CN116103039A - Novel Li and Mn codoped aluminate matrix red fluorescent powder and preparation method thereof - Google Patents
Novel Li and Mn codoped aluminate matrix red fluorescent powder and preparation method thereof Download PDFInfo
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/64—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing aluminium
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- Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps
Abstract
The invention discloses a novel Li and Mn co-doped aluminate matrix red fluorescent powder and a preparation method thereof, wherein the fluorescent powder comprises the following chemical components: sr (Sr) 4 Al 14‑a‑b O 25 ：aMn 4+ ，bLi + ，cH 3 BO 3 Wherein Mn is 4+ From MnCO 3 、MnO 2 One or two of them are combined, li + From LiF, li 2 CO 3 One or two of them are combined, H 3 BO 3 As a cosolvent, 0<a<0.05，0<b≤1.5，0<c.ltoreq.15% by weight (percentage relative to the total mass). Novel Mn obtained by the invention 4+ The aluminate matrix doped red fluorescent powder has the characteristics of capability of being effectively excited by blue light to emit red light, high quantum efficiency, good luminous performance and the like, and can obtain warm white light with good comprehensive luminous performance after the prepared red powder, commercial yellow powder and commercial blue light chip are used for device assembly, and the prepared aluminate red fluorescent powder can be widely applied to the fields of indoor and outdoor illumination, automobile headlights and the likeDomain.
Description
Technical Field
The invention relates to the technical field of inorganic luminescent materials, in particular to novel Li and Mn codoped aluminate matrix red fluorescent powder and a preparation method thereof.
Background
White light LEDs are known as fourth-generation environment-friendly illumination electric light sources, namely 21 st green light sources, and are widely applied to various fields such as indoor and outdoor illumination, landscape illumination, automobile headlamps and the like as a new-generation illumination light source.
The research and development of the material for the high-quality lighting device have important significance for promoting the economic development of areas and the innovation of industry, at present, the high-power white light LED device used as the main stream of market lighting has higher color temperature (CCT, CCT > 5000K) due to the lack of red light, lower color rendering index (CRI, ra < 70), and an assembly device mode of red fluorescent powder, yellow fluorescent powder and blue light chip is an effective way for solving the problems, and the red fluorescent powder for the white light LED with good luminous performance, particularly the oxide red fluorescent powder with good thermal stability, has important significance and market application value.
The common red luminescent material is composed of inorganic compound as matrix material and luminescent center, and the commercial blue-excited red fluorescent powder is mainly concentrated on Eu 2+ Or Mn of 4+ In a nitride or fluoride matrix (CaAlSiN) which is the luminescent center 3 ：Eu 2+ ，Ca 2 S 5 N 8 ：Eu 2+ ，KSiF 4 ：Mn 4+ Etc.), however, nitride phosphors are more strongly absorbing between 500-600nm, which is comparable to YAG for commercial white LEDs: ce (Ce) 3+ The emission spectrum of the yellow powder is partially overlapped, so that the light efficiency is reduced to a certain extent, and the energy is lost; fluoride compoundsThe fluorescent powder has poor chemical stability, can be applied only through complex wrapping and other processes, increases the use cost, and cannot guarantee the service life even if the fluorescent powder is used after being wrapped. The oxide has high thermal stability and chemical stability compared with the nitride and fluoride, and can be directly applied. Mn (Mn) 4+ Has a unique character as a transition metal element 3 D 3 Of the structure of Mn 4+ The main excitation peak of the oxide matrix fluorescent powder serving as the activator is in the near ultraviolet and blue light areas, so that light re-absorption is effectively avoided, and the oxide matrix fluorescent powder is a promising powder. In recent years, researchers have surrounded Mn 4+ The activated red phosphor has been studied in a great deal and known techniques related to the present invention are: A. lei Chen et al (Lei Chen, shaochan Xue, xiuling Chen, et al materials Research bulletin.2014; 60:604-11) report a red phosphor Sr for a white light LED 4 Al 14 O 25 ：Mn 4+ The optimal preparation temperature of 1300 ℃ is ascertained, but the blue light excitation effect is poor and the thermal stability is poor; B. mingying Peng et al (Mingying Peng, xuewen Yin, tanner, peter A, et al chemistry of materials.2015; 27:2938-2945) reported Sr 4 Al 14 O 25 ：Mn 4+ Mg is added in the synthesis reaction 2+ Can strengthen Mn 4+ Is enhanced due to Mn 4+ Ion(s) 2 E g The energy level decreases, resulting in a reduction of non-radiative transitions; C. jiaqi Long et al (Jiaqi Long, xuanyi Yuan, chaoyang Ma, et al RSC Advances.2018,8, 1469-1476) doped with Na + Ions (substituting for Sr position) to make Sr 4 Al 14 O 25 ：Mn 4+ The red fluorescent powder has enhanced luminescence, the reason is the same as B, the internal quantum yield reaches 60.8%, and the researches report series Mn 4+ Sr doped 4 Al 14 O 25 The matrix fluorescent powder also compensates Mn by substituting the non-equivalent ions of Sr position and Al position 4+ Substituted for Al 3+ The resulting charge imbalance improves luminescence, which is positively effective, however, the luminescence of the phosphor as a whole remains relatively weak, blueInsufficient absorption and excitation, and low quantum efficiency.
