CN110204209B - Up-conversion glass ceramic composite material of selective rare earth doped scandium-based fluorinated nanocrystalline - Google Patents
Up-conversion glass ceramic composite material of selective rare earth doped scandium-based fluorinated nanocrystalline Download PDFInfo
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Abstract
The invention discloses an up-conversion glass ceramic composite material of selective rare earth doped scandium-based fluoridized nanocrystalline. The glass ceramic is SiO2:66‑x‑y mol％；Al2O3:6mol％；K2CO3:9mol％；KF:18.8mol％；ScF3:x mol％；LnF3:y mol％；ErF30.2 percent; x is more than or equal to 16 and less than or equal to 20; when y is more than or equal to 1.6<6, embedding KSc in glass matrix2F7Nanocrystals, KSc2F7Nanocrystalline doping Ln3+/Er3+(ii) a When y is more than or equal to 6 and less than or equal to 12, KSc is inlaid in the glass matrix2F7And KLn2F7Nanocrystalline, nanocrystalline doped Er3+. The invention successfully obtains the alumina silicate glass matrix containing uniformly distributed orthorhombic KSc2F7Nanocrystalline, and simultaneously realizes the entry of rare earth ions into a crystal phase.
Description
Technical Field
The invention relates to the field of solid luminescent materials, in particular to a rare earth doped up-conversion luminescent glass ceramic composite material.
Background
In recent years, lanthanide doped up-conversion materials have wide application prospects in the field of photoelectrons (such as anti-counterfeiting, display, biological imaging and the like), wherein rare earth fluoride has inherent low phonon energy, higher chemical stability and is easy to react with Ln3+The dopant is combined with the other advantages, and the like, and the method is widely applied to various matrix materials. At present, Er is used3+And Tm3+To send outOptical center, Yb3+Hexagonal NaReF doped with sensitizer4(Re ═ Y, Gd, Lu) is considered to be the most efficient green and blue up-conversion material. Sc (Sc)3+As a rare earth element, the rare earth element has a unique electronic configuration and a small ionic radius, so that the rare earth element has different luminescence properties compared with the traditional rare earth up-conversion material, but has little research because the mismatch of the ionic radius of the rare earth element and the traditional rare earth is large and the rare earth element is difficult to dope. Therefore, it is necessary to find a new rare earth-dopable scandium-based up-conversion material.
The oxyfluoride glass ceramic is a composite up-conversion material combining the advantages of fluoride crystals and oxide glass matrix, has the spectral characteristics similar to or even better than those of fluoride, has the advantages of good mechanical properties and high thermal stability of oxide glass, and is a potential novel up-conversion material with high photo-thermal stability.
The invention provides a glass ceramic composite material for in-situ crystallization of selective rare earth doped scandium-based fluoride nanocrystals in glass, which has a different luminescence behavior from the conventional rare earth nanocrystals, has the characteristic of selective doping according to the radius of rare earth, and can realize color control of red, yellow and green areas by adjusting the proportion of the rare earth.
Disclosure of Invention
The invention aims to find a rare earth-doped scandium-based up-conversion material and develop the application of glass ceramics in new fields.
The glass component and the mol percentage (mol%) of the glass ceramic are as follows:
SiO2:66-x-y mol％；Al2O3:6mol％；K2CO3:9mol％；KF:18.8mol％；ScF3:x mol％；LnF3y mol% (one or more of Ln ═ Y, Yb, Lu); ErF3:0.2％；16≤x≤20；
When y is more than or equal to 1.6<6, the structural feature of the glass-ceramic is that KSc is inlaid in the glass matrix2F7Nanocrystals, KSc2F7Doping rare earth ions (Ln ═ Y, Yb, Lu) with specific small ionic radius in nano crystalOne or more) and Er3+，KSc2F7The volume content of the nano-crystal in the glass ceramic is about 12 percent.
When y is more than or equal to 6 and less than or equal to 12, the structural characteristic of the glass ceramic is that KSc is embedded in the glass matrix2F7Nanocrystal and KLn2F7Nanocrystals, KSc2F7Nanocrystal and KLn2F7Er doped with nanocrystals3+，KSc2F7The volume content of the nano-crystal in the glass ceramic is about 8 percent. KLn2F7The volume content of the nano-crystal in the glass ceramic is about 6 percent.
