Phase stable lead monoxide and process for the production thereof

• US 5,252,311 A
• Filed: 02/07/1992
• Issued: 10/12/1993
• Est. Priority Date: 04/20/1990
• Status: Expired due to Term

• Current Assignee: Rutgers University
• Original Assignee: Rutgers University
• Inventors: Munson, Michael J., Riman, Richard E.
• Primary Examiner(s): Straub, Gary P.
• Assistant Examiner(s): NGUYEN, NGOC YEN M
• Application Number:
  US07/833,565
• Time in Patent Office: 613 Days
• Field of Search: 423/619, 106/432, 252/25
• US Class Current: 423/619
• CPC Class Codes: C01G 21/06 Lead monoxide [PbO]
• CPC Class Codes: C01P 2002/02 Amorphous compounds
• CPC Class Codes: C01P 2002/72 by d-values or two theta-values, e.g. as X-ray diagram
• CPC Class Codes: C01P 2002/88 by thermal analysis data, e.g. TGA, DTA, DSC
• CPC Class Codes: C01P 2004/03 obtained by SEM
• CPC Class Codes: C01P 2004/20 extending in two dimensions, e.g. plate-like
• CPC Class Codes: C01P 2004/32 Spheres
• CPC Class Codes: C01P 2004/50 Agglomerated particles
• CPC Class Codes: C01P 2004/51 Particles with a specific particle size distribution
• CPC Class Codes: C01P 2004/61 Micrometer sized, i.e. from 1-100 micrometer
• CPC Class Codes: C01P 2004/62 Submicrometer sized, i.e. from 0.1-1 micrometer
• CPC Class Codes: C01P 2004/82 two phases having the same anion, e.g. both oxidic phases
• CPC Class Codes: C01P 2006/10 Solid density
• CPC Class Codes: C01P 2006/60 Optical properties, e.g. expressed in CIELAB-values
• CPC Class Codes: C10M 103/06 Metal compounds
• CPC Class Codes: C10M 2201/062 Oxides; Hydroxides; Carbonates or bicarbonates

Abstract

Phase stable lead monoxide powders are disclosed in which substantially pure free flowing PbO having a crystal phase which is homogeneous, and which phase may be selected from either the litharge or massicot forms, retains such phase homogeneity over extended periods under ambient storage conditions or even under the influence of ultraviolet light. Furthermore, lead monoxide powders and their oxalate precursors whose particles have a plate-like morphology and size which make them ideal for numerous applications are described. These and other compositions, as well as methods for making and utilizing these novel preparations, are included.

Claims

1. A phase homogeneous crystalline lead monoxide powder comprising substantially free flowing massicot lead monoxide having (i) a substantially plate-like morphology, and (ii) an average particle size of about 0.1 to about 10 microns in diameter as determined by photosedimentation methods, which lead monoxide retains its massicot crystalline form under ambient temperature, pressure and humidity conditions for a period of at least about 6 months as evidenced by the failure to detect any significant peaks attributable to the litharge crystalline form in the powder X-ray diffraction pattern obtained for a sample of said lead monoxide which had been stored under said conditions for said period, and which lead monoxide is chemically stable under the influence of constant exposure to ultraviolet radiation as evidenced by the substantial retention of the original color of a sample of said lead monoxide which had been exposed to a uv lamp for 3 months, said lead monoxide powder has been produced by heating lead oxalate having a plate-like morphology at a temperature ranging from about 400°

C. to about 600°

C. for a period of time sufficient to convert said lead oxalate to said lead monoxide.

2. The powder of claim 1 in which said lead monoxide contains a residual amount of carbon at a concentration of about 0.01 to about 0.5 percent by weight of said lead monoxide.

3. The powder of claim 1 in which said lead monoxide contains a residual amount of carbon at a concentration of about 0.1 percent by weight of said lead monoxide.

4. The powder of claim 1 in which said lead monoxide has a particle size ranging from about 1 to about 3 microns in diameter as determined by photosedimentation methods.

5. The powder of claim 1 in which said lead monoxide has an average particle size ranging from about 2 to about 3 microns in diameter as determined by photosedimentation methods.

6. A phase homogeneous crystalline lead monoxide powder comprising substantially pure free flowing massicot lead monoxide, which lead monoxide retains its massicot crystalline form under ambient temperature, pressure and humidity conditions for a period of at least about 24 months, or under continuous exposure to a source of ultraviolet radiation for a period of 3 months, as evidenced by the failure to detect any significant peaks attributable to the litharge crystalline form in the powder X-ray diffraction pattern obtained for a sample of said lead monoxide which had been stored under said ambient conditions for about 24 months, which lead monoxide can be further characterized as having a residual amount of carbon but is substantially free of heavy atom impurities and having a substantially plate-like morphology, an average particle size ranging from about 0.5 to about 5 microns in diameter as determined by photosedimentation methods, and containing a residual amount of carbon derived from an organic lead compound precursor, and which lead monoxide is chemically stable under the influence of constant exposure to ultraviolet radiation as evidenced by the substantial retention of the original color of a sample of said lead monoxide which had been exposed to a uv lamp for 3 months, said lead monoxide powder has been produced by heating lead oxalate having a plate-like morphology at a temperature ranging from about 400°

