未来的30年中它的用量将会取代现有的普通照明白炽灯的30%以上。 Characterized by a small current, to obtain a sufficient luminance, emission, fast response, stable performance, long life, small size, durability, impact resistance, etc. at room temperature, there is in the field of general lighting, lights, signals, etc. wide range of applications, according to the experts predict the next 30 years, its amount will replace more than 30% of the existing general illumination incandescent lamp.

目前,此种方法制造的白色LED对荧光粉的性能要求很高,主要是发光亮度要高,激发波长宽,粉体颗粒尺寸要小而且均匀。 Currently, such a method of manufacturing a white LED performance phosphor demanding, mainly emission luminance higher, excitation wave length and width, the powder particle size is smaller and uniform. 此种荧光粉主要是YAG钇铝石榴石,化学式为:(Y,Gd)3(Al,Ga)5O12:Ce。 Such phosphor mainly YAG of yttrium aluminum garnet, of the formula: (Y, Gd) 3 (Al, Ga) 5O12: Ce.

美国专利5998925报道YAG:Ce荧光粉中Y/Gd比,Al/Ga比以及加入Sm后荧光粉发光主峰波长的变化情况。 U.S. Patent No. 5,998,925 reports YAG: Ce phosphor in the Y / Gd ratio, and the change of Al / Ga ratio after addition of Sm phosphor emission peak wavelength.

发明内容 SUMMARY

本发明的目的是提供一种发光强度高、激发波长宽、而且发射主峰可以在很宽的范围移动的一种蓝光激发的白色LED用荧光粉。 Object of the present invention is to provide a high a light intensity, excitation wave length and width, and emitting white LED with a phosphor peak can excite In one blue wide range of movement.

本发明的另一个目的是提供一种简单、无污染、成本低的蓝光激发的白色LED用荧光粉的制造方法。 Another object of the present invention is to provide a simple, non-polluting, low-cost method for manufacturing a white LED with a phosphor blue light excitation.

为实现上述目的,本发明采取以下技术方案:本发明的材料结构式为:R(3-xy)M5O12:CexR′y,其中R为Y,Gd,Lu,Sc,La和Sm中至少一种;M为B,Al,Ga,In,P,Ge和Zn中至少一种;0.1≤x<1;R′可以为Eu,Dy,Pr和Mn中一种或几种;0<y<0.5。 To achieve the above object, the present invention adopts the following technical scheme: Material structural formula of the present invention are: R (3-xy) M5O12: CexR'y, wherein R is Y, Gd, Lu, Sc, La and Sm, at least one; M is B, Al, Ga, in, P, Ge, and Zn at least one; 0.1≤x <1; R 'may be Eu, Dy, Pr, and Mn, one or more; 0 <y <0.5.

本发明系统地研究荧光粉的基质、激活剂,在其中添加多种新的稀土和非稀土元素,并研究各种元素最佳的比例关系,获得的荧光粉发光强度高,激发波长宽,而且发射主峰可以在很宽的范围移动。 Systematic study of the phosphor of the present invention, a matrix, an activator, added thereto several new rare-earth and non-rare earth elements, and to study the optimal ratio between the various elements, high phosphor emission intensity obtained by the excitation wave length and width, and emission peak can be moved over a wide range.

在本发明的蓝光激发的白色LED用荧光粉中,所述的荧光粉的中心粒径(D50)在1~5um范围内。 In the white LED with a phosphor blue light according to the present invention, excitation of the central particle diameter of the phosphor (D50) of in the range of 1 ~ 5um.

