IP Library Granted Patent US 12,465,907
Granted Patent B1
US 12,465,907 · App. 19/039,906 · Granted Nov 11, 2025

Fabrication of PbO/Co

Inventor: Ehab Abdelhamed Abdelrahman Ahmed (Riyadh, SA)
Assignee: IMAM MOHAMMAD IBN SAUD ISLAMIC UNIVERSITY
B01J23/835B01J23/75B01J35/19B01J35/393B01J35/45B01J35/51B01J35/55B01J37/04B01J37/08B01J37/12
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Quick Facts
Patent No.
US 12,465,907
App. No.
19/039,906
Granted
Nov 11, 2025
Kind
B1
Abstract

A PbO/Co 3 O 4 /MgO nanocomposite material includes an orthorhombic PbO crystalline phase, a cubic Co 3 O 4 crystalline phase, and a cubic MgO crystalline phase. The average crystallite size of the PbO/Co 3 O 4 /MgO nanocomposite material is in a range from 75 to 90 nm.

Claims (33)

1 . A PbO/Co 3 O 4 /MgO nanocomposite material comprising:

an orthorhombic PbO crystalline phase;

a cubic Co 3 O 4 crystalline phase; and

a cubic MgO crystalline phase,

wherein an average crystallite size of the PbO/Co 3 O 4 /MgO nanocomposite material is in a range from 75 to 90 nm.

2 . The PbO/Co 3 O 4 /MgO nanocomposite material of claim 1 , wherein the average crystallite size of the PbO/Co 3 O 4 /MgO nanocomposite material is in a range from 78 to 85 nm.

3 . The PbO/Co 3 O 4 /MgO nanocomposite material of claim 2 , wherein the average crystallite size of the PbO/Co 3 O 4 /MgO nanocomposite material is in a range from 81 to 83 nm.

4 . The PbO/Co 3 O 4 /MgO nanocomposite material of claim 1 , wherein the atomic concentration of lead in the PbO/Co 3 O 4 /MgO nanocomposite material is in a range from 8 to 15 at. %, the atomic concentration of cobalt in the PbO/Co 3 O 4 /MgO nanocomposite material is in a range from 15 to 25 at. %, and the atomic concentration of magnesium in the PbO/Co 3 O 4 /MgO nanocomposite material is in a range from 14 to 22 at. %.

5 . The PbO/Co 3 O 4 /MgO nanocomposite material of claim 4 , wherein the atomic concentration of lead in the PbO/Co 3 O 4 /MgO nanocomposite material is in a range from 10 to 13 at. %, the atomic concentration of cobalt in the PbO/Co 3 O 4 /MgO nanocomposite material is in a range from 18 to 22 at. %, and the atomic concentration of magnesium in the PbO/Co 3 O 4 /MgO nanocomposite material is in a range from 16 to 20 at. %.

6 . The PbO/Co 3 O 4 /MgO nanocomposite material of claim 5 , wherein the atomic concentration of lead in the PbO/Co 3 O 4 /MgO nanocomposite material is in a range from 11 to 12 at. %, the atomic concentration of cobalt in the PbO/Co 3 O 4 /MgO nanocomposite material is in a range from 19 to 21 at. %, and the atomic concentration of magnesium in the PbO/Co 3 O 4 /MgO nanocomposite material is in a range from 17 to 18.5 at. %.

7 . The PbO/Co 3 O 4 /MgO nanocomposite material of claim 1 , wherein the atomic concentration of oxygen in the PbO/Co 3 O 4 /MgO nanocomposite material is in a range from 40 to 60 at. %.

8 . The PbO/Co 3 O 4 /MgO nanocomposite material of claim 1 , wherein the PbO/Co 3 O 4 /MgO nanocomposite material comprises a heterogenous structure comprising:

rod-like particles with an average length in a range from 0.5 to 10 μm and an average diameter in a range from 0.25 to 4 μm; and

agglomerations of spherical particles wherein the spherical particles have an average diameter in a range from 10 to 300 nm.