The preparation method of the glass ceramic adopts the traditional melting quenching method and the subsequent crystallization heat treatment, and the specific preparation process is as follows:
mixing powder raw material SiO2、Al2O3、K2CO3、KF、LnF3、ScF3、LnF3(Ln ═ Y, Yb, Lu) and ErF3Weighing the compounds according to the mol percentage, grinding the compounds in an agate mortar uniformly, placing the mixture in a crucible, heating the mixture in a resistance furnace to 1350-; the annealed glass is continuously heated and insulated for 2 hours at the temperature of 600-800 ℃ to crystallize, and KSc is obtained2F7A transparent glass ceramic composite material of nanocrystalline.
The glass ceramic composite material of the invention takes aluminosilicate glass as a matrix to precipitate evenly distributed orthorhombic phase KSc2F7The nano crystal has a particle size of 20-50 nm.
Quadrature phase KSc in glass ceramic composite material of the present invention2F7The nanocrystalline separation takes rare earth ions (such as Y, Yb and Lu) with specific small ionic radius as nucleating agent, and partial rare earth ions enter KSc2F7In the crystal.
By adopting the glass ceramic components and the preparation process, the glass ceramic containing uniformly distributed orthorhombic KSc in the aluminosilicate glass matrix is successfully obtained2F7Nanocrystalline, and simultaneously realizes the entry of rare earth ions into a crystalline phasePerforming the following steps; er is realized by regulating and controlling the doping concentration ratio (Ln/Sc ratio) of rare earth ions and scandium fluoride3+The up-conversion luminescence color can be regulated and controlled in red, yellow and green areas.
The glass ceramic composite material disclosed by the invention is simple in preparation process and low in cost, and simultaneously proves that the precipitated nanocrystals have selective ion replacement for doped rare earth elements, and rare earth ions (such as La, Ce, Gd, Eu and the like) with large mismatch can not be doped into the nanocrystals Sc3+And rare earth ions (such as Y, Yb and Lu) with small mismatching can be doped into the nanocrystal, and the behavior of selectively entering the nanocrystal by the rare earth ions has potential application value.
Drawings
FIG. 1 is an X-ray diffraction pattern of a glass-ceramic sample of example 1;
FIG. 2 is a field emission transmission electron micrograph of a glass-ceramic sample of example 1;
FIG. 3 is an upconversion emission spectrum of a glass-ceramic sample under 980nm laser irradiation in example 1.
Detailed Description
The present invention is further illustrated by the following examples, which are not intended to be limiting, and any modifications and variations that may be made to the present invention are intended to be within the scope of the present invention.
The glass component and the mol percentage (mol%) of the glass ceramic are as follows:
SiO2:66-x-y mol％；Al2O3:6mol％；K2CO3:9mol％；KF:18.8mol％；ScF3:x mol％；LnF3y mol% (one or more of Ln ═ Y, Yb, Lu); ErF3:0.2％；16≤x≤20；
When y is more than or equal to 1.6<6, the structural feature of the glass-ceramic is that KSc is inlaid in the glass matrix2F7Nanocrystals, KSc2F7Doping rare earth ions (one or more of Ln ═ Y, Yb and Lu) with specific small ionic radius and Er in the nano crystal3+，KSc2F7The volume content of the nano-crystal in the glass ceramic is about 12 percent.
When y is more than or equal to 6 and less than or equal to 12, the structural characteristic of the glass ceramic is that KSc is embedded in the glass matrix2F7Nanocrystal and KLn2F7Nanocrystals, KSc2F7Nanocrystal and KLn2F7Er doped with nanocrystals3+，KSc2F7The volume content of the nano-crystal in the glass ceramic is about 8 percent. KLn2F7The volume content of the nano-crystal in the glass ceramic is about 6 percent.
The preparation method of the glass ceramic adopts the traditional melting quenching method and the subsequent crystallization heat treatment, and the specific preparation process is as follows:
mixing powder raw material SiO2、Al2O3、K2CO3、KF、LnF3、ScF3、LnF3(Ln ═ Y, Yb, Lu) and ErF3Weighing the compounds according to the mol percentage, grinding the compounds in an agate mortar uniformly, placing the mixture in a crucible, heating the mixture in a resistance furnace to 1350-; the annealed glass is continuously heated and insulated for 2 hours at the temperature of 600-800 ℃ to crystallize, and KSc is obtained2F7A transparent glass ceramic composite material of nanocrystalline.