本发明的蓝光激发的白色LED用荧光粉的方法,包括下述步骤:(1)按结构式:R(3-xy)M5O12:CexR′y进行配料,其中:R为Y,Gd,Lu,Sc,La和Sm中至少一种,M为B,Al,Ga,In,P,Ge和Zn中至少一种,0.1≤x<1,R′可以为Eu,Dy,Pr和Mn中一种或几种,0<y<0.5,按照上述的结构式的配比称取上述元素的单质、或其氧化物、或其相应盐类,作为原料;(2)将上述原料进行共沉淀处理;(3)在上述原料中加入助熔剂,并混合均匀,所述的助熔剂为碱土金属、稀土金属、铝、镓、铟的任意一种的氟化物或氯化物,硼酸、氧化硼中至少一种,所述的助熔剂占总重量(即助熔剂和上述原料的重量)的百分比为0.001%~10wt%;(4)然后进行还原焙烧,还原焙烧温度为1100~1600℃,还原焙烧时间为0.5~15h;(5)将上述还原产物洗涤,过滤,烘干,得到最终产品,即得到体色为浅黄色或黄色的 The method of white LED with a phosphor excited by blue light of the present invention, comprising the steps of: (1) by the structural formula: R (3-xy) M5O12: CexR'y compounding, wherein: R is Y, Gd, Lu, Sc , La and Sm, at least one, M being B, Al, Ga, in, P, Ge, and Zn at least one, 0.1≤x <1, R 'may be one kind of Eu, Dy, Pr, and Mn or several, 0 <y <0.5, according to the above formula the ratio of said elemental take the above elements, or an oxide thereof, or the corresponding salts, as a starting material; (2) the raw material coprecipitation process; (3 ) added to the flux in the raw material and mixed uniformly, the flux is an alkaline earth metal, any one rare earth metal, aluminum, gallium, indium fluoride or chloride, boric acid, boron oxide of at least one, the percentage of the flux of the total weight (i.e. the weight of flux and of the raw material) is 0.001% ~ 10wt%; (4) followed by reduction firing, reducing the firing temperature is 1100 ~ 1600 ℃, reduction roasting time of 0.5 to 15h; (5) above was washed reduction product, filtering and drying, to obtain the final product, i.e., to obtain body color is pale yellow or yellow 末——本发明的荧光粉。 End - phosphor of the present invention.

本发明通过上述方法得到一系列各方面性能优异,可以广泛应用于白色LED的荧光粉。 The present invention was excellent in a series of various aspects of performance by the above method can be widely used as a white LED phosphor.

在上述方法中,在所述步骤(2)中,即将上述原料进行共沉淀处理。 In the above method, the step (2), i.e. the raw material coprecipitation process. 用共沉淀方法对原料进行预处理,通过共沉淀控制原料的粒径,可以得到范围在1~4um任意中心粒径的荧光粉,而且提高了粒度分布的均匀性。 Raw material is pretreated using a coprecipitation method, coprecipitation controlling the particle size of raw materials, can be obtained in the range of 1 ~ 4um any central particle diameter of the phosphor, but also improves the uniformity of particle size distribution. 另一方面由于共沉淀使原料混合更加均匀,从而会使荧光粉的发光强度有所提高。 On the other hand due to the co-precipitation of the mixed raw material more uniform, so that the luminous intensity will phosphor improved. 粉体的颗粒尺寸的大小和均匀性也是荧光粉的重要指标,其对制灯影响更为明显。 The particle size of the powder size and uniformity are phosphor important indicator of its impact on the system of lights more visible. 本发明通过对原料粒径的控制和软化学制备法,获得了中心粒径(D50)可以在1~5um范围内任意变化的白色LED用荧光粉,而且提高了粒度分布的均匀性。 The present invention is by the raw material particle size control and soft chemical preparation method to obtain a center diameter (D50) which can be changed in the range of 1 ~ 5um white LED with a phosphor, but also improves the uniformity of particle size distribution.

在上述方法中,在所述步骤(3)中,即在上述原料中加入助熔剂,并混合均匀。 In the above method, the step (3), i.e. added to the flux in the above-described raw material, and mixed well. 加入助熔剂可以提高晶体形成的质量,从而可以提高荧光粉的性能。 Add the flux can improve the quality of the crystals formed, which can improve the performance of the phosphor.

本发明的优点是:(1)通过改变基质元素的组成及调节各元素的比例可以得到发光强度高主峰位置可以任意变化的白色LED用荧光粉;(2)在激活剂中加入Tb,Eu,Dy,Pr,Mn等新物质可以改变粉的发射主峰位置;提高了粉的发光强度(3)通过共沉淀方法对原材料进行预处理,可以得到范围在1~4um任意中心粒径的荧光粉,而且提高了粒度分布的均匀性。 Advantage of the present invention are: (1) can be obtained as a white LED with a phosphor emitting high intensity peak position can be changed by changing the composition of the matrix element and adjusting the ratio of each element; (2) addition of Tb, Eu in the active agent, dy, Pr, Mn, and other new materials can change the transmission peak position of powder; increasing the luminous intensity of powder (3) pretreatment of raw materials by coprecipitation method, can be obtained in the range of phosphor 1 ~ 4um any center particle diameter, and improves the uniformity of particle size distribution.

