CN102517016A - Solid solution fluorescent light-emitting material for blue light excitation and preparation method thereof - Google Patents

Abstract

The invention provides a solid solution fluorescent material for blue light excitation, which has the atomic ratio shown in formula (I). The present invention also provides a method for preparing a solid solution fluorescent light-emitting material for blue light excitation, comprising the following steps: mixing RE-containing compounds, Ce-containing compounds, M-containing compounds, Mn-containing compounds, A-containing compounds and D-containing compounds, A mixture is obtained; the mixture is calcined under a reducing atmosphere to obtain a solid solution fluorescent material for blue light excitation. The performance of the solid solution fluorescent luminescent material provided by the present invention is stable, so that the performance of the white light LED is also relatively stable; the solid solution fluorescent luminescent material provided by the present invention has an emission spectrum that obviously expands to the red light region when excited by blue light, which improves the display of the solid solution fluorescent luminescent material. Color performance, and its emission spectrum is adjustable to meet the needs of different occasions. In addition, the preparation method of the solid solution fluorescent luminescent material provided by the present invention is simple, feasible and easy to operate.

Description

Solid solution fluorescent luminescent material for blue light excitation and preparation method thereof

technical field

The invention belongs to the technical field of luminescent materials, and in particular relates to a solid solution fluorescent luminescent material for blue light excitation and a preparation method thereof.

Background technique

White light-emitting diode (LED) is a semiconductor device that can convert electrical energy into visible light. It has many advantages such as small size, energy saving, long life, and no pollution. It has broad application value and huge market prospects. At present, white light LEDs have been applied in many fields such as LCD backlights, indicator lights, and general lighting, and will replace various bulbs and fluorescent lamps currently used as a new generation of green lighting sources. Aspects such as quality of life have broad and far-reaching implications.

The prior art discloses a variety of deployment methods for white LEDs, mainly including the following three:

(1) Multi-chip light mixing technology: fix red, blue and green three chips or blue and yellow double chips in the same package, and then adjust the current of each chip and the light output of each chip to control the light mixing ratio , to achieve the goal of mixing white light;

(2) Excite evenly mixed blue, green and red phosphors with ultraviolet LEDs, so that a certain proportion of the three primary colors are excited to mix light to output white;

(3) Yellow YAG (Yttrium Aluminum Garnet) phosphor is mixed around the blue LED, and a blue LED with a wavelength of 400-530nm is used to emit light to excite the yellow YAG phosphor to produce yellow light. The original blue light is mixed to form a two-wavelength white light mixed with blue and yellow.

Among them, the method (3) has the advantages of simple method and low cost, and is a relatively commonly used method. At present, in the prior art, yttrium aluminum garnet (YAG:Ce ³⁺ ) fluorescent materials doped with cerium ions are generally combined with blue LEDs to realize white light through the principle of complementary colors. However, the red component in the fluorescent powder is insufficient, and the color rendering property is poor.

In order to increase the content of red components in the fluorescent powder to improve the color rendering and adjustability of white light, the prior art discloses a method of combining blue LEDs with green fluorescent powder and red fluorescent powder to generate white light. However, at present, green phosphors and red phosphors are mainly oxide-based phosphors, sulfide-based phosphors, and nitride-based phosphors. Among them, oxide-based phosphors have weak absorption in the visible light region and are difficult to combine with blue phosphors. LED matching; sulfide-based phosphors have poor thermal and chemical stability, and long-term use will lead to attenuation of luminescence; although nitride-based phosphors have excellent optical properties, the preparation conditions are harsh and the cost is high. In addition, there are differences in properties between the red phosphor and the green phosphor, and the obtained white LED may have problems such as unstable performance in practical applications. Therefore, the research and development of single-matrix luminescent materials with tunable emission spectrum is an important issue for LED luminescent materials.

Contents of the invention

In view of this, the technical problem to be solved by the present invention is to provide a solid solution fluorescent luminescent material for blue light excitation and its preparation method. The solid solution fluorescent luminescent material provided by the present invention has stable performance, good color rendering performance and adjustable performance.

The present invention provides a solid solution fluorescent light-emitting material for blue light excitation, which has the atomic ratio shown in formula (I):

(1-x)[RE _3-y Ce _y M ₅ O ₁₂ ]·x[A _3-z Mn _z M ₂ (DO ₄ ) ₃ ](I);

In formula (I), RE is one or more of Y, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu;

M is one or more of B, Al, Ga and In;

A is one or more of Mg, Ca, Sr and Ba;

D is one or more of Si, Ge and Sn;

0<x≤0.50;

0<y≤0.30;

0<z≤3.

Preferably, said M is one or both of B and Al.

The present invention also provides a method for preparing a solid solution fluorescent light-emitting material for blue light excitation described in the above technical solution, comprising the following steps:

Mixing RE-containing compounds, Ce-containing compounds, M-containing compounds, Mn-containing compounds, A-containing compounds and D-containing compounds to obtain a mixture;

The mixture is calcined under a reducing atmosphere to obtain a solid solution fluorescent material for blue light excitation.

Preferably, the RE-containing compound is one or more of RE-containing oxides, hydroxides, nitrates, halides and carbonates.

Preferably, the Ce-containing compound is one or more of Ce-containing oxides, hydroxides, nitrates, halides and carbonates.

Preferably, the M-containing compound is one or more of M-containing oxides, hydroxides and oxyacids.

Preferably, the A-containing compound is one or more of A-containing oxides, hydroxides, nitrates, halides and carbonates, and the Mn-containing compound is Mn-containing oxides, hydroxides One or more of compounds, nitrates, halides and carbonates.

Preferably, the D-containing compound is one or more of D-containing oxides, hydroxides and oxyacids.

Preferably, the mixture further includes a fluoride flux.

Preferably, the calcination temperature is 1400°C-1700°C, and the calcination time is 1h-20h.

Compared with the prior art, the solid solution fluorescent material for blue light excitation provided by the present invention has the atomic ratio composition shown in formula (I), is a garnet-based solid solution, and is doped with Ce and Mn. The performance of the solid solution fluorescent luminescent material provided by the present invention is stable, so that the performance of the white light LED is relatively stable; the excitation spectrum range of the solid solution fluorescent luminescent material provided by the present invention is relatively wide, and there is strong absorption at 450nm, which can be perfectly matched with commercial blue chips Combined, a white light LED with good performance is obtained; the solid solution fluorescent luminescent material provided by the present invention has an emission spectrum that obviously expands to the red light region under blue light excitation, which improves the color rendering performance of the solid solution fluorescent luminescent material, and its emission spectrum is adjustable to meet The needs of different occasions. In addition, the preparation method of the solid solution fluorescent luminescent material provided by the present invention is simple, feasible, easy to operate, easy to mass produce, pollution-free, and low in cost.