Example 1: mixing SiO2、Al2O3、K2CO3、KF、ScF3、YbF3And ErF3According to 44.4SiO2:6Al2O3:9K2CO3:18.8KF:20ScF3:1.6YbF3:0.2ErF3The mixture ratio (molar ratio) is accurately weighed, the mixture is uniformly ground in an agate mortar and then is placed in a crucible, the mixture is heated in a resistance furnace to 1500 ℃ and is insulated for 30 minutes, and then the glass melt is quickly poured into a copper mold preheated at 400 ℃ for molding; the annealed glass is continuously heated and insulated for 2 hours at 750 ℃ to crystallize to obtain Yb3+/Er3+Doped KSc2F7An embedded transparent glass ceramic composite.
The X-ray diffraction pattern shows that the precursor glass is typical amorphousStructure, precipitation of orthorhombic structures KSc in aluminosilicate glass substrates after heat treatment2F7Crystal phase (FIG. 1), and transmission electron microscopy shows that a large amount of KSc with the size of about 40-50nm is uniformly distributed in the glass2F7Crystal grains (figure 2), and a fluorescence spectrum test shows that the glass ceramic emits orange-red light under the excitation of 980nm (figure 3).
Example 2: mixing SiO2、Al2O3、K2CO3、KF、ScF3、YbF3And ErF3According to 38SiO2:6Al2O3:9K2CO3:18.8KF:16ScF3:12YbF3:0.2ErF3The mixture ratio (molar ratio) is accurately weighed, the mixture is uniformly ground in an agate mortar and then is placed in a crucible, the mixture is heated in a resistance furnace to 1500 ℃ and is insulated for 30 minutes, and then the glass melt is quickly poured into a copper mold preheated at 400 ℃ for molding; the annealed glass is continuously heated and preserved at 750 ℃ for 2 hours to crystallize, and Er is obtained3+Doped simultaneous orthogonal structure KYb2F7And quadrature structure KSc2F7The sample of the transparent glass ceramic composite material of the two-phase nanocrystalline emits bright red light under the excitation of 980 nm.
Example 3: mixing SiO2、Al2O3、K2CO3、KF、ScF3、LuF3And ErF3According to 44.4SiO2:6Al2O3:9K2CO3:18.8KF:20ScF3:1.6LuF3:0.2ErF3The mixture ratio (molar ratio) is accurately weighed, the mixture is uniformly ground in an agate mortar and then is placed in a crucible, the mixture is heated in a resistance furnace to 1500 ℃ and is insulated for 30 minutes, and then the glass melt is quickly poured into a copper mold preheated at 400 ℃ for molding; the annealed glass is continuously heated and insulated for 2 hours at 750 ℃ to crystallize to obtain Lu3+/Er3+Doped KSc2F7An embedded transparent glass-ceramic composite, the glass-ceramic emitting orange light under 980nm excitation.
Example 4: mixing SiO2、Al2O3、K2CO3、KF、ScF3、LuF3And ErF3According to 38SiO2:6Al2O3:9K2CO3:18.8KF:16ScF3:12LuF3:0.2ErF3The mixture ratio (molar ratio) is accurately weighed, the mixture is uniformly ground in an agate mortar and then is placed in a crucible, the mixture is heated in a resistance furnace to 1500 ℃ and is insulated for 30 minutes, and then the glass melt is quickly poured into a copper mold preheated at 400 ℃ for molding; the annealed glass is continuously heated and preserved at 750 ℃ for 2 hours to crystallize, and Er is obtained3+Doped simultaneous containing orthorhombic structure KLu2F7And quadrature structure KSc2F7The sample of the transparent glass ceramic composite material of the two-phase nanocrystalline emits bright yellow light under the excitation of 980 nm.
Example 5: mixing SiO2、Al2O3、K2CO3、KF、ScF3、YF3And ErF3According to 44.4SiO2:6Al2O3:9K2CO3:18.8KF:20ScF3:1.6YF3:0.2ErF3The mixture ratio (molar ratio) is accurately weighed, the mixture is uniformly ground in an agate mortar and then is placed in a crucible, the mixture is heated in a resistance furnace to 1500 ℃ and is insulated for 30 minutes, and then the glass melt is quickly poured into a copper mold preheated at 400 ℃ for molding; the annealed glass is continuously heated and insulated for 2 hours at 750 ℃ to crystallize to obtain Y3+/Er3+Doped KSc2F7An embedded transparent glass-ceramic composite, the glass-ceramic emitting orange light under 980nm excitation.
