CN115124995B - Method for improving performance of luminescent material - Google Patents

Method for improving performance of luminescent material Download PDF

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CN115124995B
CN115124995B CN202210798578.0A CN202210798578A CN115124995B CN 115124995 B CN115124995 B CN 115124995B CN 202210798578 A CN202210798578 A CN 202210798578A CN 115124995 B CN115124995 B CN 115124995B
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luminescent
luminescent material
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sintering
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CN115124995A (en
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王赵锋
白永庆
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Lanzhou Institute of Chemical Physics LICP of CAS
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    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7743—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing terbium
    • C09K11/7744—Chalcogenides
    • C09K11/7746—Chalcogenides with alkaline earth metals
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/58—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing copper, silver or gold
    • C09K11/582—Chalcogenides
    • C09K11/584—Chalcogenides with zinc or cadmium
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  • Luminescent Compositions (AREA)

Abstract

The invention provides a method for improving the performance of a luminescent material, and belongs to the technical field of luminescent materials. The invention provides quick cooling conditions through quenching of the liquid cooling medium, causes the crystal structure of the powder luminescent material to be adjusted, can realize the re-optimization of the luminescent performance (color/intensity) of the prepared luminescent powder, can realize the regulation and control of the mechanical and photoluminescence intensity of the material, can realize the regulation and control of the photoinduced and mechanical luminescent colors, is suitable for various powder luminescent materials, and provides a new method and thinking for the performance optimization of the powder luminescent material. The method has strong universality and can be suitable for various powder luminescent materials; the operation is simple, and the cost is low; the method can be used for mass replication and realizing large-scale production; green and environment-friendly, and has no environmental pollution.

Description

Method for improving performance of luminescent material
Technical Field
The invention relates to the technical field of luminescent materials, in particular to a method for improving the performance of a luminescent material.
Background
Light is the main carrier of the human cognition and perception world, from natural light to artificial light, and human realizes reliable and effective connection with the natural world through luminescent materials. The luminescent material mainly comprises two major classes of inorganic luminescent materials and organic luminescent materials, wherein the inorganic luminescent materials have made great breakthrough in the fields of flat panel display, laser, fluorescent biological markers, optical communication, nano optoelectronic devices and the like because of the advantages of high photochemical stability, long fluorescence lifetime, tunable excitation/emission wavelength and the like.
The development/development of high performance phosphors has become one of the main research focus in this area. At present, the development of high-performance phosphors mainly involves two ideas: firstly, new materials are developed, and excellent luminescence performance is obtained by preparing new luminescent materials. Secondly, the existing luminescent material properties are optimized, such as ion co-doping, host matrix atom replacement, doping ion concentration adjustment and preparation temperature and composition regulation (Xu et al Persistent luminescence instead of phosphorescence: histor y, mechanism, and perspective, journal of Luminescence (2019) 581-620 and J.C.zhang, et al, trap-controlled mechanoluminescent materials, progres s in Materials Science 103 (2019) 678-742). However, the above performance optimization schemes are all optimization schemes in the preparation process, and the re-optimization of the luminescence performance of the prepared powder luminescent material cannot be realized.
Disclosure of Invention
The invention aims to provide a method for improving the performance of a luminescent material, which can realize the re-optimization of the luminescent performance of prepared luminescent powder and is suitable for various powder luminescent materials.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for improving the performance of a luminescent material, which comprises the following steps:
and heating the original sample of the luminescent material in a protective atmosphere, and quenching in a liquid cooling medium until the liquid cooling medium volatilizes.
Preferably, the luminescent material raw sample comprises Sr 3-x Al 2 O 5 Cl 2 :xTb 3+ 、ZnS:yCu + 、ZnS:xMn 2+ 、Li/Na 1-x NbO 3 :xPr 3+ 、Y 3-y Al 5 O 12 :yCe 3+ Or Lu 3-y Al 5 O 12 :yCe 3+ ；x＝0.001～0.06，y＝0.001～0.02。
Preferably, before the heat treatment, the luminescent material original sample is screened, and the pore diameter of a mesh screen used for screening is 1-50 μm.