Description of drawings

Fig. 1 is the XRD spectrum of the fluorescent powder prepared in Example 8 of the present invention;

Fig. 2 is the photoemission spectrum of the fluorescent powder prepared in Example 8 of the present invention under the excitation of 450nm blue light;

Fig. 3 is the XRD spectrum of the fluorescent powder prepared in Example 16 of the present invention;

Fig. 4 is the photoemission spectrum of the phosphor powder prepared in Example 16 of the present invention under the excitation of 450nm blue light;

Fig. 5 is the photoluminescence spectrum of the fluorescent powder prepared in Comparative Example 1 of the present invention under the excitation of 450nm blue light;

Fig. 6 is the photoluminescence spectrum of the fluorescent powder prepared in Comparative Example 2 of the present invention under the excitation of 450nm blue light.

Detailed ways

The present invention provides a solid solution fluorescent light-emitting material for blue light excitation, which has the atomic ratio shown in formula (I):

(1-x)[RE _3-y Ce _y M ₅ O ₁₂ ]·x[A _3-z Mn _z M ₂ (DO ₄ ) ₃ ](I);

In formula (I), RE is one or more of Y, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu, preferably Y, Pr, Nd, Sm, Gd One or more of , Tb, Dy, Er, Tm, Yb and Lu;

M is one or more of B, Al, Ga and In, preferably one or both of B and Al;

A is one or more of Mg, Ca, Sr and Ba, preferably one or more of Mg, Ca and Sr;

D is one or more of Si, Ge and Sn, preferably one or more of Si and Ge;

0<x≤0.50, preferably, x satisfies the following condition: 0.01≤x≤0.45; more preferably, x satisfies the following condition: 0.05≤x≤0.40;

0<y≤0.30, preferably, y satisfies the following condition: 0.01≤y≤0.25; more preferably, y satisfies the following condition: 0.05≤y≤0.20;

0<z≤3, preferably, z satisfies the following condition: 0.01≤z≤2.5; more preferably, z satisfies the following condition: 0.05≤z≤2.

In the present invention, the solid solution fluorescent luminescent material is a garnet-based solid solution, and is doped with Ce and Mn, so that its emission spectrum under blue light excitation extends to the red light region, thereby having good color rendering performance; in addition , the solid solution fluorescent luminescent material has good adjustability, so that its emission spectrum under blue light can be adjusted, so as to meet the needs of different occasions.

The present invention also provides a method for preparing a solid solution fluorescent light-emitting material for blue light excitation described in the above technical solution, comprising the following steps:

Mixing RE-containing compounds, Ce-containing compounds, M-containing compounds, Mn-containing compounds, A-containing compounds and D-containing compounds to obtain a mixture;

The mixture is calcined under a reducing atmosphere to obtain a solid solution fluorescent material for blue light excitation.

In the present invention, at first each raw material is mixed, obtains mixture, wherein:

The RE-containing compound is preferably one or more of RE-containing oxides, hydroxides, nitrates, halides and carbonates, more preferably RE-containing oxides, hydroxides, halides and One or more of carbonates; the RE is one or more of Y, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu, preferably Y, One or more of Pr, Nd, Sm, Gd, Tb, Dy, Er, Tm, Yb and Lu;

The Ce-containing compound is preferably one or more of Ce-containing oxides, hydroxides, nitrates, halides and carbonates, more preferably Ce-containing oxides, hydroxides, halides and One or more of carbonates;

The M-containing compound is preferably one or more of M-containing oxides, hydroxides and oxyacids, more preferably one or both of M-containing oxides and hydroxides; the M is one or more of B, Al, Ga and In, preferably one or both of B and Al;

The A-containing compound is preferably one or more of A-containing oxides, hydroxides, nitrates, halides and carbonates, more preferably A-containing oxides, hydroxides, halides and One or more of carbonates; said A is one or more of Mg, Ca, Sr and Ba, preferably one or more of Mg, Ca and Sr;

The Mn-containing compound is preferably one or more of Mn-containing oxides, hydroxides, nitrates, halides and carbonates, more preferably Mn-containing oxides, hydroxides, halides and One or more of carbonates;

The D-containing compound is preferably one or more of D-containing oxides, hydroxides and oxyacids, more preferably one or both of D-containing oxides and hydroxides; the D is one or more of Si, Ge and Sn, preferably one or more of Si and Ge.

The raw materials are thoroughly ground and mixed uniformly to obtain a mixture; the mixture is roasted in a reducing atmosphere to obtain a solid solution fluorescent material having an atomic ratio shown in formula (I) for blue light excitation. In the present invention, the reducing atmosphere can be a gas atmosphere produced by burning carbon in air, or a reducing gas atmosphere composed of hydrogen and nitrogen, and the volume ratio of hydrogen and nitrogen is preferably (1-20):( 99 to 80), more preferably (5 to 15): (95 to 85); the temperature of the calcination is preferably 1400°C to 1700°C, more preferably 1450°C to 1650°C, most preferably 1500°C to 1600°C ; The roasting time is preferably 1h-20h, more preferably 3h-18h, more preferably 5h-15h.

In order to reduce the difficulty of roasting, the present invention preferably adds a fluoride flux to the mixture of various raw materials. The fluoride flux is preferably ammonium fluoride, ammonium bifluoride, lithium fluoride, alkaline earth metal fluoride and rare earth metal fluoride. One or more of, more preferably one or more of alkaline earth metal fluorides and rare earth metal fluorides. The added amount of the fluxing agent is preferably 5% or less of the mixture composed of the various raw materials, more preferably 0.5% to 4.5%, most preferably 1% to 4%.

After the calcination is completed, the obtained sintered body is ground and dispersed to obtain a solid solution fluorescent material for blue light excitation.

After the solid solution fluorescent luminescent material is obtained, XRD analysis is performed on the solid solution fluorescent luminescent material, and the result shows that it has the atomic ratio composition shown in formula (I);

The solid solution fluorescent luminescent material is excited by blue light with a wavelength of 450nm. The results show that the solid solution fluorescent luminescent material prepared by the present invention has a wide excitation spectrum range, strong absorption at 450nm, and can be better combined with blue light chips; meanwhile, the present invention prepares The emission spectrum of the phosphor powder is obviously broadened to the red light region, which can improve the color rendering of white light.

The solid solution fluorescent material for blue light excitation provided by the present invention has the atomic ratio composition shown in formula (I), is a garnet-based solid solution, and is doped with Ce and Mn. The performance of the solid solution fluorescent luminescent material provided by the present invention is stable, so that the performance of the white light LED is relatively stable; the excitation spectrum range of the solid solution fluorescent luminescent material provided by the present invention is relatively wide, and there is strong absorption at 450nm, which can be perfectly matched with commercial blue chips Combined, a white light LED with good performance is obtained; the solid solution fluorescent luminescent material provided by the present invention has an emission spectrum that obviously expands to the red light region under blue light excitation, which improves the color rendering performance of the solid solution fluorescent luminescent material, and its emission spectrum is adjustable to meet The needs of different occasions. In addition, the preparation method of the solid solution fluorescent luminescent material provided by the present invention is simple, feasible, easy to operate, easy to mass produce, pollution-free, and low in cost.

In order to further illustrate the present invention, the solid solution fluorescent material for blue light excitation provided by the present invention and its preparation method are described in detail below in conjunction with examples.

