Lanthanum based upconverting microrods and application thereof

Patent metadata

Field	Value
Publication number	US-11078415-B2
Application number	US-201716072104-A
Country	US
Kind code	B2
Filing date	Jan 20, 2017
Priority date	Jan 22, 2016
Publication date	Aug 3, 2021
Grant date	Aug 3, 2021

Abstract

The present invention provides a monodispersed lanthanum based upconverting microrods comprising β-NaYF 4 :Yb 3+ , Er 3+ and β-NaYF 4 :Yb 3+ , Tm 3+ , capped with oleic acid. The upconverting microrods, embedded in polymer matrices is used for making security tags and for sensing application. The process of preparation of the oleic acid capped upconverting microrods is also disclosed.

First claim

We claim:

1. A monodispersed lanthanum based upconverting microrods selected from β-NaYF 4 :Yb 3+ , Er 3+ and β-NaYF 4 :Yb 3+ , Tm 3+ , capped with an organic ligand consisting of oleic acid, for making security tags and for sensing applications,
wherein the β-NaYF 4 :Yb 3+ , Er 3+ comprises β-NaYF 4 :Yb 3+ and Er 3+ but not Gd 3+ and has an aspect ratio in the range of 6 to 12, or wherein the β-NaYF 4 :Yb 3+ , Tm′ comprises β-NaYF 4 :Yb 3+ and Tm 3+ but not Gd 3+ and has an aspect ratio in the range of 3 to 7, and
wherein the microrods selected from β-NaYF 4 :Yb 3+ , Er 3+ and β-NaYF 4 :Yb 3+ , Tm 3+ have a length of 120.257 nm and 418.1457 nm respectively, and a width of 12.5412 nm and 83.9962 nm respectively.

2. A process for the preparation of monodispersed lanthanum based upconverting microrods selected from β-NaYF 4 :Yb 3+ , Er 3+ and β-NaYF 4 :Yb 3+ , Tm 3+ , capped with an organic ligand consisting of oleic acid, for making security tags and for sensing applications, where the β-NaYF 4 :Yb 3+ , Er 3+ comprises β-NaYF 4 :Yb 3+ and Er 3+ but not Gd 3+ and has an aspect ratio in the range of 6 to 12, or wherein the β-NaYF 4 :Yb 3+ , Tm 3+ comprises β-NaYF 4 :Yb 3+ and Tm 3+ but not Gd 3+ and has an aspect ratio in the range of 3 to 7 the process comprising the steps of:
a. mixing oleic acid, sodium hydroxide, absolute ethanol and water;
b. adding a solution containing a mixture of lanthanum compounds and sodium fluoride to a reaction mixture of step (a);
c. refluxing the reaction mixture of step (b) for a period in the range of 4 to 6 hrs at a temperature in the range of 160 to 180° C. and allowed to cool at room temperature; and
d. heating the reaction mixture of step (c) for a period in the range of 50 to 60 hrs at a temperature in the range of 180 to 195° C., under nitrogen atmosphere, followed by drying to afford the oleate-capped lanthanum based upconverting microrods.

3. The process as claimed in claim 2 , wherein the mixture of the lanthanum compounds of step (b) contains Yttrium(III) chloride hexahydrate (YCl 3 .6H 2 O), Ytterbium(III) Chloride Hexahydrate (YbCl 3 .6H 2 O) and Erbium(III) chloride hexahydrate (ErCl 3 .6H 2 O).

4. The process as claimed in claim 2 , wherein the oleate-capped lanthanum based upconverting microrods are embedded in polymer matrices for making security tags that respond to different wavelengths and for sensing applications.

5. The process as claimed in claim 4 , wherein the polymer matrices are selected from polydimethylsiloxane (PDMS), Ethylene propylene diene monomer (EPDM), Polyethylene oxide (PEO), Polystyrene (PS) and a natural silk scaffold.

Assignees

• Council Scient Ind Res

Inventors

• Nithyanandhan Jayaraj
• Shanmuganathan Kadhiravan
• Ananthan Alagumalai

Classifications

• C01P2004/04

  obtained by TEM, STEM, STM or AFM · CPC title

• C01P2002/72

  by d-values or two theta-values, e.g. as X-ray diagram · CPC title

• C01P2004/62

  Submicrometer sized, i.e. from 0.1-1 micrometer · CPC title

• C09K11/7773 Primary

  with alkali or alkaline earth metal · CPC title

• C01F17/36

  halogen being the only anion, e.g. NaYF4 · CPC title