Preferably, the protective atmosphere is the same as the protective atmosphere of the original sample of luminescent material.
Preferably, the target temperature of heating is less than or equal to the final sintering temperature of the original sample of luminescent material.
Preferably, the liquid cooling medium comprises liquid nitrogen or liquid helium.
Preferably, the Sr 3-x Al 2 O 5 Cl 2 :xTb 3+ The preparation method of the (C) comprises the following steps:
according to Sr 3-x Al 2 O 5 Cl 2 :xTb 3+ Chemical composition of SrCO 3 、Sr 2 Cl 2 ·6H 2 O、Al 2 O 3 And Tb 4 O 7 Mixing, pre-sintering, press forming and sintering the obtained mixed powder in sequence to obtain Sr 3-x Al 2 O 5 Cl 2 :xTb 3+ 。
Preferably, the presintering temperature is 600-1200 ℃, and the heat preservation time is 1-5 h; the sintering temperature is 1200-1400 ℃, and the heat preservation time is 2-8 h.
Preferably, the ZnS: yCu + The preparation method of the (C) comprises the following steps:
according to ZnS: yCu + Chemical composition of ZnS and CuCl 2 Mixing, sintering the obtained mixed powder in the protection of nitrogen atmosphere to obtain ZnS yCu + And (5) luminescent powder.
Preferably, the sintering temperature is 900-1200 ℃, and the heat preservation time is 1-5 h.
The invention provides a method for improving the performance of luminescent materials, which provides rapid cooling conditions through quenching of a liquid cooling medium to cause the change of the crystal structure of the luminescent materials, thereby changing the crystal field and the energy transfer efficiency, realizing the re-optimization of the luminescent performance (color/intensity) of the prepared luminescent powder, realizing the regulation and control of the mechanical and photoluminescence intensity of the materials, and also realizing the regulation and control of the photoinduced and mechanical luminescent colors, being applicable to various powder luminescent materials and providing a new method and thinking for the performance optimization of the powder luminescent materials.
The method has strong universality and can be suitable for various powder luminescent materials; the operation is simple, and the cost is low; the method can be used for mass replication and realizing large-scale production; green and environment-friendly, and has no environmental pollution.
Drawings
FIG. 1 shows Sr being quenched at different temperatures in example 1 of the present invention 2.99 Al 2 O 5 Cl 2 :Tb 0.01 XRD spectrum of powder luminescent material;
FIG. 2 shows Sr quenching at different temperatures according to example 1 of the present invention 2.99 Al 2 O 5 Cl 2 :Tb 0.01 Mechanical luminescence spectrogram of powder luminescent material;
FIG. 3 shows Sr being quenched at different temperatures according to example 1 of the present invention 2.99 Al 2 O 5 Cl 2 :Tb 0.01 Photoluminescence spectrogram of powder luminescent material;
FIG. 4 is a sample of ZnS: cu quenched at different temperatures in example 2 of the present invention 0.01 XRD spectrum of powder luminescent material;
FIG. 5 is a sample of ZnS: cu quenched at different temperatures in example 2 of the present invention 0.01 Photoinduced luminescence of powder luminescent materialA spectrogram;
FIG. 6 is a sample of ZnS: cu quenched at different temperatures in example 2 of the present invention 0.01 Mechanical luminous spectrum of powder luminous material.
Detailed Description
The invention provides a method for improving the performance of a luminescent material, which comprises the following steps:
and heating the original sample of the luminescent material in a protective atmosphere, and quenching in a liquid cooling medium until the liquid cooling medium volatilizes.
In the present invention, the preparation materials are commercially available as known to those skilled in the art unless otherwise specified.