Example 1

Weigh 33.02 grams of Y ₂ O ₃ , 25.24 grams of Al ₂ O ₃ , 0.15 grams of SiO ₂ , 0.29 grams of MnCO ₃ and 0.86 grams of CeO ₂ , carry out thorough grinding and mixing, put the resulting mixture into an alumina crucible, and Cover the surface of the mixture with a layer of carbon powder, cover the crucible lid, put it into a high-temperature furnace, bake it at 1700 ° C for 4 hours, take it out when it is cooled to 1000 ° C, remove the carbon, grind and disperse, and obtain the garnet-based crystal for blue light excitation. The solid solution phosphor is composed of Y _2.925 Ce _0.05 Mn _0.025 Al _4.975 Si _0.025 O ₁₂ .

Carry out XRD analysis to described fluorescent powder, the result shows that it has above-mentioned atomic ratio composition;

Excite the fluorescent powder with a wavelength of 450nm blue light, the results show that the fluorescent powder prepared by the present invention has a wide excitation spectrum range, strong absorption at 450nm, and can be combined with a blue light chip; the emission of the fluorescent powder prepared by the present invention The spectrum is broadened to the red light region, which can improve the color rendering of white light.

Example 2

Weigh 32.46 grams of Y ₂ O ₃ , 8.51 grams of Pr ₆ O ₁₁ , 25.24 grams of Al ₂ O ₃ , 0.15 grams of SiO ₂ , 0.29 grams of MnCO ₃ and 0.86 grams of CeO ₂ , carry out thorough grinding and mixing, and put the obtained mixture into the oxidation In an aluminum crucible, cover a layer of carbon powder on the surface of the mixture, cover the crucible lid, put it into a high-temperature furnace, bake it at 1700°C for 4 hours, take it out when it is cooled to 1000°C, remove the carbon, grind and disperse, and obtain The garnet-based solid solution phosphor excited by blue light has a composition of Y _2.875 Pr _0.50 Ce _0.05 Mn _0.025 Al _4.975 Si _0.025 O ₁₂ .

Carry out XRD analysis to described fluorescent powder, the result shows that it has above-mentioned atomic ratio composition;

Excite the fluorescent powder with a wavelength of 450nm blue light, the results show that the fluorescent powder prepared by the present invention has a wide excitation spectrum range, strong absorption at 450nm, and can be combined with a blue light chip; the emission of the fluorescent powder prepared by the present invention The spectrum is broadened to the red light region, which can improve the color rendering of white light.

Example 3

Weigh 29.07 grams of Y ₂ O ₃ , 4.21 grams of Nd ₂ O ₃ , 24.85 grams of Al ₂ O ₃ , 0.75 grams of SiO ₂ , 0.40 grams of MgO, 0.29 grams of MnCO ₃ and 0.86 grams of CeO ₂ , carry out thorough grinding and mixing, and obtain Put the mixture into an alumina crucible, cover the crucible lid, put it into a high-temperature furnace, and roast it for 20 hours at 1500°C in a 10% H ₂ /N ₂ atmosphere, take it out when it is cooled to room temperature, grind and disperse it, and obtain The garnet-based solid solution phosphor excited by blue light has a composition of Y _2.575 Nd _0.25 Ce _0.05 Mg _0.10 Mn _0.025 Al _4.875 Si _0.125 O ₁₂ .

Carry out XRD analysis to described fluorescent powder, the result shows that it has above-mentioned atomic ratio composition;

Excite the fluorescent powder with a wavelength of 450nm blue light, the results show that the fluorescent powder prepared by the present invention has a wide excitation spectrum range, strong absorption at 450nm, and can be combined with a blue light chip; the emission of the fluorescent powder prepared by the present invention The spectrum is broadened to the red light region, which can improve the color rendering of white light.

Example 4

Weigh 31.90 grams of Y ₂ O ₃ , 24.85 grams of Al ₂ O ₃ , 0.75 grams of SiO ₂ , 1.44 grams of MnCO ₃ and 0.86 grams of CeO ₂ , carry out thorough grinding and mixing, put the obtained mixture into an alumina crucible, and cover the crucible cover, put it into a high-temperature furnace, and bake it for 12 hours at 1500°C in a 10% H ₂ /N ₂ atmosphere, take it out when it is cooled to room temperature, and grind and disperse it to obtain a garnet-based solid solution phosphor for blue light excitation. The composition is Y _2.825 Ce _0.05 Mn _0.125 Al _4.875 Si _0.125 O ₁₂ .

Carry out XRD analysis to described fluorescent powder, the result shows that it has above-mentioned atomic ratio composition;

Excite the fluorescent powder with a wavelength of 450nm blue light, the results show that the fluorescent powder prepared by the present invention has a wide excitation spectrum range, strong absorption at 450nm, and can be combined with a blue light chip; the emission of the fluorescent powder prepared by the present invention The spectrum is broadened to the red light region, which can improve the color rendering of white light.

Example 5

Weigh 30.77 grams of Y ₂ O ₃ , 1.74 grams of Sm ₂ O ₃ , 24.85 grams of Al ₂ O ₃ , 0.75 grams of SiO ₂ , 0.50 grams of CaCO ₃ , 0.87 grams of MnCO ₃ and 0.86 grams of CeO ₂ , and carry out thorough grinding and mixing to obtain Put the mixture into an alumina crucible, cover the crucible lid, put it into a high-temperature furnace, and bake it for 6 hours at 1500 ° C under a 10% H ₂ /N ₂ atmosphere, take it out when it is cooled to room temperature, grind and disperse it, and obtain The garnet-based solid solution phosphor excited by blue light has a composition of Y _2.725 Sm _0.10 Ce _0.05 Ca _0.05 Mn _0.075 Al _4.875 Si _0.125 O ₁₂ .

Carry out XRD analysis to described fluorescent powder, the result shows that it has above-mentioned atomic ratio composition;

Excite the fluorescent powder with a wavelength of 450nm blue light, the results show that the fluorescent powder prepared by the present invention has a wide excitation spectrum range, strong absorption at 450nm, and can be combined with a blue light chip; the emission of the fluorescent powder prepared by the present invention The spectrum is broadened to the red light region, which can improve the color rendering of white light.

Example 6

Weigh 30.48 grams of Y ₂ O ₃ , 24.22 grams of Al ₂ O ₃ , 1.50 grams of SiO ₂ , 2.87 grams of MnCO ₃ and 0.86 grams of CeO ₂ , carry out thorough grinding and mixing, put the obtained mixture into an alumina crucible, and cover the crucible cover, put it into a high-temperature furnace, and bake it at 1550° C. under a 15% H ₂ /N ₂ atmosphere for 6 hours, take it out when it is cooled to room temperature, and grind and disperse it to obtain a garnet-based solid solution phosphor for blue light excitation. The composition is Y _2.70 Ce _0.05 Mn _0.25 Al _4.75 Si _0.25 O ₁₂ .

Carry out XRD analysis to described fluorescent powder, the result shows that it has above-mentioned atomic ratio composition;

Excite the fluorescent powder with a wavelength of 450nm blue light, the results show that the fluorescent powder prepared by the present invention has a wide excitation spectrum range, strong absorption at 450nm, and can be combined with a blue light chip; the emission of the fluorescent powder prepared by the present invention The spectrum is broadened to the red light region, which can improve the color rendering of white light.

