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mg 2+ /ge 4+ replace ga 3+ doped cr 3+ Zinc gallate-based near-infrared long afterglow material and preparation method

A technology of zinc gallate and outer length, which is applied in the field of material science, can solve the problems of insufficient luminous intensity and afterglow time for long-term observation, coarse particles, and difficulty entering the living body, etc., and achieves low cost, simple operation, and excellent uniformity Effect

Active Publication Date: 2020-07-24
NORTHEASTERN UNIV LIAONING
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

The recently developed near-infrared long-lasting materials are mostly prepared by solid-phase method and hydrothermal method. Compared with the sol-gel method, the particles prepared by the solid-phase method are coarse and difficult to enter the organism. Although the particles prepared by the hydrothermal method are small, However, its luminous intensity and afterglow time cannot meet the requirements of long-term observation in vivo

Method used

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  • mg <sup>2+</sup> /ge <sup>4+</sup> replace ga <sup>3+</sup> doped cr <sup>3+</sup> Zinc gallate-based near-infrared long afterglow material and preparation method
  • mg <sup>2+</sup> /ge <sup>4+</sup> replace ga <sup>3+</sup> doped cr <sup>3+</sup> Zinc gallate-based near-infrared long afterglow material and preparation method
  • mg <sup>2+</sup> /ge <sup>4+</sup> replace ga <sup>3+</sup> doped cr <sup>3+</sup> Zinc gallate-based near-infrared long afterglow material and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Embodiment 1 (x=0.01, y=0.01)

[0030] Accurately weigh 1.7536g EDTA and 0.0012g GeO 2 Put it into a beaker, add an appropriate amount of deionized water, start stirring, then add 5mL of ammonia water according to experience, and accurately measure 2mL of Zn(NO 3 ) 2 solution (1mol / L), 9.9mL of Ga(NO 3 ) 3 solution (0.4mol / L), 0.05mL of Mg(NO 3 ) 2 solution (0.2mol / L) and 0.2mL of Cr(NO 3 ) 3 solution (0.1mol / L), add deionized water to 50mL while stirring. The above solution was transferred to a water bath and stirred at a water temperature of 70 °C until the GeO 2 Completely dissolved, and distilled in water for 5 hours until the water evaporated, the solution formed a gel state. Take out the beaker, transfer the gel to an oven, and bake at 180°C for 6 hours to obtain ZnGa 1.99 (Mg 2+ / Ge 4+ ) 0.01 o 4 :0.01Cr 3+ Black precursor powder. After grinding the above precursors, they were calcined at 700°C for 5 hours in a flowing oxygen atmosphere to obtain ...

Embodiment 2

[0031] Embodiment 2 (x=0.5, y=0.05)

[0032] Accurately weigh 2.6304g EDTA and 0.0523gGeO 2 Add deionized water, accurately measure 2mL Zn(NO 3 ) 2 Solution (1mol / L), 7.25mL Ga(NO 3 ) 3 solution (0.4mol / L), 2.5mL Mg(NO 3 ) 2solution (0.2mol / L) and 1mL Cr(NO 3 ) 3 solution (0.1mol / L), added to the solution, and ammonia water was added dropwise until clarification. The above solution was transferred to a water bath, and stirred for 7 h at a water temperature of 80° C. to form a gel. Take out the beaker, transfer the gel to an oven, and bake at 300°C for 2 hours to obtain ZnGa 1.5 (Mg 2 + / Ge 4+ ) 0.5 o 4 :0.05Cr 3+ Black precursor powder. After the above precursor is ground, it is calcined at 1000°C for 2 hours in a flowing oxygen atmosphere to obtain the near-infrared long-lasting fluorescent material ZnGa 1.5 (Mg 2+ / Ge 4+ ) 0.5 o 4 :0.05Cr 3+ .

Embodiment 3

[0033] Embodiment 3 (x=1, y=0.005)

[0034] Accurately weigh 3.5069g EDTA and 0.1046g GeO 2 Add deionized water, accurately measure 2mL Zn(NO 3 ) 2 Solution (1mol / L), 7.465mL Ga(NO 3 ) 3 solution (0.4mol / L), 5mL Mg(NO 3 ) 2 solution (0.2mol / L) and 0.01mLCr(NO 3 ) 3 solution (0.1mol / L), added to the solution, and ammonia water was added dropwise until clarification. The above solution was transferred to a water bath, and stirred at a water temperature of 85° C. for 6 h to form a gel. Take out the beaker, transfer the gel to an oven, and bake at 230°C for 3 hours to obtain ZnGa(Mg 2 + / Ge 4+ )O 4 :0.005Cr 3+ Black precursor powder. After the above precursors were ground, they were calcined at 1400 °C for 4 h in a flowing oxygen atmosphere to obtain the near-infrared long-lasting fluorescent material ZnGa(Mg 2+ / Ge 4+ )O 4 :0.005Cr 3+ .

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Abstract

The invention belongs to the field of material science, and discloses a Cr<3+> doped zinc gallate-based near infrared long afterglow material replacing Ga<3+> by Mg<2+> / Ge<4+> and a preparation method. A sol-gel method is used, a certain complexing agent is added, and Mg<2+> / Ge<4+> ion pairs are used to replace Ga<3+> to generate more traps. Through calcination at 700-1400 DEG C, obtained near infrared long afterglow nano-phosphor powder ZnGa2-x(Mg<2+> / Ge<4+>)xO4:yCr<3+> has small size, has good dispersibility, excellent uniformity, good luminescence performance, long afterglow time and otherexcellent performance, and can be well applied to the field of bioimaging. The Cr<3+> doped zinc gallate-based near infrared long afterglow material replacing Ga<3+> by Mg<2+> / Ge<4+> and the preparation method have the advantages of simple operation, low cost and environmental protection, show a good theoretical basis for preparation of novel commercial phosphor powder, and have extremely high guiding significance and application prospect.

Description

technical field [0001] The invention belongs to the field of material science, in particular to a Mg 2+ / Ge 4+ replace Ga 3+ doped Cr 3+ Zinc gallate-based near-infrared long afterglow material and its preparation method. Background technique [0002] Long-lasting fluorescent materials are materials that absorb and store energy such as visible light, ultraviolet light, and X-rays. They can continue to emit light after the energy is cut off. They can also be called light-storing luminescent materials or luminous materials. Long afterglow materials can store energy in traps, and when the photoexcitation of the material is stopped, it is accompanied by the phenomenon of continuous luminescence. Due to this remarkable feature, long afterglow materials have been applied in the fields of lighting, emergency indication, light energy storage, detection, transportation and military affairs. With the emergence of long-lasting nanometer-sized materials, in the field of biological ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/66
CPCC09K11/682
Inventor 朱琦夏侯俊卿
Owner NORTHEASTERN UNIV LIAONING
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