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US 6,620,752 B2Granted
Method for fabrication of lead-based perovskite materials
AssigneeThe Penn State Research Foundation
InventorsGary L. Messing, Songtae Kwon, Edward M. Sabolsky
Life of this patent
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Abstract
The disclosed invention relates to PMN compounds, powders and products thereof, especially to PMN-PT compounds, powders and products which have the perovskite structure. The PMN-PT compounds are characterized by the formula (1−x)Pb(Mg1/3Nb2/3)O3−xPbTiO3 where x is about 0.0 to about 0.95, preferably x is about 0.0 to about 0.40. The compounds are made by sintering a precursor powder of the compound. PMN-PT products produced from the precursor powders have much greater densities than products produced from PMN-PT starting powder. The invention also relates to textured PMN-PT produced from the precursor powders.
Claims34
A process for preparing (1−x)Pb(Mg1/3Nb2/3)O3−xPbTiO3 where x=0.35 comprising,
- mixing (PbCO3)2Pb(OH)2 of a particle size less than about 6 μm, MgNb2O6 having a specific surface area of more than about 5 m2/g and fumed TiO2 having a specific surface area of more than about 30 m2/g to form a mixture,
- the (PbCO3)2Pb(OH)2, the fumed TiO2, and the MgNb2O6 present in amounts sufficient to produce a ratio of (PbCO3)2Pb(OH)2:MgNb2O6:fumed TiO2 of about 1:0.24:0.1 to about 1:0.0.27:0.12,
- milling the mixture in distilled water to produce a slurry having particle size of less than about 3 μm,
- heat treating the slurry to produce a dried precursor powder,
- grinding the dried precursor powder to a size less than about 200 μm, and
- sintering the dried precursor powder to a temperature of about 900° C. to about 1300° C. in an atmosphere selected from the group consisting of oxygen, nitrogen and air to produce a ceramic of (1−x)Pb(Mg1/3Nb2/3)O3−xPbTiO3 where x=0.35.
3 more elements
A process for preparing (1−x)Pb(Mg1/3Nb2/3)O3−xPbTiO3 where x=0.35 comprising,
- mixing (PbCO3)2Pb(OH)2 of a particle size less than about 4 μm, MgNb2O6 having a specific surface area of more than about 7.5 m2/g and fumed TiO2 having a specific surface area of more than about 50 m2/g to form a mixture,
- the (PbCO3)2Pb(OH)2, the fumed TiO2, and the MgNb2O6 present in amounts sufficient to produce a ratio of (PbCO3)2Pb(OH)2:MgNb2O6:fumed TiO2 of about 1:0.256:0.109,
- milling said mixture in distilled water to produce a slurry having particle size of less than about 1 μm,
- heat treating the slurry to produce a dried precursor powder,
- grinding the dried precursor powder to produce a ground dried precursor powder of less than about 90 μm, and
- sintering the dried precursor powder to about 1000° C. to about 1150° C. in oxygen to produce a ceramic product of (1−x)Pb(Mg1/3Nb2/3)O3−xPbTiO3 where x=0.35.
3 more elements
A process for preparing (1−x)Pb(Mg1/3Nb2/3)O3−xPbTiO3 where x=0.35 comprising,
- mixing (PbCO3)2Pb(OH)2 of a particle size less than about 4 μm, MgNb2O6 having a specific surface area of more than about 7.5 m2/g and fumed TiO2 having a specific surface area of more than about 50 m2/g to form a mixture,
- the (PbCO3)2Pb(OH)2, the fumed TiO2, and the MgNb2O6 present in amounts sufficient to produce a ratio of (PbCO3)2Pb(OH)2:MgNb2O6:fumed TiO2 of about 1:0.256:0.109,
- milling said mixture in distilled water to produce a slurry having particle size of less than about 1 μm,
- heat treating the slurry to produce a dried precursor powder,
- grinding the dried precursor powder to produce a ground dried precursor powder of less than about 90 μm, and
- sintering the dried precursor powder to about 1000° C. to about 1150° C. in oxygen and then in nitrogen to produce a ceramic product of (1−x)Pb(Mg1/3Nb2/3)O3−xPbTiO3 where x=0.35.