Example 7

Weigh 19.19 g of Y ₂ O ₃ , 18.13 g of Gd ₂ O ₃ , 24.22 g of Al ₂ O ₃ , 1.50 g of SiO ₂ , 1.47 g of SrCO ₃ , 1.97 g of BaCO ₃ , 0.57 g of MnCO ₃ and 0.86 g of CeO ₂ . Grinding and mixing, put the obtained mixture into an alumina crucible, cover the crucible lid, put it into a high-temperature furnace, and bake it at 1500°C and 15% H ₂ /N ₂ atmosphere for 5 hours, take it out when it is cooled to room temperature, and grind it After dispersion, a garnet-based solid solution phosphor for blue light excitation is obtained, the composition of which is Y _1.70 Gd _1.00 Ce _0.05 Sr _0.10 Ba _0.10 Mn _0.05 Al _4.75 Si _0.25 O ₁₂ .

Carry out XRD analysis to described fluorescent powder, the result shows that it has above-mentioned atomic ratio composition;

Excite the fluorescent powder with a wavelength of 450nm blue light, the results show that the fluorescent powder prepared by the present invention has a wide excitation spectrum range, strong absorption at 450nm, and can be combined with a blue light chip; the emission of the fluorescent powder prepared by the present invention The spectrum is broadened to the red light region, which can improve the color rendering of white light.

Example 8

Weigh 29.92 grams of Y ₂ O ₃ , 23.96 grams of Al ₂ O ₃ , 1.80 grams of SiO ₂ , 3.45 grams of MnCO ₃ and 0.86 grams of CeO ₂ , carry out thorough grinding and mixing, put the obtained mixture into an alumina crucible, and cover the crucible cover, put it into a high-temperature furnace, and bake it at 1600°C in a 10% H ₂ /N ₂ atmosphere for 3 hours, take it out when it is cooled to room temperature, and grind and disperse it to obtain a garnet-based solid solution phosphor for blue light excitation. The composition is Y _2.65 Ce _0.05 Mn _0.30 Al _4.70 Si _0.30 O ₁₂ .

Carry out XRD analysis to described fluorescent powder, see Fig. 1 for the result, Fig. 1 is the XRD spectrum of the fluorescent powder prepared in the embodiment of the present invention 8, as can be seen from Fig. 1, the phosphor powder prepared in the embodiment of the present invention has the above atomic ratio composition ;

Excite the fluorescent powder with a wavelength of 450nm blue light, the results are shown in Figure 2, Figure 2 is the photoemission spectrum of the fluorescent powder prepared in Example 8 of the present invention under the excitation of 450nm blue light, as can be seen from Figure 2, the present invention prepared The phosphor powder has a wide range of excitation spectrum and strong absorption at 450nm, and can be better combined with blue light chips; the emission spectrum of the phosphor powder prepared by the invention is broadened to the red light region, which can improve the color rendering of white light.

Example 9

Weigh 30.78 grams of Y(OH) _{3 ,} 9.35 grams of Tb ₄ O ₇ , 23.71 grams of Al ₂ O ₃ , 0.62 grams of H ₃ BO ₃ , 1.50 grams of SiO ₂ , 2.50 grams of CaCO ₃ and 0.86 grams of CeO ₂ , and carry out thorough grinding and mixing , put the obtained mixture into an alumina crucible, cover the crucible lid, put it into a high-temperature furnace, and bake it at 1400°C and 20% H ₂ /N ₂ atmosphere for 16 hours, take it out when it is cooled to room temperature, grind and disperse , to obtain a garnet-based solid solution phosphor for blue light excitation, whose composition is Y _2.20 Tb _0.50 Ce _0.05 Ca _0.25 Al _4.65 B _0.10 Si _0.25 O ₁₂ .

Carry out XRD analysis to described fluorescent powder, the result shows that it has above-mentioned atomic ratio composition;

Excite the fluorescent powder with a wavelength of 450nm blue light, the results show that the fluorescent powder prepared by the present invention has a wide excitation spectrum range, strong absorption at 450nm, and can be combined with a blue light chip; the emission of the fluorescent powder prepared by the present invention The spectrum is broadened to the red light region, which can improve the color rendering of white light.

Example 10

Weigh 31.24 grams of YCl ₃ , 19.90 grams of Lu ₂ O ₃ , 24.22 grams of Al ₂ O ₃ , 1.95 grams of H ₂ SiO ₃ , 0.40 grams of MgO, 2.21 grams of SrCO ₃ and 2.96 grams of CeF ₃ , and carry out thorough grinding and mixing to obtain Put the mixture into an alumina crucible, cover the surface of the mixture with a layer of carbon powder, cover the crucible lid, put it in a high-temperature furnace, bake it at 1650°C for 3 hours, take it out when it is cooled to 1000°C, remove the carbon, and grind After dispersion, the garnet-based solid solution phosphor for blue light excitation is obtained, and its composition is Y _1.60 Lu _1.00 Ce _0.15 Sr _0.15 Mg _0.10 Al _4.75 Si _0.25 O ₁₂ .

Carry out XRD analysis to described fluorescent powder, the result shows that it has above-mentioned atomic ratio composition;

Excite the fluorescent powder with a wavelength of 450nm blue light, the results show that the fluorescent powder prepared by the present invention has a wide excitation spectrum range, strong absorption at 450nm, and can be combined with a blue light chip; the emission of the fluorescent powder prepared by the present invention The spectrum is broadened to the red light region, which can improve the color rendering of white light.

Example 11

Weigh 31.24 grams of YCl _{3 ,} 9.33 grams of Dy ₂ O ₃ , 17.25 grams of Tb(NO ₃ ) ₃ , 24.22 grams of Al ₂ O ₃ , 1.50 grams of SiO ₂ , 2.17 grams of MnO ₂ and 2.58 grams of CeO ₂ , carry out thorough grinding and mixing, Put it into an alumina crucible, put the obtained mixture into an alumina crucible, cover the surface of the mixture with a layer of carbon powder, cover the crucible lid, put it into a high-temperature furnace, bake it at 1500°C for 8 hours, and cool it to Take it out at 1000°C, remove the carbon, and grind and disperse to obtain a garnet-based solid solution phosphor for blue light excitation, the composition of which is Y _1.60 Tb _0.50 Dy _0.50 Ce _0.15 Mn _0.25 Al _4.75 Si _0.25 O ₁₂ .

Carry out XRD analysis to described fluorescent powder, the result shows that it has above-mentioned atomic ratio composition;

Excite the fluorescent powder with a wavelength of 450nm blue light, the results show that the fluorescent powder prepared by the present invention has a wide excitation spectrum range, strong absorption at 450nm, and can be combined with a blue light chip; the emission of the fluorescent powder prepared by the present invention The spectrum is broadened to the red light region, which can improve the color rendering of white light.

