Cr<3+>-doped zinc gallate near-infrared long-afterglow luminescent nanoparticles and preparation method

[0039] Example 1

[0040] Add 10ml 0.1mol/L Zn(NO 3 ) 2 Solution, 19.95ml 0.1mol/L Ga(NO 3 ) 3 Solution, 0.1ml 0.05mol/L Cr(NO 3 ) 3 After stirring the solution, the reactant nitrate mixture is obtained. Then, 0.2459 g of glycine and 0.1180 g of carbohydrazide were added to the above mixed solution as organic fuel. Slowly evaporate in a water bath at 80°C until the mixed solution becomes a uniform and transparent sol. The above-mentioned sol is put into a muffle furnace with a furnace temperature of 600° C. and ignited. The combustion reaction is completed rapidly within several tens of seconds, and a white fluffy product is obtained. The above white product was transferred into an agate mortar, and 5 mmol/L sodium hydroxide solution was added to fully grind for 1 hour. After grinding the mixed slurry into distilled water and ultrasonic treatment for 1h, the mass ratio of distilled water to white product is 1000:1. After standing for 72h, take the supernatant and centrifuge at 10000rpm for 10min to obtain near infrared with average particle size less than 100nm Long afterglow luminescent nanoparticles. The atomic ratio composition of the near-infrared long afterglow luminescent nanoparticles is ZnGa 1.995 Cr 0.005 O 4.

[0041] Test the samples prepared in the examples:

[0042] Excitation and emission spectra of samples see figure 1 , Under the excitation of 254nm ultraviolet light, the sample produces Cr 3+ of 2 E→ 4 A 2 Broadband emission, the broadband emission peak ranges from 600nm to 850nm, and the peak is at 690-715nm. The excitation spectrum of the sample covers a wide area from the ultraviolet region to the red region.

[0043] The near-infrared afterglow attenuation curve of the sample see figure 2 The near-infrared afterglow attenuation curve of the sample is obtained by monitoring the relationship between the near-infrared afterglow emission intensity and the attenuation time of the sample at 693nm.

[0044] For the scanning electron micrograph of the sample, see image 3 As can be seen from the figure, the obtained near-infrared long afterglow luminescent nanoparticles are approximately spherical, with a uniform particle size distribution between 50-100nm, which can meet the requirements of biological imaging.

[0045] Example 2

[0046] Add 10ml Zn(NO 3 ) 2 Solution, 19.98ml Ga(NO 3 ) 3 Solution, 0.04ml Cr(NO 3 ) 3 The solution is stirred to obtain the reactant nitrate mixture. Then, 0.2459 g of glycine and 0.1180 g of carbohydrazide were added to the above mixed solution as organic fuel. Slowly evaporate in a water bath at 80°C until the mixed solution becomes a uniform and transparent sol. The above sol is put into a muffle furnace with a furnace temperature of 500° C. and ignited, and the combustion reaction is completed quickly within several tens of seconds to obtain a white fluffy product. Transfer the white product to an agate mortar, add 5mmol/L sodium hydroxide solution and grind thoroughly for 1h. After grinding the mixed slurry into distilled water and ultrasonic treatment for 1h, the mass ratio of distilled water to white product is 1000:1. After standing for 72h, take the supernatant and centrifuge at 10000rpm for 10min to obtain near infrared with average particle size less than 100nm Long afterglow luminescent nanoparticles. The atomic ratio composition of the near-infrared long afterglow luminescent nanoparticles is ZnGa 1.998 Cr 0.002 O 4.

[0047] Example 3

[0048] Add 10ml Zn(NO 3 ) 2 Solution, 19.9ml Ga(NO 3 ) 3 Solution, 0.2ml Cr(NO 3 ) 3 The solution is stirred to obtain the reactant nitrate mixture. Then, 0.2459 g of glycine and 0.1180 g of carbohydrazide were added to the above mixed solution as organic fuel. Slowly evaporate in a water bath at 80°C until the mixed solution becomes a uniform and transparent sol. The above-mentioned sol is put into a muffle furnace with a furnace temperature of 700° C. and ignited, and the combustion reaction is completed rapidly within tens of seconds, and a white fluffy product is obtained. Transfer the white product to an agate mortar, add 5mmol/L sodium hydroxide solution and grind thoroughly for 1h. After grinding the mixed slurry into distilled water and ultrasonic treatment for 1h, the mass ratio of distilled water to white product is 1000:1. After standing for 72h, take the supernatant and centrifuge at 10000rpm for 10min to obtain near infrared with average particle size less than 100nm Long afterglow luminescent nanoparticles. The atomic ratio composition of the near-infrared long afterglow luminescent nanoparticles is ZnGa 1.99 Cr 0.01 O 4.