The invention designs the composition scheme based on the above work and study, adopts LiF and Li 2 CO 3 In the preparation method, li is substituted for Al to perform charge compensation (or enter lattice gap compensation), cosolvent is added to assist, crystal crystallinity is enhanced, and the oxide matrix red fluorescent powder with blue light effective excitation, high quantum efficiency and good luminous effect is prepared through experiments.
Disclosure of Invention
The invention aims to provide novel Li and Mn codoped aluminate matrix red fluorescent powder and a preparation method thereof, so as to solve the problems in the prior art.
In order to achieve the above purpose, the present invention provides the following technical solutions: a novel Li and Mn co-doped aluminate matrix red fluorescent powder comprises the following chemical components: sr (Sr) 4 Al 14-a-b O 25 ：aMn 4+ ，bLi + ，cH 3 BO 3 Wherein Mn is 4+ From MnCO 3 、MnO 2 One or two of them are combined, li + From LiF, li 2 CO 3 One or two of them are combined, H 3 BO 3 Is a cosolvent.
Preferably, the 0< a <0.05,0< b.ltoreq.1.5, 0< c.ltoreq.15 wt.% (percentage relative to the total mass).
A preparation method of novel Li and Mn co-doped aluminate matrix red fluorescent powder comprises the following steps:
A. according to formula Sr 4 Al 14-a-b O 25 ：aMn 4+ ，bLi + ，cH 3 BO 3 Weighing Sr, al, mn, li and other element raw materials according to stoichiometric ratio, fully mixing, grinding uniformly, and sieving;
B. placing the mixture obtained in the step A into a corundum crucible or a graphite crucible, placing the corundum crucible or the graphite crucible into a muffle furnace, sintering at 700-1000 ℃ and preserving heat for 1-5 hours (presintering), then heating to 1200-1400 ℃ and preserving heat for 2-8 hours, wherein the heating rate is 5-20 ℃/min, and cooling to room temperature along with the furnace;
C. and C, crushing the sintered product obtained in the step B, fully grinding, washing with clear water or one or more of absolute ethyl alcohol, acetone, acetic acid and other organic solvents for 2-5 times, filtering, and drying to obtain the novel Li and Mn co-doped aluminate red fluorescent powder.
Preferably, the raw material containing Sr and Al is SrCO 3 And Al 2 O 3 。
Preferably, the heating rate of the electric furnace is 5-20 ℃/min, the heating mode is muffle furnace heating or electromagnetic induction furnace heating, and meanwhile, the heating atmosphere is air atmosphere.
Compared with the prior art, the invention has the following beneficial effects:
novel Mn obtained by the invention 4+ The aluminate matrix doped red fluorescent powder has the characteristics of capability of being effectively excited by blue light to emit red light, high quantum efficiency, good luminous performance and the like, and can obtain warm white light with good comprehensive luminous performance after the prepared red powder, commercial yellow powder and commercial blue light chip are used for device assembly, and the prepared aluminate red fluorescent powder can be widely applied to the fields of indoor and outdoor illumination, automobile headlights and the like.
Drawings
FIG. 1 is an excitation pattern of a phosphor sample prepared according to an embodiment of the present invention;
FIG. 2 is a graph of the emission spectrum of the present invention;
FIG. 3 is a commercial yellow powder (YAG: ce) of the present invention 3+ ) And mixing and packaging the spectrograms after the blue light chip.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
According to chemical formula Sr 4 Al 14-a-b O 25 ：aMn 4+ ，bLi + ，cH 3 BO 3 Preparing Li and Mn co-doped aluminate red fluorescent powder, wherein Mn 4+ Is MnO as raw material 2 ，Li + Wherein a=0.05, b=1.5, c=15 wt.% in the chemical formula, the preparation process is as follows:
A. weighing analytically pure SrCO according to stoichiometric ratio 3 ：2.953g，Al 2 O 3 ：3.174g，MnO 2 ：0.022g，LiF：0.196g，H 3 BO 3 :0.951g, fully mixing the above raw materials, grinding uniformly, and sieving with a 200 mesh sieve for later use;
B. placing the mixture into a corundum crucible, placing the corundum crucible into a box-type furnace, heating to 700 ℃ at a heating rate of 10 ℃/min, preserving heat for 1h, heating to 1200 ℃ at a heating rate of 5 ℃/min, preserving heat for 8h, and cooling to room temperature along with the furnace;
C. and C, fully grinding the sintering product obtained in the step B, washing the sintering product with deionized water for 2 times, drying and sieving the sintering product to obtain the Li and Mn co-doped aluminate red fluorescent powder.