Example 6: mixing SiO2、Al2O3、K2CO3、KF、ScF3、YF3And ErF3According to 38SiO2:6Al2O3:9K2CO3:18.8KF:16ScF3:12YF3:0.2ErF3The mixture ratio (molar ratio) is accurately weighed, the mixture is uniformly ground in an agate mortar and then is placed in a crucible, the mixture is heated in a resistance furnace to 1500 ℃ and is insulated for 30 minutes, and then the glass melt is quickly poured into a copper mold preheated at 400 ℃ for molding; the annealed glass is continuously added at 750 DEG CThermally insulating for 2 hours to crystallize to obtain Er3+Doping and simultaneously containing KYF with hexagonal structure4And quadrature structure KSc2F7The sample of the transparent glass ceramic composite material of the two-phase nanocrystalline emits bright green light under the excitation of 980 nm.
Example 7: mixing SiO2、Al2O3、K2CO3、KF、ScF3、YF3And ErF3According to 44SiO2:6Al2O3:9K2CO3:18.8KF:16ScF3:6YF3:0.2ErF3The mixture ratio (molar ratio) is accurately weighed, the mixture is uniformly ground in an agate mortar and then is placed in a crucible, the mixture is heated in a resistance furnace to 1500 ℃ and is insulated for 30 minutes, and then the glass melt is quickly poured into a copper mold preheated at 400 ℃ for molding; the annealed glass is continuously heated and preserved at 750 ℃ for 2 hours to crystallize, and Er is obtained3+Doping and simultaneously containing KYF with hexagonal structure4And quadrature structure KSc2F7The sample of the transparent glass ceramic composite material of the two-phase nanocrystalline emits bright yellow light under the excitation of 980 nm.
The above embodiments are not intended to limit the present invention, and the present invention is not limited to the above embodiments, and all embodiments are within the scope of the present invention as long as the requirements of the present invention are met.
Claims (3)
1. The up-conversion glass ceramic composite material of the selective rare earth doped scandium-based fluoridated nanocrystalline is characterized in that the glass components and the molar percentage are as follows:
SiO2: 66-x-y mol%； Al2O3: 6 mol%； K2CO3: 9 mol%；KF: 18.8 mol%；ScF3: x mol%； LnF3y mol% (one or more of Ln = Y, Yb, Lu); ErF30.2 mol percent; wherein x is more than or equal to 16 and less than or equal to 20, and y is more than or equal to 1.6<6；
The structural feature of the glass ceramic is that KSc is inlaid in the glass matrix2F7Nanocrystals, KSc2F7Nanocrystalline doping rare earth ions Ln with specific small ionic radius3+And Er3+；KSc2F7The volume content of the nano-crystal in the glass ceramic is up to 12 percent.
2. The up-conversion glass ceramic composite material of the selective rare earth doped scandium-based fluoridated nanocrystalline is characterized in that the glass components and the molar percentage are as follows:
SiO2: 66-x-y mol%； Al2O3: 6 mol%； K2CO3: 9 mol%；KF: 18.8 mol%；ScF3: x mol%； LnF3y mol% (one or more of Ln = Y, Yb, Lu); ErF30.2 mol percent; wherein x is more than or equal to 16 and less than or equal to 20, and y is more than or equal to 6 and less than or equal to 12;
the structural feature of the glass ceramic is that KSc is inlaid in the glass matrix2F7Nanocrystal and KLn 2F7Nanocrystals, KSc2F7Nanocrystal and KLn 2F7Er doped with nanocrystals3+；
KSc2F7The volume content of the nano-crystal in the glass ceramic reaches 8 percent; KLn 2F7The volume content of the nano-crystal in the glass ceramic is up to 6 percent.
3. A method for preparing the up-conversion glass-ceramic composite material of the selective rare earth doped scandium-based fluorinated nanocrystal of claim 1 or 2, which is characterized in that the method comprises:
mixing powder raw material SiO2、Al2O3、K2CO3、KF、LnF3(one or more of Ln = Y, Yb, Lu), ScF3And ErF3The compound is prepared according to the molar percentage of 66-x-y: 6: 9: 18.8: x: y: 0.2, weighing the mixture, uniformly grinding the mixture in an agate mortar, putting the mixture in a crucible, heating the mixture in a resistance furnace to 1350-; pouring the glass melt into a copper mold preheated at the temperature of 400-500 ℃ for molding to obtain precursor glass; the annealed precursor glass is continuously heated and insulated for 2 hours at the temperature of 600-800 ℃ to crystallize, and KSc is obtained2F7A transparent glass ceramic composite material of nanocrystalline.
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| RU2295495C1 (en) * | 2005-11-01 | 2007-03-20 | Государственное образовательное учреждение высшего профессионального образования "Московский государственный институт стали и сплавов" (технологический университет) | COMPOUND KSc2F7 PREPARATION METHOD |
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