本发明所得的荧光粉可用于制造白色发光二极管。 The resultant of the present invention phosphor may be used for producing white light emitting diode.

具体实施方式 Detailed ways

实施例1:称取Y2O33.1316g,Gd2O31.6753g,Al(OH)34.9736g,CeO20.2195g,再加入总重量1%的助熔剂BaF2、H3BO3,以上原料均为优级纯,将以上原料混磨均匀以后,在1400℃还原条件下焙烧2小时,即得到分子组成为Y2.175Gd0.725Al5O12:Ce0.1的样品,其发射主峰波长高于比较例,亮度高于比较例。 Example 1: Weigh Y2O33.1316g, Gd2O31.6753g, Al (OH) 34.9736g, CeO20.2195g, added 1% of the total weight of the flux BaF2, H3BO3, the above raw materials are excellent pure, the above raw material mixture after grinding uniform, and calcined for 2 hours at 1400 deg.] C reducing conditions to obtain molecular composition Y2.175Gd0.725Al5O12: sample Ce0.1 which emission peak wavelength higher than Comparative Example, a brightness above Comparative Examples.

比较例:称取Y2O34.596g,Al(OH)35.2874g,CeO20.1166g,其助熔剂含量及制造方法均与实施例1相同,得到分子组成为Y2.94Al5O12:Ce0.1的样品。 Comparative Example: Weigh Y2O34.596g, Al (OH) 35.2874g, CeO20.1166g, which flux content and manufacturing method were the same as in Example 1, to obtain molecules of Y2.94Al5O12: Ce0.1 sample.

实施例2~实施例71:改变实施例1的基质、激活剂,按照以下分子式的化学剂量比合成样品其相对亮度和发射主峰波长列于表中。 Example 2 ~ Example 71: changing the matrix, the activator of Example 1, the following formula stoichiometry of the relative luminance and emission peak wavelengths shown in Table ratio of synthetic samples.

表1 Table 1

实施例72:用共沉淀方法对原料进行预处理,通过共沉淀控制原料的粒径,可以得到范围在1-4um任意中心粒径的荧光粉,而且提高了粒度分布的均匀性。 Example 72: raw material is pretreated using a coprecipitation method, coprecipitation controlling the particle size of raw materials, can be obtained in the range of 1-4um any central particle diameter of the phosphor, but also improves the uniformity of particle size distribution. 另一方面由于共沉淀会使原料混合更加均匀,从而会使荧光粉的发光强度有所提高。 On the other hand due to the coprecipitation make material more uniform mixing, so will the light emission intensity of phosphor is improved. 按Y1.45Gd1.45Al5O12:Ce0.1比例称取Y2O31.9637g,Gd2O33.1516g,Al(NO3)3·9H2O22.73g,CeO20.2065g,以上原料均为优级纯,首先用沸腾的硝酸将Y2O3,Gd2O3,Al(NO3)3·9H2O,CeO2,分别溶解,在将各溶液相互均匀混合,熔液仍然澄清。 Press Y1.45Gd1.45Al5O12: Ce0.1 ratio weighed Y2O31.9637g, Gd2O33.1516g, Al (NO3) 3 · 9H2O22.73g, CeO20.2065g, the above raw materials are excellent pure, first with boiling nitric Y2O3 , Gd2O3, Al (NO3) 3 · 9H2O, CeO2, were dissolved, each solution is uniformly mixed with each other, melt remains clear. 向其中加入草酸溶液,通过控制加入草酸的浓度和速度可以控制原料的粒度。 To this was added oxalic acid solution by controlling the addition of oxalic acid concentration and speed can be controlled size of the material. 沉淀下来的物质经850℃烧结后得到处理后的原料,本样原料中心粒径0.3um。 After firing 850 ℃ for precipitated material obtained feedstock treated, the present sample material center particle diameter 0.3um. 再加入总重量1%的助熔剂BaF2、H3BO3,混磨均匀,在1400℃还原条件下焙烧2小时得到样品,中心粒径为0.934nm。 Then add 1% of the total weight of the flux BaF2, H3BO3, mixed grinding uniform, fired at 1400 deg.] C reduction for 2 hours to give a sample, the central particle diameter of 0.934nm. 其亮度高于比较例。 Whose luminance is higher than the Comparative Example.