Example 12

Weigh 54.21 grams of Tb ₄ O ₇ , 25.24 grams of Al ₂ O ₃ , 0.30 grams of SiO ₂ , 0.50 grams of CaCO ₃ and 1.63 grams of Ce(NO ₃ ) ₃ , carry out thorough grinding and mixing, and put the obtained mixture into an alumina crucible , cover the crucible lid, put it into a high-temperature furnace, and bake it for 3 hours at 1700 ° C in a 20% H ₂ /N ₂ atmosphere, take it out when it is cooled to room temperature, grind and disperse it, and obtain a garnet-based solid solution for blue light excitation The phosphor powder is composed of Tb _2.90 Ce _0.05 Ca _0.05 Al _4.95 Si _0.05 O ₁₂ .

Carry out XRD analysis to described fluorescent powder, the result shows that it has above-mentioned atomic ratio composition;

Excite the fluorescent powder with a wavelength of 450nm blue light, the results show that the fluorescent powder prepared by the present invention has a wide excitation spectrum range, strong absorption at 450nm, and can be combined with a blue light chip; the emission of the fluorescent powder prepared by the present invention The spectrum is broadened to the red light region, which can improve the color rendering of white light.

Example 13

Weigh 72.55 grams of TbCl ₃ , 9.45 grams of Ho ₂ O ₃ , 22.59 grams of Al ₂ O ₃ , 4.69 grams of Ga ₂ O ₃ , 0.72 grams of H ₄ SiO ₄ , 0.86 grams of MnCO ₃ and 0.86 grams of CeO ₂ , and carry out thorough grinding and mixing, Put the obtained mixture into an alumina crucible, cover the crucible lid, put it into a high-temperature furnace, and bake it for 20 hours at 1400°C in a 10% H ₂ /N ₂ atmosphere, take it out when it is cooled to room temperature, grind and disperse it, A garnet-based solid solution phosphor for blue light excitation is obtained, the composition of which is Tb _2.735 Ho _0.50 Ce _0.15 Mn _0.075 Al _4.425 Ga _0.50 Si _0.075 O ₁₂ .

Carry out XRD analysis to described fluorescent powder, the result shows that it has above-mentioned atomic ratio composition;

Excite the fluorescent powder with a wavelength of 450nm blue light, the results show that the fluorescent powder prepared by the present invention has a wide excitation spectrum range, strong absorption at 450nm, and can be combined with a blue light chip; the emission of the fluorescent powder prepared by the present invention The spectrum is broadened to the red light region, which can improve the color rendering of white light.

Example 14

Weigh 72.55 grams of TbCl ₃ , 9.56 grams of Er ₂ O ₃ , 22.59 grams of Al ₂ O ₃ , 1.74 grams of B ₂ O ₃ , 0.72 grams of H ₄ SiO ₄ , 0.86 grams of MnCO ₃ and 0.86 grams of CeO ₂ , and carry out thorough grinding and mixing, Put the obtained mixture into an alumina crucible, cover the crucible lid, put it into a high-temperature furnace, and bake it for 20 hours at 1400°C in a 10% H ₂ /N ₂ atmosphere, take it out when it is cooled to room temperature, grind and disperse it, A garnet-based solid solution phosphor for blue light excitation is obtained, the composition of which is Tb _2.735 Er _0.50 Ce _0.15 Mn _0.075 Al _4.425 B _0.50 Si _0.075 O ₁₂ .

Carry out XRD analysis to described fluorescent powder, the result shows that it has above-mentioned atomic ratio composition;

Excite the fluorescent powder with a wavelength of 450nm blue light, the results show that the fluorescent powder prepared by the present invention has a wide excitation spectrum range, strong absorption at 450nm, and can be combined with a blue light chip; the emission of the fluorescent powder prepared by the present invention The spectrum is broadened to the red light region, which can improve the color rendering of white light.

Example 15

Weigh 57.70 grams of Lu ₂ O ₃ , 25.24 grams of Al ₂ O ₃ , 0.30 grams of SiO ₂ , 0.57 grams of MnCO ₃ , 0.35 grams of B ₂ O ₃ and 0.86 grams of CeO ₂ . In an aluminum crucible, cover the crucible lid, put it into a high-temperature furnace, and bake it for 3 hours at 1650°C in a 10% H ₂ /N ₂ atmosphere, take it out when it cools down to room temperature, grind and disperse it, and obtain the pomegranate for blue light excitation The stone-based solid solution phosphor is composed of Lu _2.90 Ce _0.05 Mn _0.05 Al _4.85 B _0.10 Si _0.05 O ₁₂ .

Carry out XRD analysis to described fluorescent powder, the result shows that it has above-mentioned atomic ratio composition;

Excite the fluorescent powder with a wavelength of 450nm blue light, the results show that the fluorescent powder prepared by the present invention has a wide excitation spectrum range, strong absorption at 450nm, and can be combined with a blue light chip; the emission of the fluorescent powder prepared by the present invention The spectrum is broadened to the red light region, which can improve the color rendering of white light.

Example 16

Weigh 55.71 grams of Lu ₂ O ₃ , 24.72 grams of Al ₂ O ₃ , 0.90 grams of SiO ₂ , 0.57 grams of MnCO ₃ and 0.86 grams of CeO ₂ , grind and mix them thoroughly, put the resulting mixture into an alumina crucible, and cover the crucible cover, put it into a high-temperature furnace, and bake it at 1600°C in a 10% H ₂ /N ₂ atmosphere for 3 hours, take it out when it is cooled to room temperature, and grind and disperse it to obtain a garnet-based solid solution phosphor for blue light excitation. The composition is Lu _2.80 Ce _0.05 Mn _0.15 Al _4.85 Si _0.15 O ₁₂ .

Carry out XRD analysis on the phosphor powder, see Figure 3 for the results, and Figure 3 is the XRD pattern of the phosphor powder prepared in Example 16 of the present invention. It can be seen from Figure 3 that the phosphor powder prepared in the embodiment of the present invention has the above atomic ratio composition ;

Excite the phosphor powder with a wavelength of 450nm blue light, the results are shown in Figure 4, Figure 4 is the photoemission spectrum of the phosphor powder prepared in Example 16 of the present invention under the excitation of 450nm blue light, as can be seen from Figure 4, the present invention prepared The phosphor powder has a wide range of excitation spectrum and strong absorption at 450nm, and can be better combined with blue light chips; the emission spectrum of the phosphor powder prepared by the invention is broadened to the red light region, which can improve the color rendering of white light.

Example 17

Weigh 45.76 grams of Lu ₂ O ₃ , 9.56 grams of Er ₂ O ₃ , 24.72 grams of Al ₂ O ₃ , 0.30 grams of SiO ₂ , 1.05 grams of GeO ₂ , 0.57 grams of MnCO ₃ and 0.86 grams of CeO ₂ , and carry out thorough grinding and mixing to obtain Put the mixture into an alumina crucible, cover the crucible lid, put it into a high-temperature furnace, and bake it for 3 hours at 1600 ° C under a 10% H ₂ /N ₂ atmosphere, take it out when it is cooled to room temperature, grind and disperse it, and obtain The garnet-based solid solution phosphor excited by blue light is composed of Lu _2.30 Er _0.50 Ce _0.05 Mn _0.15 Al _4.85 Si _0.05 Ge _0.10 O ₁₂ .

