Refractory NZP-type structures and method of making and...

Compositions: ceramic – Ceramic compositions – Titanate – zirconate – stannate – niobate – or tantalate or...

Reexamination Certificate

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C501S080000, C501S081000, C501S135000, C501S136000, C501S152000, C501S154000, C428S116000, C264S177120, C055S523000, C055SDIG003, C060S311000, C095S273000

Reexamination Certificate

active

06413895

ABSTRACT:

FIELD OF THE INVENTION
This invention relates to NZP type structures of high permeability suitable for use in filtration applications such as in diesel particulate filtration.
BACKGROUND OF THE INVENTION
Refractory NZP bodies are suitable for use in high temperature applications due to their high melting point and low coefficient of thermal expansion.
Present methods of making such bodies are disclosed in U.S. Pat. Nos. 4,675,302, 4,751,206, 4,801,566, 4,925,816, 5,102,836, 5,128,288, 5,254,510, and 5,488,018. Such bodies are expected to have low permeability due to low porosity or fine pore size; or in other cases, to have porosities and pore sizes so large that the bodies would be expected to exhibit poor filtration efficiency in removal of particles from a gas stream.
A need therefore exists to have low thermal expansion refractory NZP-type bodies with higher permeability than has been achieved up to now, while at the same time with useful filtration efficiency.
The present invention provides such a body and a method of making and using it.
SUMMARY OF THE INVENTION
In accordance with one aspect of the invention, there is provided a structure made predominately of an NZP-type phase having the general formula R
x
Z
4
P
6−y
Si
y
O
24
, where 0≦x≦8, 0≦y≦6, R is Li, Na, K, Rb, Cs, Mg, Ca, Sr, Ba, Y, and/or lanthanides, and Z is Zr, Ti, Nb, Ta, Y, and/or lanthanides, and optionally a sintering additive. The structure has an open porosity of at least 20% by volume, a median pore diameter in micrometers equal to or greater than a value defined by the quantity [10−0.10(% open porosity)], both as measured by mercury porosimetry, and four-point modulus of rupture as measured on a solid rod of circular cross section, of at least 300 psi.
In accordance with another aspect of the invention, there is provided a method of making the structure that involves forming a mixture of NZP-forming raw material powders that are metal oxide sources capable of reacting to form an NZP-type reaction product, and/or pre-reacted powder having the above general formula. The volumetric average of the median particle diameters of the raw material powders in the raw materials combination is at least 15 micrometers, and the particle diameters of at least 65% of the totality of the raw material particles are greater than 11 micrometers. The mixture is shaped into a green structure, and fired to produce the finished structure.
The structure is preferably multicellular, e.g. a honeycomb, and most preferably an alternately plugged honeycomb suitable for use as a diesel particulate filter.
In accordance with another aspect of the invention, there is provided a method of removing particulates from a fluid stream that involves passing the stream through an alternately plugged honeycomb to retain the particulates in the pores of the honeycomb.


REFERENCES:
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patent: 4675302 (1987-06-01), Roy et al.
patent: 4751206 (1988-06-01), Yamai et al
patent: 4781831 (1988-11-01), Goldsmith
patent: 4801566 (1989-01-01), Limaye et al.
patent: 4925816 (1990-05-01), Watanabe et al.
patent: 4968648 (1990-11-01), Watanabe et al.
patent: 5009781 (1991-04-01), Goldsmith
patent: 5102836 (1992-04-01), Brown et al.
patent: 5108601 (1992-04-01), Goldsmith
patent: 5128288 (1992-07-01), Ohashi et al.
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patent: 5217934 (1993-06-01), Matsuhiro et al.
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patent: 6238779 (2001-12-01), He et al.
C.Y. Huang, PhD thesis, Pennsylvania State University, May 1990, p. 9.
E. Breval and D. Agrawal, “Thermal expansion characteristics of [NZP], NaZr2P3012-type materials: a Review”, 1995 The Institute of Materials, pp.27-32.

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