In the present invention, the luminescent material raw sample preferably comprises Sr 3-x Al 2 O 5 Cl 2 :xTb 3+ 、ZnS:yCu + 、ZnS:xMn 2+ 、Li/Na 1-x NbO 3 :xPr 3+ 、Y 3-y Al 5 O 12 :yCe 3+ Or Lu 3-y Al 5 O 12 :yCe 3+ . The method for preparing the original sample of the luminescent material is not particularly limited, and the original sample of the luminescent material can be prepared according to a method known in the art.
In the present invention, the Sr 3-x Al 2 O 5 Cl 2 :xTb 3+ In x=0.001 to 0.06, more preferably 0.005 to 0.06, still more preferably 0.01 to 0.02; yCu of ZnS + In this formula, y=0.001 to 0.02, more preferably 0.005 to 0.06, and still more preferably 0.01 to 0.03. In an embodiment of the invention, sr is specifically 2.98 Al 2 O 5 Cl 2 :Tb 0.02 Luminescent powder, sr 2.99 Al 2 O 5 Cl 2 :Tb 0.01 Luminescent powder, znS and Cu 0.01 Luminescent powder or ZnS: cu 0.005 And (5) luminescent powder. In the present invention, sr 3-x Al 2 O 5 Cl 2 :xTb 3+ The strength of the photoinduced and mechanical luminescence of the luminescent powder is obviously improved along with the increase of the quenching temperature, znS: yCu + The photoinduced and mechanical luminescence of the luminescent powder generates red shift along with the increase of quenching temperature.
In the present invention, the Sr 3-x Al 2 O 5 Cl 2 :xTb 3+ The preparation method of (2) preferably comprises the following steps:
according to Sr 3-x Al 2 O 5 Cl 2 :xTb 3+ Chemical composition of SrCO 3 、Sr 2 Cl 2 ·6H 2 O、Al 2 O 3 And Tb 4 O 7 Mixing, pre-sintering, press forming and sintering the obtained mixed powder in sequence to obtain Sr 3-x Al 2 O 5 Cl 2 :xTb 3+ 。
In the present invention, the SrCO 3 、Sr 2 Cl 2 ·6H 2 O and Al 2 O 3 All preferably AR grade; the Tb is 4 O 7 The purity of (2) is preferably 99.99% or more.
The invention relates to the SrCO 3 、Sr 2 Cl 2 ·6H 2 O、Al 2 O 3 And Tb 4 O 7 The mode of mixing is not particularly limited, and any mode known in the art that can be uniformly mixed may be used. In the embodiment of the invention, the raw materials are placed in an agate mortar, fully ground and mixed after adding alcohol, and dried to obtain mixed powder.
The present invention preferably transfers the obtained mixed powder to an alumina crucible for calcination. In the present invention, the burn-in is preferably performed in an air atmosphere; the temperature of the presintering is preferably 600-1200 ℃, more preferably 700-1100 ℃, and even more preferably 800-900 ℃; the holding time for the preliminary firing is preferably 1 to 5 hours, more preferably 3 to 4 hours. The invention removes the crystal water in the raw materials by presintering, so that SrCO 3 And Sr 2 Cl 2 ·6H 2 O breaks down in advance to form a precursor. In the present invention, the burn-in is preferably performed in a box-type resistance furnace.
In the present invention, the sample obtained after the calcination is preferably ground to obtain a calcined powder. The grinding process is not particularly limited, and may be performed according to a process well known in the art.
The invention preferably presses the presintered powder; the pressure of the press molding is preferably 20 to 50MPa, more preferably 30 to 40MPa. The invention presses the presintered powder to be beneficial to improving the reaction efficiency of subsequent sintering, and can improve the crystallinity and the luminous performance. The invention has no special requirements on the size of the compression molding. In the examples of the invention, a round blank of diameter 20mm and thickness 2mm is pressed in particular.
In the present invention, the sintering is preferably performed in air; the sintering temperature is preferably 1200-1400 ℃, more preferably 1250-1350 ℃; the holding time is preferably 2 to 8 hours, more preferably 4 to 6 hours. In the sintering process, the precursor further reacts to generate a target product Sr 3-x Al 2 O 5 Cl 2 :xTb 3+ 。
After the sintering is completed, the invention is cooled to room temperature along with a furnace, and a sample is taken out and ground into powder to obtain Sr 3- x Al 2 O 5 Cl 2 :xTb 3+ And (5) luminescent powder. The process of grinding into powder is not particularly limited, and may be performed according to a process well known in the art.