Carry out XRD analysis to described fluorescent powder, the result shows that it has above-mentioned atomic ratio composition;

Excite the fluorescent powder with a wavelength of 450nm blue light, the results show that the fluorescent powder prepared by the present invention has a wide excitation spectrum range, strong absorption at 450nm, and can be combined with a blue light chip; the emission of the fluorescent powder prepared by the present invention The spectrum is broadened to the red light region, which can improve the color rendering of white light.

Example 18

Weigh 45.20 grams of Lu(OH) ₃ , 6.77 grams of Y ₂ O ₃ , 169.64 grams of Al(NO ₃ ) ₃ .9H ₂ O, 1.50 grams of SiO ₂ , 0.57 grams of MnCO ₃ , 1.56 grams of CaF ₂ and 2.58 grams of CeO ₂ , Carry out thorough grinding and mixing, put the obtained mixture into an alumina crucible, cover the crucible lid, put it into a high-temperature furnace, and bake it at 1400°C and 10% H ₂ /N ₂ atmosphere for 8 hours, and take it out when it cools to room temperature , after grinding and dispersing, the garnet-based solid solution phosphor for blue light excitation is obtained, the composition of which is Lu _2.00 Y _0.60 Ce _0.15 Mn _0.05 Ca _0.20 Al _4.75 Si _0.25 O ₁₂ .

Carry out XRD analysis to described fluorescent powder, the result shows that it has above-mentioned atomic ratio composition;

Excite the fluorescent powder with a wavelength of 450nm blue light, the results show that the fluorescent powder prepared by the present invention has a wide excitation spectrum range, strong absorption at 450nm, and can be combined with a blue light chip; the emission of the fluorescent powder prepared by the present invention The spectrum is broadened to the red light region, which can improve the color rendering of white light.

Example 19

Weigh 56.27 grams of LuCl ₃ , 13.08 grams of Tb ₄ O ₇ , 66.00 grams of AlCl ₃ , 0.30 grams of SiO ₂ , 2.88 grams of MnCO ₃ and 2.58 grams of CeO ₂ , grind and mix them thoroughly, put them into an alumina crucible, and cover the crucible lid , placed in a high-temperature furnace, baked at 1450°C and 10% H ₂ /N ₂ atmosphere for 3 hours, took it out when cooled to room temperature, and after grinding and dispersing, a garnet-based solid solution phosphor for blue light excitation was obtained. The composition It is Lu _2.00 Tb _0.70 Ce _0.25 Mn _0.05 Al _4.95 Si _0.05 O ₁₂ .

Carry out XRD analysis to described fluorescent powder, the result shows that it has above-mentioned atomic ratio composition;

Excite the fluorescent powder with a wavelength of 450nm blue light, the results show that the fluorescent powder prepared by the present invention has a wide excitation spectrum range, strong absorption at 450nm, and can be combined with a blue light chip; the emission of the fluorescent powder prepared by the present invention The spectrum is broadened to the red light region, which can improve the color rendering of white light.

Example 20

Weigh 49.74 grams of Lu ₂ O ₃ , 1.93 grams of Tm ₂ O ₃ , 24.98 grams of Al ₂ O ₃ , 0.30 grams of SiO ₂ , 0.52 grams of GeO _{2 ,} 1.26 grams of MnCl ₂ and 7.39 grams of CeCl ₃ , and carry out thorough grinding and mixing to obtain Put the mixture into an alumina crucible, cover the crucible lid, put it into a high-temperature furnace, and bake it for 3 hours at 1550 ° C under a 10% H ₂ /N ₂ atmosphere, take it out when it is cooled to room temperature, grind and disperse it, and obtain The garnet-based solid solution phosphor excited by blue light is composed of Lu _2.50 Tm _0.10 Ce _0.30 Mn _0.10 Al _4.90 Si _0.05 Ge _0.05 O ₁₂ .

Carry out XRD analysis to described fluorescent powder, the result shows that it has above-mentioned atomic ratio composition;

Excite the fluorescent powder with a wavelength of 450nm blue light, the results show that the fluorescent powder prepared by the present invention has a wide excitation spectrum range, strong absorption at 450nm, and can be combined with a blue light chip; the emission of the fluorescent powder prepared by the present invention The spectrum is broadened to the red light region, which can improve the color rendering of white light.

Example 21

Weigh 44.77 grams of Lu ₂ O ₃ , 12.75 grams of Al ₂ O ₃ , 14.06 grams of Ga _{2 O 3} , 6.94 grams of In ₂ O 3 , 3.00 grams of SiO ₂ , 5.75 grams of MnCO ₃ and 8.63 grams of CeO ₂ , and carry out thorough grinding and mixing, Put the obtained mixture into an alumina crucible, cover the crucible lid, put it into a high-temperature furnace, and bake it at 1600°C in a 10% H ₂ /N ₂ atmosphere for 3 hours, take it out when it is cooled to room temperature, grind and disperse it, A garnet-based solid solution phosphor for blue light excitation is obtained, the composition of which is Lu _2.25 Ce _0.25 Mn _0.50 Al _2.50 Ga _1.50 In _0.50 Si _0.50 O ₁₂ .

Carry out XRD analysis to described fluorescent powder, the result shows that it has above-mentioned atomic ratio composition;

Excite the fluorescent powder with a wavelength of 450nm blue light, the results show that the fluorescent powder prepared by the present invention has a wide excitation spectrum range, strong absorption at 450nm, and can be combined with a blue light chip; the emission of the fluorescent powder prepared by the present invention The spectrum is broadened to the red light region, which can improve the color rendering of white light.

Example 22

Weigh Lu ₂ O ₃ 43.77 g, Yb ₂ O ₃ 0.99 g, Al ₂ O ₃ 12.75 g, Ga ₂ O ₃ 18.74 g, SiO ₂ 1.50 g, GeO ₂ 2.60 g, MnCO ₃ 5.75 g and CeO ₂ 8.63 g, Carry out thorough grinding and mixing, put it into an alumina crucible, cover the crucible lid, put it into a high-temperature furnace, and bake it for 3 hours at 1500°C in a 10% H ₂ /N ₂ atmosphere, take it out when it is cooled to room temperature, and grind and disperse , to obtain a garnet-based solid solution phosphor for blue light excitation, whose composition is Lu _2.20 Yb _0.05 Ce _0.25 Mn _0.50 Al _2.50 Ga _2.00 Si _0.25 Ge _0.25 O ₁₂ .

Carry out XRD analysis to described fluorescent powder, the result shows that it has above-mentioned atomic ratio composition;

Excite the fluorescent powder with a wavelength of 450nm blue light, the results show that the fluorescent powder prepared by the present invention has a wide excitation spectrum range, strong absorption at 450nm, and can be combined with a blue light chip; the emission of the fluorescent powder prepared by the present invention The spectrum is broadened to the red light region, which can improve the color rendering of white light.