9 . The PbO/Co 3 O 4 /MgO nanocomposite material of claim 8 , wherein the PbO/Co 3 O 4 /MgO nanocomposite material comprises a heterogenous structure comprising:

rod-like particles with an average length in a range from 1 to 5 μm and an average diameter in a range from 0.25 to 2.0 μm; and

agglomerations of spherical particles wherein the spherical particles have an average diameter in a range from 25 to 200 nm.

10 . The PbO/Co 3 O 4 /MgO nanocomposite material of claim 9 , wherein the PbO/Co 3 O 4 /MgO nanocomposite material comprises a heterogenous structure comprising:

rod-like particles with an average length in a range from 1 to 3 μm and an average diameter in a range from 0.5 to 1.5 μm; and

agglomerations of spherical particles wherein the spherical particles have an average diameter in a range from 25 to 100 nm.

11 . A method for making the PbO/Co 3 O 4 /MgO nanocomposite material of claim 1 , comprising:

adding a tartaric acid solution to a solution of magnesium nitrate hexahydrate (Mg(NO 3 ) 2 ·6H 2 O), cobalt acetate tetrahydrate (Co(CH 3 COO) 2 ·4H 2 O), and lead nitrate (Pb(NO 3 ) 2 ) under stirring to form a reaction mixture;

adding polyethylene glycol 400 to the reaction mixture to form a stabilized mixture and stirring at 250° C. until complete evaporation of water, forming a solid; and

calcining the solid at a temperature in a range from 550 to 650° C. for 2 to 4 hours to form the PbO/Co 3 O 4 /MgO nanocomposite material.

12 . The method of claim 11 , wherein the solid is calcined at a temperature in a range from 575 to 625° C. for 2 to 4 hours to form the PbO/Co 3 O 4 /MgO nanocomposite material.

13 . The method of claim 11 , wherein the solid is calcined at 600° C. for 3 hours to form the PbO/Co 3 O 4 /MgO nanocomposite material.

14 . The method of claim 11 , wherein the concentration of tartaric acid in the reaction mixture is in a range from 120 to 140 g/L.

15 . The method of claim 11 , wherein the concentration of Mg(NO 3 ) 2 ·6H 2 O in the reaction mixture is in a range from 75 to 85 g/L.

16 . The method of claim 11 , wherein the concentration of Co(CH 3 COO) 2 ·4H 2 O in the reaction mixture is in a range from 75 to 85 g/L.

17 . The method of claim 11 , wherein the concentration of Pb(NO 3 ) 2 in the reaction mixture is in a range from 75 to 85 g/L.

18 . The method of claim 11 , wherein the concentration of tartaric acid in the reaction mixture is in a range from 130 to 135 g/L, the concentration of Mg(NO 3 ) 2 ·6H 2 O in the reaction mixture is in a range from 79 to 81 g/L, the concentration of Co(CH 3 COO) 2 ·4H 2 O in the reaction mixture is in a range from 79 to 81 g/L, and the concentration of Pb(NO 3 ) 2 in the reaction mixture is in a range from 79 to 81 g/L.

19 . The method of claim 11 , wherein the concentration of polyethylene glycol 400 in the stabilized mixture is in a range from 50 to 60 ml per liter of stabilized solution.

20 . The method of claim 11 , wherein the concentration of polyethylene glycol 400 in the stabilized mixture is in a range from 55 to 58 ml per liter of stabilized mixture.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 29, 2025
From: AHMED, EHAB ABDELHAMED ABDELRAHMAN
To: IMAM MOHAMMAD IBN SAUD ISLAMIC UNIVERSITY
Reel/Frame 070042/0644 →
References Cited (5)
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EP 071485081 · 1999 [cited by applicant]
Mosab Kaseema. et al., “Electrochemical response of MgO/Co3O4 oxide layers produced by plasma electrolytic oxidation and post treatment using cobalt nitrate”, Journal of Magnesium and Alloys, vol. 11, Issue 3, Mar. 2023… [cited by applicant]
Grigory B. Veselov, et al., “Sol-gel prepared Co—Mg—O oxide systems: redox behavior, thermal stability and catalytic performance in CO oxidation”, Reaction Kinetics, Mechanisms and Catalysis, vol. 136, 2023, p. 233-250,… [cited by applicant]