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US-20260125310-A1 - RARE-EARTH DOPED FUNCTIONAL NANOCRYSTAL GLASS CERAMIC AND METHOD OF PREPARING THE SAME

US20260125310A1US 20260125310 A1US20260125310 A1US 20260125310A1US-20260125310-A1

Abstract

Disclosed is an Er 3+ doped Lu 4 Zr 3 O 12 functional nanocrystal glass ceramic and a method of preparing the same. The glass ceramic comprises components in mole percentages of: 57% to 59% of SiO 2 , 12% to 16% of Al 2 O 3 , 14% to 18% of ZnO, 6% to 8% of Li 2 O, 3% to 5% of ZrO 2 , 2% to 3% of Lu 2 O 3 , 0.05% to 0.2 of Er 2 O 3 . Through composition design and heat treatment process control, the present invention achieves the controllable preparation of Er 3+ rare-earth ion-doped Lu 4 Zr 3 O 12 functional nanocrystals within the glass. This functional nanocrystalline glass has potential application value in low-temperature optical thermometry.

Inventors

  • Gang Zhang
  • Wenyue Sun
  • SIHUA MENG
  • Zhipeng Tang
  • Kaiming Wu
  • TAO FU
  • JUN ZONG

Assignees

  • WUHAN UNIVERSITY OF SCIENCE AND TECHNOLOGY
  • SHANGHAI SIIC ZHENTAI CHEMICAL CO., LTD.

Dates

Publication Date
20260507
Application Date
20251028
Priority Date
20241105

Claims (4)

  1. 1 . A rare-earth ion doped functional nanocrystal glass ceramic, comprising a glass matrix and Lu 4 Zr 3 O 12 nanocrystals doped with Er 3+ dispersed within the glass matrix, the glass ceramic comprises components in mole percentages of: 57% to 59% of SiO 2 , 12% to 16% of Al 2 O 3 , 14% to 18% of ZnO, 6% to 8% of Li 2 O, 3% to 5% of ZrO 2 , 2% to 3% of Lu 2 O 3 , 0.05% to 0.2 of Er 2 O 3 , a total mole percent of the components is 100%.
  2. 2 . The rare-earth ion doped functional nanocrystal glass ceramic according to claim 1 , wherein size of the nanocrystal is 5-10 nm.
  3. 3 . The rare-earth ion doped functional nanocrystal glass ceramic according to claim 1 , wherein the glass ceramic further comprises 0.1 mol % to 0.3 mol % of Sb 2 O 3 .
  4. 4 . A method for preparing the rare-earth ion doped functional nanocrystal glass ceramic according to claim 1 , comprising steps of: weighing and uniformly mixing all raw materials to obtain a raw material mixture; placing the raw material mixture in a crucible, and melting at 1600° C. to 1650° C. from 1 h to 3 h to obtain a molten glass; pouring the molten glass into a mold for quenching to obtain a quenched glass; annealing the quenched glass at 600-650° C. for 2-4 hours and cooling to room temperature to obtain an as-prepared glass; heat-treating the as-prepared glass at 700-800° C. for 5-7 hours to obtain the Lu 4 Zr 3 O 12 functional nanocrystal glass ceramic.