Example 23

Weigh 44.77 grams of Lu ₂ O ₃ , 12.75 grams of Al ₂ O ₃ , 18.74 grams of Ga _{2 O 3} , 1.50 grams of SiO ₂ , 1.30 grams of GeO ₂ , 1.88 grams of SnO ₂ , 5.75 grams of MnCO ₃ and 8.63 grams of CeO ₂ . Grinding and mixing, put the obtained mixture into an alumina crucible, cover the crucible lid, put it into a high-temperature furnace, and bake it at 1500°C and 10% H ₂ /N ₂ atmosphere for 5 hours, take it out when it is cooled to room temperature, and grind it After dispersion, the garnet-based solid solution phosphor for blue light excitation is obtained, and its composition is Lu _2.25 Ce _0.25 Mn _0.50 Al _2.50 Ga _2.00 Si _0.25 Ge _0.125 Sn _0.125 O ₁₂ .

Carry out XRD analysis to described fluorescent powder, the result shows that it has above-mentioned atomic ratio composition;

Excite the fluorescent powder with a wavelength of 450nm blue light, the results show that the fluorescent powder prepared by the present invention has a wide excitation spectrum range, strong absorption at 450nm, and can be combined with a blue light chip; the emission of the fluorescent powder prepared by the present invention The spectrum is broadened to the red light region, which can improve the color rendering of white light.

Example 24

Weigh 31.90 grams of Y ₂ O ₃ , 24.85 grams of Al ₂ O ₃ , 0.75 grams of SiO ₂ , 1.44 grams of MnCO ₃ , 0.86 grams of CeO ₂ , 0.06 grams of NaF and 0.10 grams of NH ₄ HF ₂ , carry out thorough grinding and mixing, and obtain Put the mixture into an alumina crucible, cover the crucible lid, put it into a high-temperature furnace, and roast it for 1 hour at 1600 ° C under a 10% H ₂ /N ₂ atmosphere, take it out when it is cooled to room temperature, grind and disperse it, and obtain The garnet-based solid solution phosphor excited by blue light has a composition of Y _2.825 Ce _0.05 Mn _0.125 Al _4.875 Si _0.125 O ₁₂ .

Carry out XRD analysis to described fluorescent powder, the result shows that it has above-mentioned atomic ratio composition;

Excite the fluorescent powder with a wavelength of 450nm blue light, the results show that the fluorescent powder prepared by the present invention has a wide excitation spectrum range, strong absorption at 450nm, and can be combined with a blue light chip; the emission of the fluorescent powder prepared by the present invention The spectrum is broadened to the red light region, which can improve the color rendering of white light.

Example 25

Weigh 31.90 g of Y ₂ O ₃ , 24.85 g of Al ₂ O ₃ , 0.75 g of SiO ₂ , 1.44 g of MnCO ₃ , 0.86 g of CeO ₂ and 0.16 g of CaF ₂ , grind and mix thoroughly, and put the resulting mixture into an alumina crucible Inside, cover the crucible lid, put it into a high-temperature furnace, and bake it for 4 hours at 1500°C in a 10% H ₂ /N ₂ atmosphere, take it out when it is cooled to room temperature, grind and disperse it, and obtain a phosphor powder for white LEDs excited by blue light , whose composition is Y _2.825 Ce _0.05 Mn _0.125 Al _4.875 Si _0.125 O ₁₂ .

Carry out XRD analysis to described fluorescent powder, the result shows that it has above-mentioned atomic ratio composition;

Excite the fluorescent powder with a wavelength of 450nm blue light, the results show that the fluorescent powder prepared by the present invention has a wide excitation spectrum range, strong absorption at 450nm, and can be combined with a blue light chip; the emission of the fluorescent powder prepared by the present invention The spectrum is broadened to the red light region, which can improve the color rendering of white light.

Example 26

Weigh 31.90 g of Y ₂ O ₃ , 24.85 g of Al ₂ O ₃ , 0.75 g of SiO ₂ , 1.85 g of SrCO ₃ , 0.86 g of CeO ₂ , 0.03 g of LiF and 0.13 g of SrF ₂ , grind and mix thoroughly, and place the obtained mixture Put it into an alumina crucible, cover the crucible lid, put it into a high-temperature furnace, and bake it for 3 hours at 1400°C in a 10% H ₂ /N ₂ atmosphere, take it out when it is cooled to room temperature, and get white light excited by blue light after grinding and dispersing Phosphor powder for LED, its composition is Y _2.825 Ce _0.05 Sr _0.125 Al _4.875 Si _0.125 O ₁₂ .

Carry out XRD analysis to described fluorescent powder, the result shows that it has above-mentioned atomic ratio composition;

Excite the fluorescent powder with a wavelength of 450nm blue light, the results show that the fluorescent powder prepared by the present invention has a wide excitation spectrum range, strong absorption at 450nm, and can be combined with a blue light chip; the emission of the fluorescent powder prepared by the present invention The spectrum is broadened to the red light region, which can improve the color rendering of white light.

Example 27

Weigh 55.71 grams of Lu ₂ O ₃ , 24.72 grams of Al ₂ O ₃ , 0.90 grams of SiO ₂ , 0.60 grams of MgO, 0.86 grams of CeO _{2 ,} 0.12 grams of LaF ₃ and 0.10 grams of NH ₄ HF ₂ , carry out thorough grinding and mixing, and obtain Put the mixture into an alumina crucible, cover the crucible lid, put it into a high-temperature furnace, and bake it for 3 hours at 1450°C in a 10% H ₂ /N ₂ atmosphere, take it out when it is cooled to room temperature, grind and disperse it, and obtain blue light excitation Phosphor powder for white LEDs, the composition of which is Lu _2.80 Ce _0.05 Mg _0.15 Al _4.85 Si _0.15 O ₁₂ .

Carry out XRD analysis to described fluorescent powder, the result shows that it has above-mentioned atomic ratio composition;

Excite the fluorescent powder with a wavelength of 450nm blue light, the results show that the fluorescent powder prepared by the present invention has a wide excitation spectrum range, strong absorption at 450nm, and can be combined with a blue light chip; the emission of the fluorescent powder prepared by the present invention The spectrum is broadened to the red light region, which can improve the color rendering of white light.

Example 28

Weigh 55.71 grams of Lu ₂ O ₃ , 24.72 grams of Al ₂ O ₃ , 0.90 grams of SiO ₂ , 0.57 grams of MnCO ₃ , 0.86 grams of CeO _{2 ,} 0.10 grams of NH ₄ F and 0.08 grams of BaF ₂ , carry out thorough grinding and mixing, and obtain Put the mixture into an alumina crucible, cover the crucible lid, put it into a high-temperature furnace, and bake it at 1400°C in a 10% H ₂ /N ₂ atmosphere for 6 hours, take it out when it is cooled to room temperature, grind and disperse it, and obtain blue light excitation Phosphor powder for white LEDs, the composition of which is Lu _2.80 Ce _0.05 Mn _0.15 Al _4.85 Si _0.15 O ₁₂ .

Carry out XRD analysis to described fluorescent powder, the result shows that it has above-mentioned atomic ratio composition;

Excite the fluorescent powder with a wavelength of 450nm blue light, the results show that the fluorescent powder prepared by the present invention has a wide excitation spectrum range, strong absorption at 450nm, and can be combined with a blue light chip; the emission of the fluorescent powder prepared by the present invention The spectrum is broadened to the red light region, which can improve the color rendering of white light.