实施例73~78:按照实施例72的方法溶解各原料,通过加入草酸的浓度和速度来控制沉降速度,制成的原料粒度分别为0.5、1.0、1.5、2.0、2.5、3.0um的荧光粉。 Examples 73 to 78: dissolve the starting material according to the method of Example 72, to control the sedimentation rate by the addition of concentration and velocity of oxalic acid, the raw material particle size prepared were phosphors 0.5,1.0,1.5,2.0,2.5,3.0um of . 用此原料制成的样品的相对亮度和中心粒径列于表2表2 The relative brightness and the center of the sample using this raw material of particle diameter shown in Table 2. Table 2

综上所述,本发明的荧光粉具有发光亮度高、粒度均匀、发射波长可根据需要调节、激发波长宽、化学稳定性好等特点,制造方法简单、无污染、成本低。 As described above, the phosphor of the present invention has high emission luminance, a uniform particle size, the emission wavelength can be adjusted as needed, excitation wave length and width, good chemical stability, a manufacturing method is simple, no pollution, and low cost.

Claims (3)

1.一种蓝光激发的白色LED用荧光粉,其特征在于:该蓝光激发的白色LED用荧光粉的结构式为:R(3-xy)M5O12:CexR′y;其中:R为Y,Gd,Lu,Sc,La和Sm中至少一种;M为B,Al,Ga,In,P,Ge和Zn中至少一种;0.1≤x<1;R'可以为Eu,Dy,Pr和Mn中的一种或几种;0<y<0.5。 A blue light excited white LED with a phosphor, wherein: the formula the blue excited white LED with a phosphor are: R (3-xy) M5O12: CexR'y; wherein: R is Y, Gd, Lu, Sc, La and Sm, at least one; M is B, Al, Ga, in, P, Ge, and Zn at least one; 0.1≤x <1; R 'may be Eu, Dy, Pr, and Mn one or more; 0 <y <0.5.
2.根据权利要求1所述的蓝光激发的白色LED用荧光粉,其特征在于:所述的荧光粉的中心粒径(D50)在1~5um范围内。 The blue light excited white LED with a phosphor according to claim 1, wherein: said central particle diameter of the phosphor (D50) of in the range of 1 ~ 5um.
3.一种制造权利要求1所述的蓝光激发的白色LED用荧光粉的方法,其特征在于:该方法包括下述步骤:(1)按结构式:R(3-xy)M5O12:CexR′y进行配料,其中:R为Y,Gd,Lu,Sc,La和Sm中至少一种,M为B,Al,Ga,In,P,Ge和Zn中至少一种,0.1≤x<1,R′为Eu,Dy,Pr和Mn中一种或几种,0<y<0.5,按照上述的结构式的配比称取上述元素的单质、或其氧化物、或其相应盐类,作为原料;(2)将上述原料进行共沉淀处理;(3)在上述原料中加入助熔剂,并混合均匀,所述的助熔剂为碱土金属、稀土金属、铝、镓、铟的任意一种的氟化物或氯化物,硼酸、氧化硼中至少一种,所述的助熔剂占总重量即助熔剂和上述原料的重量的百分比为0.001%~10wt%;(4)然后进行还原焙烧,还原焙烧温度为1100~1600℃,还原焙烧时间为0.5~15h;(5)将上述还原产物洗涤,过滤,烘干,得到最终产品 The method of the blue light excited white LED with a phosphor 3. A method of manufacturing as claimed in claim 1, wherein: the method comprising the steps of: (1) by the structural formula: R (3-xy) M5O12: CexR'y compounding, wherein: R is Y, Gd, Lu, Sc, La and Sm at least one, M is B, Al, Ga, in, P, Ge, and Zn at least one, 0.1≤x <1, R 'one for the Eu, Dy, Pr, and Mn or more, 0 <y <0.5, according to the above formula the ratio of said elemental take the above elements, or an oxide thereof, or the corresponding salts, as a starting material; (2) the raw material coprecipitation process; (3) was added flux in the raw material and mixed uniformly, the flux is any rare earth metal, aluminum, gallium, indium, a fluoride or chloride, boric acid, boron oxide of at least one of said flux total weight i.e. the weight percent of the flux and the raw material is 0.001% ~ 10wt%; (4) followed by reductive roasting, reduction roasting temperature 1100 ~ 1600 ℃, reduction roasting time of 0.5 ~ 15h; (5) above was washed reduction product, filtering and drying, to give the final product .
CN 02130949 2002-09-13 2002-09-13 Blue light-excitated white phosphor powder for LED and production method thereof CN1318540C (en)

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