A kind of core-shell nano-luminescent material and preparation method thereof
A nano-luminescent material and nano-material technology, applied in the field of core-shell nano-luminescent material and its preparation, can solve the problem of low imaging recognition rate of tumor cells
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Embodiment 1
[0040] Mix 2g NaOH, 7mL distilled water, 12mL ethanol, 20mL oleic acid, and 1.0g polyvinylpyrrolidone, stir magnetically to form a transparent solution, and add 0.0775g YbCl to the transparent solution 3 ·6H 2 O, 0.2367g YCl 3 ·6H 2 O and 0.00541 g ErCl 3 2mL rare earth mixed aqueous solution (mole fraction: 78%Y, 20%Yb, 2%Er), stir well. After stirring evenly, 5mL of 1mol / L NaF solution was added dropwise, stirred for 10min, transferred to a 50mL reactor, reacted at 180°C for 8h, and naturally cooled to room temperature in an oven. Take it out, dissolve and collect it with cyclohexane, add ethanol to precipitate the sample, centrifuge at 8000rpm / min for 10min, wash the obtained precipitate with ethanol and distilled water three times, and finally dry it in a vacuum oven at 90°C for 4h to obtain UCNPs. The topography images of large-particle core-shell nanoluminescent materials, small-particle core-shell nanoluminescent materials and rod-shaped core-shell nanoluminescent m...
Embodiment 2
[0045] Preparation of rare earth chloride aqueous solution. 2mL rare earth chloride (0.5mol / L LnCl 3 , Ln is 78%Y+20%Yb+2%Er (mol fraction)) aqueous solution is added in 20mL ethylene glycol, stir well, obtain solution A after 10 minutes. The specific weighing data is as follows: 0.0775g YbCl 3 ·6H 2 O, 0.2367g YCl 3 ·6H 2 O and 0.00541 g ErCl 3 (2) Configuration of NaF solution: Weigh 0.18900g NaF, add 4.5mL of water, and prepare a 1.0 mol / L aqueous solution. Add the compounded aqueous solution into 20mL of ethylene glycol, stir evenly, and obtain solution B after 10 minutes. (3) Mix A and B solutions. Pour solution B into solution A quickly, and stir the mixed solution rapidly with a glass plate for about 10 min. (4) After uniform stirring, the prepared solution was transferred to a 100mL reactor, sealed and placed in an oven at 200°C for 10 hours. (5) Take out the sample, wash, separate and dry. After the reaction, after the sample is naturally cooled, transfer th...
Embodiment 3
[0049] NaOH 1.2g, 9mL H 2 O, 10mL ethanol, 20mL oleic acid, 2.0g carboxymethyl cellulose to form a mixture; 0.6mmol (1.2mL, 0.5M) rare earth mixture was added under magnetic stirring. 1M 4mL NaF was added dropwise to the solution, mixed for 10min, transferred to a 50mL reactor at 160°C for 8h, and naturally cooled to room temperature with the sample at the bottom. Cyclohexane collected. Ethanol precipitation. After centrifugation, oleic acid and sodium oleate were washed with ethanol. Dry to obtain UCNPs.
[0050] Water-soluble UCNPs: Add 0.1g UCNPs to 100mL cyclohexane, 7mL tert-butanol, 10mL deionized water, 5wt% potassium carbonate, stir at room temperature for 20min, then add 20mL (0.01801g KMnO 4 +0.4492gNaIO 4 ) was stirred at 40°C for more than 48 h, and the obtained samples were separated by centrifugation and washed with acetone, ethanol, and deionized water. The sample was stirred in hydrochloric acid with pH=4-5 for 30min, centrifuged, washed with deionized wa...
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