In the present invention, the ZnS: yCu + The preparation method of (2) preferably comprises the following steps:
according to ZnS: yCu + Chemical composition of ZnS and CuCl 2 Mixing, sintering the obtained mixed powder in the protection of nitrogen atmosphere to obtain ZnS yCu + And (5) luminescent powder.
In the present invention, the ZnS and CuCl 2 The purity of (2) is preferably 99.99% or more. The invention is applicable to ZnS and CuCl 2 The mode of mixing is not particularly limited, and any mode known in the art that can be uniformly mixed may be used. In the embodiment of the invention, the raw materials are placed in an agate mortar, fully ground and mixed after adding alcohol, and dried to obtain mixed powder.
The present invention preferably transfers the obtained mixed powder to an alumina crucible for sintering. In the present invention, the sintering is preferably performed in a nitrogen atmosphere; the saidThe sintering temperature is preferably 900-1200 ℃, more preferably 1100-1150 ℃; the holding time for the sintering is preferably 1 to 5 hours, more preferably 3 to 4 hours. In the present invention, the sample obtained after sintering is preferably ground to obtain ZnS: yCu + And (5) luminescent powder.
In the present invention, the raw sample of the luminescent material is preferably subjected to screening, and the mesh screen used for the screening has a pore diameter of preferably 1 to 50. Mu.m, more preferably 2 to 30. Mu.m, and still more preferably 5. Mu.m. According to the invention, the luminescent powder materials with uniform morphology and size are obtained through screening, so that the influence of different internal stresses and different performance optimization degrees on the optimization effect of the luminescent powder materials with different particle diameters under the same quenching conditions is avoided.
In the present invention, the protective atmosphere is preferably the same as that of the original sample of the luminescent material.
In the invention, the target temperature for heating is preferably not more than the final sintering temperature of the original sample of the luminescent material, so that the influence of high temperature on the crystal structure is avoided; the heating is preferably performed in a high temperature furnace. The invention provides more extreme quenching conditions and more rapid cooling speed through heating, so as to realize the micro adjustment of the crystal structure of the luminescent powder, thereby improving the luminescence performance. In the present invention, the holding time of the heating is preferably 10 minutes.
After the heating is completed, the present invention preferably removes the resulting material immediately to a liquid cooling medium for quenching.
In the present invention, the liquid cooling medium preferably includes liquid nitrogen or liquid helium; the amount of the liquid cooling medium is not particularly limited, and the luminescent material powder can be completely immersed.
The quenching is preferably performed until the liquid cooling medium is completely volatilized, and the quenching is finished. The invention provides an extreme rapid cooling process through quenching, so that the crystal structure of the material is finely adjusted, and finally, the crystal field of the material and the energy transfer and conversion efficiency are changed, and further, the luminous color and the intensity of the material are changed.
In the present invention, the Sr 3-x Al 2 O 5 Cl 2 :xTb 3+ The quenching temperature of the luminescent powder is preferably 200 to 1000 ℃, more preferably 200 to 800 ℃, and even more preferably 400 to 600 ℃.
In the present invention, the ZnS: yCu + The quenching temperature of the luminescent powder is preferably 200 to 800, more preferably 400 to 600 ℃.
The invention has no special requirement on the specification of the container used for quenching, and the container well known in the art can be selected according to actual requirements.
After the quenching is finished, the invention preferably collects the powder luminescent material for drying to obtain the quenched luminescent material. The drying process is not particularly limited and may be performed according to a process well known in the art.
