IP Library Granted Patent US 9,073,761
Granted Patent B2
US 9,073,761 · App. 14/203,900 · Granted Jul 7, 2015

Controlled synthesis of nanoparticles using ultrasound in continuous flow

Inventors: Barath Palanisamy (Corvallis, OR); Brian K. Paul (Corvallis, OR); Ravindranadh Tagore Eluri (Corvallis, OR)
Assignee: THE STATE OF OREGON ACTING BY AND THROUGH THE STATE BOARD OF HIGHER EDUCATION, OREGON STATE UNIVERSITY
C01G11/02B06B3/00Y10S977/896Y10S977/773B82Y40/00B82Y30/00
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Quick Facts
Patent No.
US 9,073,761
App. No.
14/203,900
Granted
Jul 7, 2015
Kind
B2
Abstract

Apparatuses and methods for synthesizing nanoparticles are provided. Methods for synthesizing nanoparticles are provided comprising mixing at least two solutions comprising the components of the nanoparticles within a micromixer; exposing the resultant mixed, unreacted, azeotropic solution to ultrasound; and collecting the generated nanoparticles. Apparatuses are also provided for synthesizing nanoparticles comprising a micromixer in fluid connection with a continuous reactor comprising at least one inlet, at least one outlet, and an ultrasound horn oriented such that the acoustic energy is transferred to the fluid within the continuous reactor.

Claims (35)

1. A method for synthesizing nanoparticles, said method comprising:

a) mixing at least two solutions comprising the components of the nanoparticles within a micromixer, wherein the resultant mixed solution is azeotropic;

b) exposing the mixed, unreacted solution from step a) to ultrasound; and

c) collecting the nanoparticles generated from step b).

2. The method of claim 1 , wherein said nanoparticles are cadmium sulfide nanoparticles.

3. The method of claim 1 , wherein said micromixer comprises at least two inlets and an outlet, wherein said inlets direct fluid streams into a confined mixing region.

4. The method of claim 3 , wherein said micromixer is a T-mixer.

5. The method of claim 1 , wherein said method further comprises quenching the nanoparticles generated in step b).

6. The method of claim 1 , wherein said ultrasound has an average power of about 10 W to 200W and a frequency of about 10 kHz to about 100 kHz.

7. The method of claim 1 , wherein the fluid residence time in the exposure to ultrasound in step b) is less than about three minutes.

8. The method of claim 7 , wherein the fluid residence time in the exposure to ultrasound in step b) is about 30 seconds to about 60 seconds.

9. The method of claim 1 , wherein the mixed, unreacted solution from step a) is exposed to ultrasound within a continuous reactor, wherein said continuous reactor comprises at least one inlet, at least one outlet, and an ultrasound horn, wherein said ultrasound horn is oriented such that the tip of the ultrasound horn is in contact with the mixed, unreacted solution.

10. The method of claim 9 , wherein the internal volume of the continuous reactor is less than about 10 ml.

11. The method of claim 9 , wherein the depth of the fluid in front of the tip of the ultrasound horn is less than about 5 mm.

12. The method of claim 9 , further comprising a cooling system around the continuous reactor.

13. The method of claim 1 , wherein the mixed, unreacted solution from step a) is exposed to ultrasound within tubing comprising a conical portion, wherein an ultrasound horn is oriented such that the tip of the ultrasound horn is within the conical portion of the tubing.

14. The method of claim 13 , wherein said conical portion of tubing and said ultrasound horn tip are submerged in a cooling system.

15. An apparatus for synthesizing nanoparticles of binary compounds, said apparatus comprising a micromixer in fluid connection with a continuous reactor, wherein the continuous reactor comprises at least one inlet, at least one outlet, and an ultrasound horn oriented such that the acoustic energy is transferred to the fluid within the continuous reactor.

16. The apparatus of claim 15 further comprising at least one of the following:

a) a control unit for regulating the ultrasound horn of the continuous reactor;

b) a pump in fluid connection with the mixer and, optionally, in fluid connection with reservoirs or vessels comprising the solutions for formation of the nanoparticles;

c) a vessel or reservoir in fluid connection with the outlet of the continuous reactor; and

d) a cooling system.

17. The apparatus of claim 15 , wherein the internal volume of the continuous reactor is less than about 10 ml.

18. The apparatus of claim 15 , wherein the depth of the fluid in front of the tip of the ultrasound horn is less than about 5 mm.

19. An apparatus for synthesizing nanoparticles of binary compounds, said apparatus comprising:

1) a micromixer in fluid connection with tubing comprising a conical shape; and

2) an ultrasound horn oriented with the horn tip within the conical shape portion of the tubing, and wherein the conical portion of the tubing and the ultrasound horn tip are submerged in a liquid cooling system.

20. The apparatus of claim 19 further comprising at least one of the following:

a) a control unit for regulating the ultrasound horn of the continuous reactor;

b) a pump in fluid connection with the mixer and, optionally, in fluid connection with reservoirs or vessels comprising the solutions for formation of the nanoparticles; and

c) a receiving vessel or reservoir in fluid connection with the tubing.

21. The method of claim 1 , wherein said nanoparticles comprise binary compounds.

22. The method of claim 21 , wherein said binary compounds are chalcogenides.

23. The method of claim 22 , wherein said chalcogenides are selected from the group consisting of CdS, PdS, CdSe, InSe, ZnS, ZnSe, CdTe, PbSe, SnS, SnTe, ZnO, Bi 2 Te 3 , CeO 2 , SiO 2 , and TiO 2 .

Assignments (2)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 30, 2014
From: PALANISAMY, BARATH; PAUL, BRIAN K; ELURI, RAVINDRANADH TAGORE
To: THE STATE OF OREGON ACTING BY AND THROUGH THE STATE BOARD OF HIGHER EDUCATION, OREGON STATE UNIVERSITY
Reel/Frame 032997/0866 →
CONFIRMATORY LICENSE Recorded May 1, 2014
From: OREGON STATE UNIVERSTIY
To: U.S. DEPARTMENT OF ENERGY
Reel/Frame 032801/0530 →
Continuity (2)
Provisional Application 61776232 · Mar 11, 2013
Related Publication 20140255293A1 · Sep 11, 2014