The red fluorescent powder obtained in the example is subjected to photoluminescence spectrum measurement by using 450nm blue light, and the result shows that the emission peak of the obtained fluorescent powder is between 600 and 700nm, the half-peak width is 20nm, the internal quantum efficiency is 85 percent, and the obtained fluorescent powder is compared with commercial YAG: ce (Ce) 3+ After the yellow powder is compounded and a 450nm blue light chip is packaged, the photoelectric index is 4085K of color temperature and 89 of color rendering index and the lumen efficiency is 137.12lm/W when 60mA current is supplied.
Example 2
According to chemical formula Sr 4 Al 14-a-b O 25 ：aMn 4+ ，bLi + ，cH 3 BO 3 Preparing Li and Mn co-doped aluminate red fluorescent powder, wherein Mn 4+ The raw material of (2) is MnCO 3 ，Li + Is Li as raw material 2 CO 3 In the formula, a=0.01, b=1, c=10 wt.%, the preparation process is as follows:
A. weighing analytically pure SrCO according to stoichiometric ratio 3 ：2.362g，Al 2 O 3 ：2.751g，MnCO 3 ：0.046g，Li 2 CO 3 ：0.148g，H 3 BO 3 :0.527g, fully mixing the above raw materials, grinding uniformly, and sieving with a 200 mesh sieve for later use;
B. placing the mixture into a corundum crucible, placing the corundum crucible into a box-type furnace, heating to 1000 ℃ at a heating rate of 5 ℃/min, preserving heat for 5 hours, heating to 1400 ℃ at a heating rate of 20 ℃/min, preserving heat for 2 hours, and cooling to room temperature along with the furnace;
C. and C, fully grinding the sintering product obtained in the step B, washing with absolute ethyl alcohol for 5 times, drying and sieving to obtain the Li and Mn co-doped aluminate red fluorescent powder.
The red fluorescent powder obtained in the example is subjected to photoluminescence spectrum measurement by using 450nm blue light, and the result shows that the emission peak of the obtained fluorescent powder is between 600 and 700nm, the half-peak width is 18nm, the internal quantum efficiency is 79 percent, and the obtained fluorescent powder is compared with commercial YAG: ce (Ce) 3+ After the yellow powder is compounded and a 450nm blue light chip is packaged, the photoelectric index is the color temperature 4376K, the color rendering index is 82 and the lumen efficiency is 156.15lm/W when 60mA current is supplied.
Example 3
According to chemical formula Sr 4 Al 14-a-b O 25 ：aMn 4+ ，bLi + ，cH 3 BO 3 Preparing Li and Mn co-doped aluminate red fluorescent powder, wherein Mn 4+ Is MnO as raw material 2 ，Li + Is Li as raw material 2 CO 3 A mixture of LiF, of the formula a=0.005, b=0.5, c=8 wt.%, prepared as follows:
A. weighing analytically pure SrCO according to stoichiometric ratio 3 ：3.543g，Al 2 O 3 ：4.158g，MnO 2 ：0.026g，LiF：0.047g，Li 2 CO 3 ：0.044g，H 3 BO 3 :0.624g, fully mixing the above raw materials, grinding uniformly, and sieving with a 200 mesh sieve for later use;
B. placing the mixture into a corundum crucible, placing the corundum crucible into a box-type furnace, heating to 900 ℃ at a heating rate of 8 ℃/min, preserving heat for 3 hours, heating to 1350 ℃ at a heating rate of 5 ℃/min, preserving heat for 5 hours, and cooling to room temperature along with the furnace;
C. and C, fully grinding the sintering product obtained in the step B, washing with acetone for 3 times, drying and sieving to obtain the Li and Mn co-doped aluminate red fluorescent powder.