The luminescent property of the phosphor is a luminescence center (e.g. Tb 3+ And Cu + ) With a matrix (Sr) 3-x Al 2 O 5 Cl 2 And ZnS), crystallinity, defects, stress level, crystal form, and the like of the matrix affect energy transfer and transfer between the matrix and the light emitting center, and finally affect light emitting efficiency, so that light emitting intensity is changed. The energy band structure of the luminescence center is easily affected by surrounding crystal fields, strong crystal fields cause luminescence blue shift, weak crystal fields cause luminescence red shift, so that the intensity of the crystal fields changes the luminescence color of the luminescence center. The invention provides quick cooling conditions through quenching of the liquid cooling medium, and causes the crystal structure of the luminescent material to change, thereby changing the crystal field and the energy transfer efficiency, realizing the re-optimization of the luminescent performance (color/intensity) of the prepared luminescent powder, realizing the regulation and control of the mechanical and photoluminescence intensity of the material and also realizing the regulation and control of the photoinduced and mechanical luminescent colors.
The technical solutions of the present invention will be clearly and completely described in the following in connection with the embodiments of the present invention. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. 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
(1) In stoichiometric ratio (Sr) 2.99 Al 2 O 5 Cl 2 :Tb 0.01 ) Weighing SrCO 3 (AR)、Sr 2 Cl 2 .6H 2 O(AR)、Al 2 O 3 (AR) and Tb 4 O 7 (99.99%), each raw material was sufficiently ground in an agate mortar, dried and transferred to an alumina crucible;
(2) Placing an alumina crucible in a box-type resistance furnace, presintering for 4 hours at 900 ℃, grinding the presintered sample into powder, pressing and forming (with the diameter of 20mm and the thickness of 2 mm) under 50MPa, and sintering for 4 hours at 1200 ℃ in the box-type resistance furnace in air; cooling to room temperature, taking out the sample, grinding into powder again to obtain Sr 2.99 Al 2 O 5 Cl 2 :Tb 0.01 A luminescent powder;
(3) The Sr prepared 2.99 Al 2 O 5 Cl 2 :Tb 0.01 Sieving the luminous powder with a mesh sieve with a pore diameter of 5 μm and a pore diameter of 30 μm in sequence, and then heating to 200 ℃, 400 ℃, 600 ℃, 800 ℃ and 1000 ℃ in a box-type resistance furnace respectively and preserving heat for 10min;
(4) Sr to be preheated 2.99 Al 2 O 5 Cl 2 :Tb 0.01 Taking out the luminescent powder from the box-type resistance furnace, quickly immersing the luminescent powder in liquid nitrogen, and drying the luminescent powder after the liquid nitrogen is completely volatilized to obtain quenched Sr 2.99 Al 2 O 5 Cl 2 :Tb 0.01 And (5) luminescent powder.
Example 2
(1) In stoichiometric ratio (ZnS: cu) 0.01 ) ZnS (99.99%) and CuCl were weighed out 2 (99.99%), the raw material was sufficiently ground in an agate mortar, dried and transferred to an alumina crucible;
(2) Placing the crucible in a tube furnace, sintering at 1150 ℃ in nitrogen for 4 hours, cooling the sintered sample along with the furnace to room temperature, and grinding into powder to obtain ZnS: cu 0.01 A luminescent powder;
(3) The ZnS: cu prepared 0.01 The luminous powder is sequentially sieved by a mesh sieve with the aperture of 2 mu m and 5 mu mSieving, heating to 200deg.C, 400deg.C, 600deg.C and 800deg.C in a box-type resistance furnace (nitrogen protection), respectively, and maintaining for 10min;
(4) Preheating ZnS: cu 0.01 Taking out the luminescent powder from the box-type resistance furnace, quickly immersing the luminescent powder in liquid nitrogen, and drying the luminescent powder after the liquid nitrogen is completely volatilized to obtain quenched ZnS: cu 0.01 And (5) luminescent powder.
Example 3
The only difference from example 1 is that: the concentration of Tb element is 6%, the pressing pressure is 40MPa, the presintering temperature is 800 ℃, the final sintering temperature is 1250 ℃, and the quenching low-temperature liquid cooling medium is liquid helium.