Example 29

Weigh 55.71 grams of Lu ₂ O ₃ , 24.72 grams of Al ₂ O ₃ , 0.90 grams of SiO ₂ , 0.57 grams of MnCO ₃ , 0.86 grams of CeO _{2 ,} 0.14 grams of AlF ₃ and 0.06 grams of GdF ₃ , and thoroughly grind and mix the resulting mixture Put it into an alumina crucible, cover the crucible lid, put it into a high-temperature furnace, and bake it for 6 hours at 1450 ° C under a 10% H ₂ /N ₂ atmosphere, take it out when it is cooled to room temperature, grind and disperse it, and obtain blue light-excited Phosphor powder for white LED, its composition is Lu _2.80 Ce _0.05 Mn _0.15 Al _4.85 Si _0.15 O ₁₂ .

Carry out XRD analysis to described fluorescent powder, the result shows that it has above-mentioned atomic ratio composition;

Excite the fluorescent powder with a wavelength of 450nm blue light, the results show that the fluorescent powder prepared by the present invention has a wide excitation spectrum range, strong absorption at 450nm, and can be combined with a blue light chip; the emission of the fluorescent powder prepared by the present invention The spectrum is broadened to the red light region, which can improve the color rendering of white light.

Example 30

Weigh 55.71 grams of Lu ₂ O ₃ , 24.72 grams of Al ₂ O ₃ , 0.90 grams of SiO ₂ , 0.57 grams of MnCO ₃ , 0.86 grams of CeO ₂ , 0.10 grams of LuF ₃ and 0.10 grams of NH ₄ HF ₂ , and carry out thorough grinding and mixing to obtain Put the mixture into an alumina crucible, cover the crucible lid, put it into a high-temperature furnace, and bake it for 1 hour at 1500 ° C in a 10% H ₂ /N ₂ atmosphere, take it out when it is cooled to room temperature, grind and disperse it, and get a blue light The phosphor powder for the excited white light LED is composed of Lu _2.80 Ce _0.05 Mn _0.15 Al _4.85 Si _0.15 O ₁₂ .

Carry out XRD analysis to described fluorescent powder, the result shows that it has above-mentioned atomic ratio composition;

Excite the fluorescent powder with a wavelength of 450nm blue light, the results show that the fluorescent powder prepared by the present invention has a wide excitation spectrum range, strong absorption at 450nm, and can be combined with a blue light chip; the emission of the fluorescent powder prepared by the present invention The spectrum is broadened to the red light region, which can improve the color rendering of white light.

Comparative example 1

Weigh 33.31 grams of Y ₂ O ₃ , 25.49 grams of Al ₂ O ₃ and 0.86 grams of CeO ₂ , carry out thorough grinding and mixing, put the obtained mixture in an alumina crucible, cover the crucible lid, and put it in a high-temperature furnace. under 10% H ₂ /N ₂ atmosphere for 3 hours, take it out when cooled to room temperature, and grind and disperse to obtain blue-light-excited phosphor powder for white light LED, the composition of which is Y _2.95 Ce _0.05 Al ₅ O ₁₂ .

Carry out XRD analysis to described fluorescent powder, the result shows that it has the above atomic ratio composition

Excite the fluorescent powder with a wavelength of 450nm blue light, the results are shown in Figure 5, Figure 5 is the photoemission spectrum of the fluorescent powder prepared in Comparative Example 1 of the present invention under the excitation of 450nm blue light, as can be seen from Figure 5, the preparation of Comparative Example 1 The emission spectrum of the fluorescent powder is wider in the yellow-green light region, and the red light region is insufficient, and the color rendering of the obtained white light is poor.

Comparative example 2

Weigh 58.69 grams of Lu ₂ O ₃ , 25.49 grams of Al ₂ O ₃ and 0.86 grams of CeO ₂ , carry out thorough grinding and mixing, put the resulting mixture in an alumina crucible, cover the crucible lid, and put it in a high-temperature furnace. ℃, under 10% H ₂ /N ₂ atmosphere for 8 hours, take it out when cooled to room temperature, and grind and disperse to obtain blue light-excited phosphor powder for white light LED, whose composition is Lu _2.95 Ce _0.05 Al ₅ O ₁₂ .

Carry out XRD analysis to described fluorescent powder, the result shows that it has above-mentioned atomic ratio composition;

Excite the phosphor powder with a wavelength of 450nm blue light, the results are shown in Figure 6, Figure 6 is the photoemission spectrum of the phosphor powder prepared in Comparative Example 2 of the present invention under the excitation of 450nm blue light, as can be seen from Figure 6, Comparative Example 2 prepared The emission spectrum of the fluorescent powder is wider in the green light area, and the red light area is insufficient, and the color rendering of the white light obtained is poor.

The above is only a preferred embodiment of the present invention, it should be pointed out that, for those of ordinary skill in the art, without departing from the principle of the present invention, some improvements and modifications can also be made, and these improvements and modifications can also be made. It should be regarded as the protection scope of the present invention.

Claims (10)

1. one kind is used for blue-light excited sosoloid fluorescence luminescent material, has atomic ratio shown in the formula (I):

(1-x)[RE _3-yCe _yM ₅O ₁₂]·x[A _3-zMn _zM ₂(DO ₄) ₃](I)；

In the formula (I), RE is one or more among Y, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm, Yb and the Lu;

M is one or more among B, Al, Ga and the In;

A is one or more of Mg, Ca, Sr and Ba;

D is one or more of Si, Ge and Sn;

0＜x≤0.50；

0＜y≤0.30；

0＜z≤3。

2. sosoloid fluorescence luminescent material according to claim 1 is characterized in that, said M is one or both among B and the Al.

3. claim 1 or the 2 described preparing methods that are used for blue-light excited sosoloid fluorescence luminescent material may further comprise the steps:

To contain the RE compound, contain the Ce compound, contain the M compound, contain the Mn compound, contain the A compound and contain the D compound, obtain mixture;

With the roasting under reducing atmosphere of said mixture, obtain being used for blue-light excited sosoloid fluorescence luminescent material.

4. preparation method according to claim 3 is characterized in that, the said RE of containing compound is one or more in oxide compound, oxyhydroxide, nitrate salt, halogenide and the carbonate that contains RE.

5. preparation method according to claim 3 is characterized in that, the said Ce of containing compound is one or more in oxide compound, oxyhydroxide, nitrate salt, halogenide and the carbonate that contains Ce.

6. preparation method according to claim 3 is characterized in that, the said M of containing compound is one or more in oxide compound, oxyhydroxide and the oxygen acid that contains M.

7. preparation method according to claim 3; It is characterized in that; The said A of containing compound is one or more in oxide compound, oxyhydroxide, nitrate salt, halogenide and the carbonate that contains A, and the said Mn of containing compound is one or more in oxide compound, oxyhydroxide, nitrate salt, halogenide and the carbonate that contains Mn.

8. preparation method according to claim 3 is characterized in that, the said D of containing compound is one or more in oxide compound, oxyhydroxide and the oxygen acid that contains D.

9. according to any described preparation method of claim 3～8, it is characterized in that said mixture also comprises fluoride flux.

10. preparation method according to claim 9 is characterized in that, the temperature of said roasting is 1400 ℃～1700 ℃, and the time of said roasting is 1h～20h.

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