The red fluorescent powder obtained in the example is subjected to photoluminescence spectrum measurement by using 450nm blue light, and the result shows that the emission peak of the obtained fluorescent powder is between 600 and 700nm, the half-peak width is 22nm, the internal quantum efficiency is 76 percent, and the obtained fluorescent powder is compared with commercial YAG: ce (Ce) 3+ After the yellow powder is compounded and a 450nm blue light chip is packaged, the photoelectric index is the color temperature 3528K, the color rendering index is 90 and the lumen efficiency is 122.78lm/W when 60mA current is supplied.
Example 4
According to chemical formula Sr 4 Al 14-a-b O 25 ：aMn 4+ ，bLi + ，cH 3 BO 3 Preparing Li and Mn co-doped aluminate red fluorescent powder, wherein Mn + The raw material of (2) is MnCO 3 、MnO 2 Is a mixture of (1), li + Wherein a=0.02, b=0.8, c=5 wt.% in the chemical formula, the preparation process is as follows:
A. weighing analytically pure SrCO according to stoichiometric ratio 3 ：3.248g，Al 2 O 3 ：3.696g，MnO 2 ：0.005g，MnCO 3 ：0.006g，LiF：0.114g，H 3 BO 3 :0.353g, fully mixing the above raw materials, grinding uniformly, and sieving with a 200 mesh sieve for later use;
B. placing the mixture into a corundum crucible, placing the corundum crucible into a box-type furnace, heating to 900 ℃ at a heating rate of 10 ℃/min, preserving heat for 2 hours, heating to 1300 ℃ at a heating rate of 10 ℃/min, preserving heat for 6 hours, and cooling to room temperature along with the furnace;
C. and C, fully grinding the sintering product obtained in the step B, washing with acetic acid for 3 times, drying and sieving to obtain the Li and Mn co-doped aluminate red fluorescent powder.
The red fluorescent powder obtained in the example is subjected to photoluminescence spectrum measurement by using 450nm blue light, and the result shows that the emission peak of the obtained fluorescent powder is between 600 and 700nm, the half-peak width is 18nm, the internal quantum efficiency is 88 percent, and the obtained fluorescent powder is compared with commercial YAG: ce (Ce) 3+ Yellow powder composite and packaged 450nm blue light chipAfter that, when 60mA current is supplied, the photoelectric index is color temperature 4876K, the color rendering index is 84, and the lumen efficiency is 140.15lm/W.
Meanwhile, the prepared red powder, commercial yellow powder and commercial blue light chip are used for device assembly, so that warm white light with good comprehensive luminous performance can be obtained.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. A novel Li and Mn codoped aluminate matrix red fluorescent powder is characterized in that: the chemical composition of the fluorescent powder is as follows: sr (Sr) 4 Al 14-a-b O 25 ：aMn 4+ ，bLi + ，cH 3 BO 3 Wherein Mn is 4+ From MnCO 3 、MnO 2 One or two of them are combined, li + From LiF, li 2 CO 3 One or two of them are combined, H 3 BO 3 Is a cosolvent.
2. The novel Li and Mn codoped aluminate matrix red fluorescent powder according to claim 1, which is characterized in that: the 0< a <0.05,0< b.ltoreq.1.5, 0< c.ltoreq.15 wt.% (percentage relative to the total mass).
3. A preparation method of novel Li and Mn co-doped aluminate matrix red fluorescent powder is characterized by comprising the following steps: the preparation method comprises the following steps:
A. according to formula Sr 4 Al 14-a-b O 25 ：aMn 4+ ，bLi + ，cH 3 BO 3 Weighing Sr, al, mn, li and other element materials according to stoichiometric ratio, mixing thoroughly, grindingUniform sieving;
B. placing the mixture obtained in the step A into a corundum crucible or a graphite crucible, placing the corundum crucible or the graphite crucible into a muffle furnace, sintering at 700-1000 ℃ and preserving heat for 1-5 hours (presintering), then heating to 1200-1400 ℃ and preserving heat for 2-8 hours, wherein the heating rate is 5-20 ℃/min, and cooling to room temperature along with the furnace;
C. and C, crushing the sintered product obtained in the step B, fully grinding, washing with clear water or one or more of absolute ethyl alcohol, acetone, acetic acid and other organic solvents for 2-5 times, filtering, and drying to obtain the novel Li and Mn co-doped aluminate red fluorescent powder.
4. The method for preparing the novel Li and Mn codoped aluminate matrix red fluorescent powder according to claim 3, which is characterized in that: the raw material containing Sr and Al is SrCO 3 And Al 2 O 3 。
5. The method for preparing the novel Li and Mn codoped aluminate matrix red fluorescent powder according to claim 3, which is characterized in that: the heating rate of the electric furnace is 5-20 ℃/min, the heating mode is muffle furnace heating or electromagnetic induction furnace heating, and meanwhile, the heating atmosphere is air atmosphere.
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