Example 4
The only difference from example 2 is that: the concentration of Cu element is 0.5%, the sintering temperature is 1100 ℃, the time is 3 hours, and the quenching low-temperature liquid cooling medium is liquid helium.
Characterization and performance testing
1. The powder luminescent material of example 1 was subjected to XRD test, mechanoluminescence test and photoluminescence test under the same test conditions after quenching at 200 ℃, 400 ℃, 600 ℃, 800 ℃ and 1000 ℃ as it is and the results obtained are shown in FIGS. 1 to 3. As can be seen from FIG. 1, sr changes with the quenching temperature 2.99 Al 2 O 5 Cl 2 :Tb 0.01 The crystal structure of the powder luminescent material is basically unchanged. As can be seen from fig. 2 and 3, the luminous intensity of both the photoinduced and mechanoluminescence increases with the quenching temperature, increases and decreases, and an optimum value is obtained at 600 ℃.
2. The powder luminescent material of example 2 was subjected to XRD test, mechanoluminescence test and photoluminescence test under the same test conditions after quenching at 200 ℃, 400 ℃, 600 ℃ and 800 ℃ as it is and the luminescent material as it is, respectively, and the obtained results are shown in FIGS. 4 to 6. As can be seen from FIG. 4, znS: cu, as the quenching temperature changes 0.01 The crystal structure of the powder luminescent material is basically unchanged. As can be seen from fig. 5 and 6, the emission color of both the photoinduced and mechanoluminescence red shifts with an increase in quenching temperature.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.

Claims (7)

1. A method for improving the performance of a luminescent material, comprising the steps of:
heating an original sample of the luminescent material in a protective atmosphere, and quenching in a liquid cooling medium until the liquid cooling medium volatilizes; the liquid cooling medium comprises liquid nitrogen or liquid helium;
the original sample of the luminescent material is Sr 3-x Al 2 O 5 Cl 2 :xTb 3+ Or ZnS: yCu + ；x＝0.001～0.06，y＝0.001～0.02；
The original sample of the luminescent material is Sr 3-x Al 2 O 5 Cl 2 :xTb 3+ When the temperature of the heated target is 200-1000 ℃, the final sintering temperature of the original sample of the luminescent material is 1200-1400 ℃;
the original sample of the luminescent material is ZnS yCu + And when the target temperature for heating is 200-800 ℃, the final sintering temperature of the original sample of the luminescent material is 900-1200 ℃.
2. The method according to claim 1, wherein the luminescent material raw sample is screened before heating, and the mesh screen used for screening has a pore size of 1-50 μm.
3. The method of claim 1, wherein the protective atmosphere is the same as the protective atmosphere used to prepare the original sample of luminescent material.
4. The method according to claim 1, characterized in that the Sr 3-x Al 2 O 5 Cl 2 :xTb 3+ The preparation method of the (C) comprises the following steps:
according to Sr 3-x Al 2 O 5 Cl 2 :xTb 3+ Chemical composition of SrCO 3 、Sr 2 Cl 2 ·6H 2 O、Al 2 O 3 And Tb 4 O 7 Mixing, pre-sintering, press forming and sintering the obtained mixed powder in sequence to obtain Sr 3-x Al 2 O 5 Cl 2 :xTb 3+ 。
5. The method according to claim 4, wherein the presintering temperature is 600-1200 ℃ and the holding time is 1-5 h; the sintering heat preservation time is 2-8 h.
6. The method according to claim 1, wherein ZnS: yCu + The preparation method of the (C) comprises the following steps:
according to ZnS: yCu + Chemical composition of ZnS and CuCl 2 Mixing, sintering the obtained mixed powder in the protection of nitrogen atmosphere to obtain ZnS yCu + And (5) luminescent powder.
7. The method of claim 6, wherein the sintering is performed for a soak time of 1 to 5 hours.
CN202210798578.0A 2022-07-06 2022-07-06 Method for improving performance of luminescent material Active CN115124995B (en)

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