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Cobalt-nickel co-doped ZnAl2O4 nanocrystalline glass and preparation method thereof

A znal2o4, co-doping technology, applied in glass manufacturing equipment, glass molding, manufacturing tools, etc., can solve the problems of reducing the service life of glass, growing crystals, and consuming time

Pending Publication Date: 2022-03-18
HAINAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the traditional preparation process of transparent glass-ceramics, it is necessary to continuously adjust the composition of spinel to obtain spinel nano-glass of suitable size. Therefore, it is necessary to adjust the composition of the glass many times, which is very time-consuming.
At the same time, in order to obtain high-strength spinel nano glass, long-term heat treatment is necessary, but this may cause the crystals inside the glass to grow continuously, and the mismatch between the larger crystal size and the expansion coefficient of the glass phase will cause the glass to be in Cracks appear during use, reducing the service life of the glass

Method used

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  • Cobalt-nickel co-doped ZnAl2O4 nanocrystalline glass and preparation method thereof
  • Cobalt-nickel co-doped ZnAl2O4 nanocrystalline glass and preparation method thereof

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preparation example Construction

[0025] The invention provides a cobalt-nickel co-doped ZnAl 2 o 4 The preparation method of nanocrystalline glass comprises the following steps:

[0026] A) will include SiO 2 、Al 2 o 3 , ZnO, TiO 2 , CoO, NiO and Mn 2 o 3 The raw materials are mixed, melted, and solidified;

[0027] The SiO 2 、Al 2 o 3 , ZnO, TiO 2 , CoO, NiO and Mn 2 o 3 The molar ratio is 20~50:8~50:9~23:2~16:0.002~0.5:0.003~0.9:0.002~0.7;

[0028] B) Heat the solidified sample at 540-560°C, then cool it to 190-210°C at 0.8-1.2°C / min, and then cool it naturally to obtain a glass sample;

[0029] C) The glass sample is sliced, polished, nucleated, and crystallized to obtain cobalt-nickel co-doped ZnAl 2 o 4 nanocrystalline glass;

[0030] The crystallization is carried out in the presence of an electric field.

[0031] In step A):

[0032] In some embodiments of the present invention, the SiO 2 、Al 2 o 3 , ZnO, TiO 2 , CoO, NiO and Mn 2 o 3 The molar ratio is 20-50:8-50:9-23:2-16:0.0...

Embodiment 1

[0061] 1) Select SiO with a molar ratio of 25:50:23:2:0.002:0.003:0.002 2 、Al 2 o 3 , ZnO, TiO 2 , CoO, NiO and Mn 2 o 3 The raw materials are mixed in an alumina crucible, put into a silicon-molybdenum rod furnace at 1350°C for preheating, and then heated up to 1600°C at 10°C / min, kept for 3 hours and then poured into a 250°C iron plate to solidify and form;

[0062] 2) Put the solidified sample into the annealing furnace, keep it at 550°C for 2 hours, then cool it down to 200°C at 1°C / min, close the annealing furnace, and cool it down to room temperature naturally to obtain a glass sample;

[0063] 3) Cut the glass sample into thin slices of 2cm×2cm×0.5cm with a wire cutting machine, polish the upper and lower surfaces into a mirror surface, put it into a thermoelectric coupling device, and start the heating program to raise the temperature at 10°C / min to 650°C, nucleate at 650°C for 2 hours, heat up to 780°C at 10°C / min, crystallize at 780°C and apply an electric field...

Embodiment 2

[0071] 1) Select SiO with a molar ratio of 50:25:9:16:0.5:0.9:0.7 2 、Al 2 o 3 , ZnO, TiO 2 , CoO, NiO and Mn 2 o 3 The raw materials are mixed in an alumina crucible, put into a silicon-molybdenum rod furnace at 1350°C for preheating, and then heated up to 1600°C at 10°C / min, kept for 3 hours and then poured into a 250°C iron plate to solidify and form;

[0072] 2) Put the solidified sample into the annealing furnace, keep it at 550°C for 2 hours, then cool it down to 200°C at 1°C / min, close the annealing furnace, and cool it down to room temperature naturally to obtain a glass sample;

[0073] 3) Cut the glass sample into thin slices of 2cm×2cm×0.5cm with a wire cutting machine, polish the upper and lower surfaces into a mirror surface, put it into a thermoelectric coupling device, and start the heating program to raise the temperature at 10°C / min to 620°C, nucleate at 620°C for 2 hours, heat up to 800°C at 10°C / min, crystallize at 800°C and apply an electric field at th...

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Abstract

The invention relates to the technical field of glass ceramics, in particular to cobalt-nickel co-doped ZnAl2O4 nanocrystalline glass and a preparation method thereof. The preparation method comprises the following steps: A) mixing SiO2, Al2O3, ZnO, TiO2, CoO, NiO and Mn2O3 according to a molar ratio of (20 to 50): (8 to 50): (9 to 23): (2 to 16): (0.002 to 0.5): (0.003 to 0.9): (0.002 to 0.7), melting, and solidifying and forming; b) preserving the heat of the solidified and formed sample at 540-560 DEG C, cooling to 190-210 DEG C at the speed of 0.8-1.2 DEG C / min, and naturally cooling to obtain a glass sample; and C) slicing the glass sample, polishing, nucleating and crystallizing to obtain the cobalt-nickel co-doped ZnAl2O4 nanocrystalline glass, the devitrification is carried out in the presence of an electric field. And the obtained nanocrystalline glass has excellent light transmission and mechanical properties.

Description

technical field [0001] The invention relates to the technical field of glass ceramics, in particular to a cobalt-nickel co-doped ZnAl 2 o 4 Nanocrystalline glass and its preparation method. Background technique [0002] Manganese, cobalt, nickel doped ZnAl 2 o 4 Spinel nano glass is mainly used in the field of optics. Glass is widely used in our life, and has many application prospects in construction, medical supplies and optical instruments. At the same time, spinel nano glass has excellent mechanical properties and can be used in high-strength devices. In the traditional preparation process of transparent glass-ceramics, it is necessary to continuously adjust the composition of spinel to obtain spinel nano-glass with suitable size. Therefore, it is necessary to adjust the composition of the glass many times, which is very time-consuming. At the same time, in order to obtain high-strength spinel nano glass, long-term heat treatment is necessary, but this may cause th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C03C10/06C03B19/02C03B25/02C03B32/02
CPCC03C10/0036C03B19/02C03B25/025C03B32/02
Inventor 李长久易兰林
Owner HAINAN UNIVERSITY