C. to about 600°

C. for a period of time sufficient to convert said lead oxalate to said lead monoxide.

7. A biphasic crystalline lead monoxide powder comprising substantially pure free flowing lead monoxide having (i) a substantially plate-like morphology, and (ii) an average particle size of about 0.1 to about 10 microns in diameter as determined by photosedimentation methods, the crystal phase of which is proportioned between preselected amounts of litharge and massicot, which proportion remains substantially unchanged under ambient temperature, pressure and humidity conditions for a period of at least about 6 months as evidenced by the failure to detect any significant change in the ratio of the height of the strongest peak attributable to the litharge crystalline form to the height of the strongest peak attributable to the massicot crystalline form in the powder X-ray diffraction pattern obtained for a sample of said biphasic lead monoxide, and which lead monoxide is chemically stable under the influence of constant exposure to ultraviolet radiation as evidenced by the substantial retention of the original color of a sample of said lead monoxide which had been exposed to a uv lamp for 3 months, said lead monoxide powder has been produced by heating lead oxalate having a plate-like morphology at a temperature ranging from about 400°

C. to about 600°

C. for a period of time sufficient to convert said lead oxalate to said lead monoxide.

8. The powder of claim 7 in which said lead monoxide contains a residual amount of carbon at a concentration of about 0.01 to about 0.5 percent by weight of said lead monoxide.

9. The powder of claim 7 in which said lead monoxide contains a residual amount of carbon at a concentration of about 0.1 percent by weight of said lead monoxide.

10. The powder of claim 7 in which the crystal phase of said lead monoxide is proportioned between about 2 to about 98 wt % litharge and about 98 to about 2 wt % massicot.

11. The powder of claim 7 in which the crystal phase of said lead monoxide is proportioned between about 30 to about 70 wt % litharge and about 70 to about 30 wt % massicot.

12. The powder of claim 7 in which the crystal phase of said lead monoxide is proportioned between about 50 wt % litharge and about 50 wt % massicot.

13. A crystalline lead monoxide powder comprising substantially pure free flowing lead monoxide having (i) a substantially plate-like morphology, and (ii) having an average particle size of about 0.1 to about 10 microns in diameter as determined by photosedimentation methods, effective to convey plasticity or workability to compositions comprising at least about 50 volume percent of said lead monoxide and up to about 50 volume percent of a suitable volatile liquid component, and which lead monoxide is chemically stable under the influence of constant exposure to ultraviolet radiation as evidenced by the substantial retention of the original color of a sample of said lead monoxide which had been exposed to a uv lamp for 3 months, said lead monoxide powder has been produced by heating lead oxalate having a plate-like morphology at a temperature ranging from about 400°

C. to about 600°

C. for a period of time sufficient to convert said lead oxalate to said lead monoxide.

14. The powder of claim 13 in which at least 10 percent by weight of said lead monoxide particles is colloidal.

15. The powder of claim 14 in which the particles that are colloidal have a particle size distribution ranging from about 0.1 to about 5 microns in diameter as determined by photosedimentation methods.

16. The powder of claim 13 in which the crystal phase of said lead monoxide is substantially homogeneous.

17. The powder of claim 16 in which said crystal phase is litharge.

18. The powder of claim 16 in which said crystal phase is massicot.

19. The powder of claim 13 in which the crystal phase of said lead monoxide is proportioned between litharge and massicot.

20. The powder of claim 13 in which the crystal phase of said lead monoxide is proportioned between about 10 to about 85 wt % litharge and about 90 to about 15 wt % massicot.

21. A lubricant comprising a sufficient amount of lead monoxide or a precursor thereof, which lead monoxide or precursor has (i) a substantially plate-like morphology, and (ii) an average particle size of about 0.5 to about 5 microns in diameter as determined by photosedimentation methods, and which lead monoxide is chemically stable under the influence of constant exposure to ultraviolet radiation as evidenced by the substantial retention of the original color of a sample of said lead monoxide which had been exposed to a uv lamp for 3 months, said lead monoxide powder has been produced by heating lead oxalate having a plate-like morphology at a temperature ranging from about 400°

C. to about 600°

C. for a period of time sufficient to convert said lead oxalate to said lead monoxide.

22. The lubricant of claim 21 in which said lead monoxide is substantially phase homogeneous.

23. The lubricant of claim 21 in which said lead monoxide is primarily in the litharge form.

24. The lubricant of claim 21 in which said lead monoxide is primarily in the massicot form.

25. The lubricant of claim 21 in which said lead monoxide is present as a mixture of the litharge and massicot forms.

26. The lubricant of claim 21 in which said lead monoxide has an average particle size of about 1 to about 3 microns in diameter as determined by photosedimentation methods.