Description

FIELD The disclosure relates to the field of glass, and in particular to an Er3+ doped Lu4Zr3O12 functional nanocrystal glass ceramic and a method of preparing the same. BACKGROUND OF THE INVENTION Oxides composed of RE2O3-MO2 (RE=La—Lu; M=Ti, Zr, Hf) are interesting materials and possess many interesting properties. These oxides could have defect-fluorite structure, pyrochlore structure, or delta (δ)-phase rhombohedral structure, depending on the chemical compositions of these oxides and exhibit order-disorder transitions, such as pyrochlore to defect fluorite, rhombohedral 8-phase to defect fluorite, and β-phase (hexagonal) to defect fluorite, which are strongly dependent on the temperature and the annealing time. Chemical formula of oxides in these systems can be generally expressed as [AB]2O8-x such as A2B2O7 pyrochlores, A4B3O12 δ-phase, and A2BO5 β-phase, where A and B are trivalent and tetravalent cations, respectively. In most cases, these oxides have good physical and chemical properties, especially the low thermal conductivity and high solubility of rare-earth ions. These particular properties make these oxides promising for applications as thermal barrier coatings, nuclear waste form, host for luminescent rare-earth ions, and pigments. In recent years, δ-phase RE4Zr3O12 crystals are intensely studied for their optical properties, such as UV-emission from Y4Zr3O12:Gd3+, red-emission from Y4Zr3O12:Eu3+ for latent fingerprint. Most of these materials are synthesized through the sol-gel technique followed by high temperature sintering, sintering, co-precipitation or mechanical activation, and solution combustion method. However, δ-phase RE4Zr3O12 crystals were not directly synthesized in glasses. Therefore, there is a need to provide a new material and method capable of precipitating δ-phase RE4Zr3O12 in glass. BRIEF DESCRIPTION OF DRAWINGS To describe technical solutions in embodiments of the disclosure more clearly, accompanying drawings required in description of the embodiments will be briefly introduced below. Apparently, the accompanying drawings in the following description merely show some embodiments of the disclosure, and a person of ordinary skill in the art can still derive other accompanying drawings from structures shown in these accompanying drawings without creative efforts. FIG. 1 is XRD patterns of Lu4Zr3O12 functional nanocrystal glass ceramic obtained by heat-treating as-prepared (hereinafter referred to as AP) glass of First Embodiment at different temperatures. FIG. 2 shows transmission electron microscopy (TEM) images of the functional nanocrystal glass ceramic obtained at 760° C. in FIG. 1, where Chart a illustrates a bright-field image, Chart b illustrates a magnified image, and Chart c illustrates an HR-TEM image. FIG. 3 shows EDS mapping results of the functional nanocrystal glass ceramic obtained at 760° C. in FIG. 1, where Chart a illustrates dual-field image of the specimen, Chart b illustrates distribution of Lu, Chart c illustrates distribution of Zr, Chart d illustrates distribution of Er, Chart e illustrates distribution of Si, Chart f illustrates distribution of Zn, Chart g illustrates distribution of Al, and Chart h illustrates distribution of O. FIG. 4 shows temperature dependent emission properties of the functional nanocrystal glass ceramic heat-treated at 760° C. for 6 h, where Chart a illustrates normalized emission spectra of the functional nanocrystal glass ceramic, Chart b illustrates emission intensity ratio between the 2H11/2→4I15/2 and 4S3/2→4I15/2 transitions, and Chart c illustrates relative sensitivity (SR) and absolute sensitivity (SA) curves. DETAILED DESCRIPTION OF THE INVENTION The following will provide a further explanation of the present disclosure in conjunction with the accompanying drawings. The patent or application file contains at least one drawing executed in color, which is for illustrative purpose only and forms no part thereof. First Embodiment An Er3+ doped Lu4Zr3O12 functional nanocrystal glass ceramic is provided in the first embodiment. The glass ceramic includes a glass matrix and nanocrystals composed of Lu4Zr3O12 and Er3+ within the glass matrix. The glass ceramic composition, in mole percent, includes 58 mol % of SiO2, 13 mol % of Al2O3, 15 mol % of ZnO, 7 mol % of Li2O, 4 mol % of ZrO2, 2.9 mol % of Lu2O3, 0.1 mol % of Er2O3, and additionally includes 0.2 mol % of Sb2O3 as an extra component. The raw materials are weighed according to the above composition and mixed uniformly, then melted at 1630° C. for 2 h in platinum crucible and then poured into brass mold for quenching. The quenched glass is swiftly transferred into a muffle furnace for annealing at 630° C. for 3 h and cooling down to room temperature with furnace by switching off the power. Glass thus obtained is named as as-prepared (hereinafter referred to as AP) glass. The AP glass is then heat-treated at 700° C., 720° C., 740° C., and 760° C. for 6 hours to obtain t