IP Library › Granted Patent US 10,442,988
Granted Patent B2
US 10,442,988 · App. 14/946,140 · Granted Oct 15, 2019

Method for preparing water-dispersible quantum dots, colloid and a method for preparing the colloid

Inventors: Jakub Cichos (Olawa, PL); Miroslaw Karbowiak (Wroclaw, PL)
Assignee: UNIWERSYTET WROCLAWSKI
C09K11/562C09K11/025B82Y20/00B82Y40/00Y10S977/774Y10S977/892Y10S977/95
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Quick Facts
Patent No.
US 10,442,988
App. No.
14/946,140
Granted
Oct 15, 2019
Kind
B2
Abstract

The method for preparing water-dispersible core-shell quantum dots stabilized with a layer of hydrophilic surface ligands includes making a core of PbS nanocrystals, and obtaining the shell of CdS layer and the surface ligands of dithiocarbamates obtained by reacting amino acids with carbon disulphide, while maintaining the photoluminescence. The emulsion formed of an aqueous solution of amino acid and carbon disulphide includes adding a solution of PbS/CdS in chloroform (CHCl 3 ). Then, the contents are stirred vigorously for at least 20 hours, then the phases are separated. The upper, aqueous phase, being a solution of PbS/CdS/DTC-amino acid residue, is subjected to purification. The present invention is also colloid and a method for preparing colloid.

Claims (31)

1. A method for preparing water-dispersible core-shell quantum dots stabilized with a layer of hydrophilic surface ligands, the method comprising the steps of:

making a core of PbS nanocrystals; and

reacting amino acids with carbon disulphide so as to obtain a shell of CdS layer and surface ligands comprised of dithiocarbamates and so as to maintain photoluminescence,

wherein the step of reacting amino acids comprises the steps of:

adding a solution of PbS/CdS in chloroform to an emulsion of an aqueous solution of amino acid and carbon disulphide so as to form a mixture;

stirring said mixture vigorously for at least 20 hours so as to form a stirred mixture;

separating said stirred mixture into phases, wherein at least one phase is comprised of an upper aqueous phase, said upper aqueous phase being comprised of a solution of PbS/CdS/DTC-amino acid residue; and

purifying said solution of PbS/CdS/DTC-amino acid residue.

2. The method for preparing water-dispersible core-shell quantum dots, according to claim 1 , wherein said amino acids are comprised of at least one of lysine, valine, proline, glycine, arginine, alanine, and beta-alanine.

3. The method for preparing water-dispersible core-shell quantum dots, according to claim 1 , wherein the step of reacting amino acids further comprises the step of:

mixing stoichiometric amounts of amino acids in carbon disulphide, wherein maximum concentration of amino acids is limited by solubility in water.

4. The method for preparing water-dispersible core-shell quantum dots, according to claim 1 , wherein at least one phase is comprised of an emulsion phase, said emulsion phase being comprised of dithiocarbamate.

5. The method for preparing water-dispersible core-shell quantum dots, according to claim 1 , wherein said solution of PbS/CdS in chloroform has a concentration ranging from 0 to 100 mg/cm3.

6. The method for preparing water-dispersible core-shell quantum dots, according to claim 1 , wherein a volume ratio of said solution of PbS/CdS in chloroform to said emulsion has a range of from 1:10 to 10:1.

7. The method for preparing water-dispersible core-shell quantum dots, according to claim 1 , wherein the step of purifying said solution of PbS/CdS/DTC-amino acid residue comprises the steps of:

centrifuging said solution of PbS/CdS/DTC-amino acid residue;

adding acetone so as to form a clouded solution with a first cloudiness;

centrifuging said clouded solution so as to form a centrifuged precipitate;

dissolving said centrifuged precipitate in a minimum amount of water so as to form a dissolved precipitate solution; and

adding acetone to said dissolved precipitate solution so as to form a dispersed colloid solution.

8. The method for preparing water-dispersible core-shell quantum dots, according to claim 7 , further comprising the steps of:

washing said centrifuged precipitate with acetone, after the step of re-centrifuging said clouded solution, so as to form a washed precipitate,

wherein the step of dissolving said centrifuged precipitate is comprised of dispersing said washed precipitate as said centrifuged precipitate in distilled water so as to obtain said dissolved precipitate solution.

9. The method for preparing water-dispersible core-shell quantum dots, according to claim 1 , wherein said solution of PbS/CdS/DTC-amino acid residue is comprised of particles sized from 4 to 20 nm.

10. A The method for preparing water-dispersible core-shell quantum dots, according to claim 1 , wherein the step of purifying said solution of PbS/CdS/DTC-amino acid residue is comprised of the steps of:

adding an excess of a solution of a quaternary ammonium salt to said solution of the PbS/CdS-DTC-amino acid residue so as to form a mixed solution;

stirring said mixed solution at room temperature for 24 hours so as to form a stirred solution;

centrifuging said stirred solution so as to separate quantum dots from said PbS/CdS-DTC-amino acid residue;

washing said quantum dots with distilled water; and

dispersing said quantum dots in a phosphate buffer at pH 7.4 so as to obtain a colloidal solution of quantum dots in a PBS buffer.

11. The method for preparing water-dispersible core-shell quantum dots, according to claim 10 , wherein said quaternary ammonium salt is comprised of diallyl-dimethyl-ammonium polyhydroxide.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 30, 2015
From: CICHOS, JAKUB; KARBOWIAK, MIROSLAW
To: UNIWERSYTET WROCLAWSKI
Reel/Frame 037172/0386 →
Priority Claims (1)
PL PL413504 · Aug 11, 2015 · national
Continuity (1)
Related Publication 20170044430A1 · Feb 16, 2017