3 more elements
A process for preparing (1−x)Pb(Mg1/3Nb2/3)O3−xPbTiO3 where x=0.35 comprising,
- mixing (PbCO3)2Pb(OH)2 of a particle size less than about 6 μm, MgNb2O6 having a specific surface area of more than about 5 m2/g and fumed TiO2 having a specific surface area of more than about 30 m2/g to form a mixture,
- the (PbCO3)2Pb(OH)2, the fumed TiO2, and the MgNb2O6 present in amounts sufficient to produce a ratio of (PbCO3)2Pb(OH)2:MgNb2O6:fumed TiO2 of about 1:0.24:0.1 to about 1:0.0.27:0.12,
- milling the mixture in distilled water to produce a slurry having particle size of less than about 3 μm,
- heat treating the slurry to produce a dried precursor powder,
- grinding the dried precursor powder to produce a ground dried precursor powder of a size less than about 200 μm,
- compressing the ground dried precursor powder to produce a green preform,
- placing the green preform in an embedding powder which can generate lead oxide during sintering of the green preform, and
- sintering the green preform to a temperature of about 900° C. to about 1300 ° C. in an atmosphere selected from the group consisting of oxygen, nitrogen and air to produce a ceramic of (1−x)Pb(Mg1/3Nb2/3)O3−xPbTiO3 where x=0.35.
5 more elements
A process of manufacture of a single crystal of 0.65PMN-0.35PT comprising,
- mixing (PbCO3)2Pb(OH)2 of a particle size less than about 6 μm, MgNb2O6 having a specific surface area of more than about 5 m2/g and fumed TiO2 having a specific surface area of more than about 30 m2/g to form a mixture,
- the (PbCO3)2Pb(OH)2, the fumed TiO2, and the MgNb2O6 present in amounts sufficient to produce a ratio of (PbCO3)2Pb(OH)2:MgNb2O6:fumed TiO2 of about 1:0.24:0.1 to about 1:0.0.27:0.12,
- milling said mixture in distilled water to produce a slurry having particle size of less than about 3 μm,
- heat treating the slurry to produce a dried precursor powder,
- grinding the dried precursor powder to produce a ground dried precursor powder of a size less than about 200 μm,
- compressing the dried ground powder to produce a compressed preform,
- placing a barium titanate single crystal on the compressed preform,
- depositing an additional amount of the ground dried precursor powder over the barium titanate single crystal,
- compressing the preform having the dried precursor powder and barium titanate single crystal thereon to produce a compact, and
- sintering the compact to produce a single crystal of 0.65PMN-0.35PT.
7 more elements
A process for preparing a lead magnesium niobate-lead titanate product comprising,
- mixing a blend including a lead-containing substance selected from the group consisting of lead acetates-lead hydroxides, lead acetates, lead hydroxides and lead carbonates with magnesium niobate and fumed titanium oxide to form a mixture,
- milling the mixture to produce a blend having particle size of less than about 3 μm,
- heat treating the blend to produce a dried precursor powder, and
- sintering the dried precursor powder to a temperature of about 900° C. to about 1300° C. to produce a lead magnesium niobate-lead titanate compound.
1 more element
A process of manufacture of textured 0.675PMN-0.325PT ceramic comprising,
- mixing (PbCO3)2Pb(OH)2 of a particle size less than about 4 μm, MgNb2O6 having a specific surface area of more than about 7.5 m2/g and fumed TiO2 having a specific surface area of more than about 50 m2/g to form a blend,
- milling the blend in water to produce a mixture,
- drying the mixture to produce a dried precursor powder,
- grinding the dried precursor powder to produce a ground precursor powder of a size less than about 90 μm,
- mixing the ground precursor powder with an organic liquid, an organic binder and SrTiO3 single crystal templates to form a slurry,
- milling the slurry to a particle size of about 1 μm to form a milled slurry,
- tape casting the milled slurry to form a tape,
- cutting the tape into a plurality of shapes,
- stacking the shapes into an assembly,
- compressing the assembly to form a laminated sample,
- heating the laminated sample to burn out the binder to produce a green preform,
- and sintering the preform to form textured 0.675PMN-0.325PT.
9 more elements
A process of manufacture of a single crystal of 0.65PMN-0.35PT comprising,
- mixing (PbCO3)2Pb(OH)2 of a particle size less than about 6 μm, MgNb2O6 having a specific surface area of more than about 5 m2/g and fumed TiO2 having a specific surface area of more than about 30 m2/g to form a mixture,
- the (PbCO3)2Pb(OH)2, the fumed TiO2, and the MgNb2O6 present in amounts sufficient to produce a ratio of (PbCO3)2Pb(OH)2:MgNb2O6:fumed TiO2 of about 1:0.24:0.1 to about 1:0.0.27:0.12,
- milling said mixture in distilled water to produce a slurry having particle size of less than about 3 μm,
- heat treating the slurry to produce a dried precursor powder,
- grinding the dried precursor powder to produce a ground dried precursor powder of a size less than about 200 μm,
- compressing the dried ground powder to produce a compressed preform,
- placing a lead titanate single crystal on the compressed preform,
- depositing an additional amount of the ground dried precursor powder over the lead titanate single crystal,
- compressing the preform having the dried precursor powder and barium titanate single crystal thereon to produce a compact, and
- sintering the compact to produce a single crystal of 0.65PMN-0.35PT.
7 more elements
Dependencies are inferred from the claim text.