Process for the preparation of uniform sized phosphor aerogel

Patent metadata

Field	Value
Publication number	US-10633257-B2
Application number	US-201715612540-A
Country	US
Kind code	B2
Filing date	Jun 2, 2017
Priority date	Jun 6, 2016
Publication date	Apr 28, 2020
Grant date	Apr 28, 2020

Abstract

The present invention provides a process for the preparation of phosphor aerogel of uniform size having high porosity, low density; high thermal insulation and high luminescence, which is useful for various applications like lighting, display, sensing and other applications. More specifically, the present invention provides a simple and versatile process for the formation of monolithic gel, at room temperature, which on further drying at supercritical temperature and pressure result in dry aerogel.

First claim

We claim:

1. A process for the preparation of a uniformly sized phosphor aerogel comprising:
(a) dissolving an alkoxide, a transition metal salt and/or alkaline earth metal salt, a dopant, a polar solvent, and demineralized water in molar ratio ranging from 1: 1-2:1-20: 5-10: 4-10 to obtain a clear transparent solution that forms a wet gel within 30 min to 5 hours, and optionally forming the gel into a desired shape or size;
(b) subjecting the wet gel obtained in step (a) to supercritical drying in an autoclave for 5-6 hours at a temperature ranging from 250° C. to 300° C. at 60-120 bars pressure to obtain a dried aerogel followed by flushing with nitrogen gas 2-3 times to remove adsorbed solvent molecules from the pores of the dried aerogel;
(c) subjecting the dried aerogel as obtained in step (b) to an annealing treatment in a controlled atmosphere of a high temperature furnace at a temperature in the range of 800° C. to 1500° C. for 1-5 hours so as to obtain the desired phosphor aerogel.

2. The process as claimed in claim 1 , wherein the molar ratio of alkoxide, transition metal salt and/or alkaline earth metal salt, dopant, polar solvent and demineralized water is 1:1-2:1-20:10:4.

3. The process as claimed in claim 1 , wherein the said process yields a phosphor aerogel that emits a color selected from the group consisting of violet, indigo, blue, green, yellow, orange and red.

4. The process as claimed in claim 1 , wherein the polar solvent is selected from the group consisting of methanol, ethanol, isopropyl alcohol, acetone and demineralized water.

5. The process as claimed in claim 1 , wherein the transition metal and/or alkaline earth metal is selected from the group consisting of zinc, cadmium, nickel, beryllium, magnesium, calcium, strontium and barium.

6. The process as claimed in claim 1 , wherein the dopant is a soluble salt of transition metal and/or rare-earth metal selected from the group consisting of manganese, copper, silver, cobalt, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium and ytterbium.

7. The process as claimed in claim 1 , wherein the dopant's concentration is 1-20 molar parts to 1-2 molar parts of a precursor salt that is a transition metal or alkaline earth metal salt selected from the group consisting of zinc, cadmium, nickel, beryllium, magnesium, calcium, strontium and barium.

8. The process as claimed in claim 1 , wherein the wet gel is autoclaved at a temperature from 250° C. to 300° C. for 5-6 hours and a pressure of from 60 to 120 bars.

9. The process as claimed in claim 1 , wherein the aerogel is annealed under a controlled atmosphere at a temperature ranging from 800° C. to 1500° C. in a high temperature furnace for 1 to 5 hours.

10. A phosphor aerogel obtained by the process as claimed in claim 1 , having a particle size of 5-25 nm within a ±2 nm size distribution, a high porosity of >90% and a low density of <100 kg m −3 , and exhibiting thermal insulating properties, wherein the phosphor aerogel emits a color in the visible and/or near infrared range from 400-1500 nm when excited by ultraviolet light having a wavelength in the range of 200 to 400 nm.

11. The phosphor aerogel as claimed in claim 10 , wherein the phosphor aerogel is in the form of a powder or is in the form of a shape selected from the group consisting of a square, rectangular, cylindrical and circular shape.

Assignees

• Council Scient Ind Res

Inventors

• Divi Haranath
• Singh Nahar
• Chawla Sneha

Classifications

• C09K11/595

  with zinc or cadmium · CPC title

• C01B25/36

  Aluminium phosphates · CPC title

• C01B33/1585 Primary

  Dehydration into aerogels · CPC title

• C01B25/265

  General methods for obtaining phosphates · CPC title

• C01B25/372

  of titanium, vanadium, zirconium, niobium, hafnium or tantalum · CPC title