US3956150A
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Method of preparing ferroelectric ceramics
Assignee: Panasonic Holdings Corp
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Filing: 1974-11-18
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Granted: 1976-05-11
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Expires: 1994-11-18
Abstract
Abstract A process for preparing strengthened ferroelectric ceramics, which comprises heat treatment of sintered ceramics after sintering of ceramic materials at a temperature range from about 100 DEG to about 400 DEG C. lower than the final sintering temperature of ceramics, holding it for about 1 to about 60 hrs, and then cooling it at a cooling rate from about 300 DEG to about 10 DEG C. per hour. Strengthened ferroelectric ceramics are obtained among the following ferroelectric ceramic compositions:
Inventors
- 👤 Hiromu Ouchi
- 👤 Masamitsu Nishida
- 👤 Kazunori Numata
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-28 21:13
CPC Classifications
C; C04; C04B; C04B35/00; C04B35/01; C04B35/48; C04B35/49; C04B35/491; C04B35/493; H; H10; H10N; H10N30/00; H10N30/80; H10N30/85; H10N30/853
Claims Analysis
Total Claims: 14
Claim 1
Independent Claim
312 words
A method of preparing ferroelectric ceramics selected from the group consisting of: I pb ([B 1 ] A Nb 1-A )O 3 -PbTiO 3 -PbZrO 3 , where [B 1 ] is one member selected from the group consisting of Mg, Zn, Cd, Sn, Mn, Fe, Co and Ni when A=1/3, and [B 1 ] is one member selected from the group consisting of Li and Cu when A=1/4, Ii. pb ([B 2 ] B Nb 1-B )O 3 -Pb([B 3 ] C Nb 1-C )O 3 -PbTiO 3 -PbZrO 3 , where each of [B 2 ] and [B 3 ], [B 2 ]≠[B 3 ], is one member selected from the group consisting of Mg, Zn, Cd, Sn, Mn, Fe, Co and Ni when B and C=1/3, and each of [B 2 ] and [B 3 ], [B 2 ]≠[B 3 ], is one member selected from the group consisting of Li and Cu when B and C=1/4, Iii. pb ([B 1 ] A Nb 1-A )O 3 -PbTiO 3 -PbZrO 3 with MnO 2 , where [B 1 ] is one member selected from the group consisting of Mg, Zn, Cd, Sn, Fe, Co and Ni when A=1/3, and [B 1 ] is one member selected from the group consisting of Li and Cu when A=1/4, and Iv. pb([B 2 ] B Nb 1-B )O 3 -Pb([B 3 ] C Nb 1-C )O 3 -PbTiO 3 -PbZrO 3 with MnO 2 , where each of [B 2 ] and [B 3 ], [B 2 ≠B 3 ], is one member selected from the group consisting of Mg, Zn, Cd, Sn, Fe, Co and Ni when B and C=1/3, and each of [B 2 ] and [B 3 ], [B 2 ]≠[B 2 ], is one member selected from the group consisting of Li and Cu when B and C=1/4,
Claim 2
Independent Claim
312 words
A method of preparing ferroelectric ceramics selected from the group consisting of: I pb ([B 1 ] A Nb 1-A )O 3 -PbTiO 3 -PbZrO 3 , where [B 1 ] is one member selected from the group consisting of Mg, Zn, Cd, Sn, Mn, Fe, Co and Ni when A=1/3, and [B 1 ] is one member selected from the group consisting of Li and Cu when A=1/4, Ii. pb ([B 2 ] B Nb 1-B )O 3 -Pb([B 3 ] C Nb 1-C )O 3 -PbTiO 3 -PbZrO 3 , where each of [B 2 ] and [B 3 ], [B 2 ]≠[B 3 ], is one member selected from the group consisting of Mg, Zn, Cd, Sn, Mn, Fe, Co and Ni when B and C=1/3, and each of [B 2 ] and [B 3 ], [B 2 ]≠[B 3 ], is one member selected from the group consisting of Li and Cu when B and C=1/4, Iii. pb ([B 1 ] A Nb 1-A )O 3 -PbTiO 3 -PbZrO 3 with MnO 2 , where [B 1 ] is one member selected from the group consisting of Mg, Zn, Cd, Sn, Fe, Co and Ni when A=1/3, and [B 1 ] is one member selected from the group consisting of Li and Cu when A=1/4, and Iv. pb([B 2 ] B Nb 1-B )O 3 -Pb([B 3 ] C Nb 1-C )O 3 -PbTiO 3 -PbZrO 3 with MnO 2 , where each of [B 2 ] and [B 3 ], [B 2 ≠B 3 ], is one member selected from the group consisting of Mg, Zn, Cd, Sn, Fe, Co and Ni when B and C=1/3, and each of [B 2 ] and [B 3 ], [B 2 ]≠[B 2 ], is one member selected from the group consisting of Li and Cu when B and C=1/4,
Claim 3
Dependent Claim
107 words
said method comprising: calcining at 700° to 900°C a powdered mixture of the oxides, hydroxides or carbonates of the metals to be contained in the ceramics to form a solid solution and then sintering at 1200° to 1300°C, then heat treating at a temperature lower by about 100°C to about 400°C than the sintering temperature, maintaining said heat treating for from about 1 hour to about 60 hours, and then cooling the material subjected to said heat treatment at a cooling rate from about 300°C per hour to about 10°C per hour, so as to increase the tensile strength and decrease the resonant impedance of said ceramics.
Claim 4
Dependent Claim
107 words
said method comprising: calcining at 700° to 900°C a powdered mixture of the oxides, hydroxides or carbonates of the metals to be contained in the ceramics to form a solid solution and then sintering at 1200° to 1300°C, then heat treating at a temperature lower by about 100°C to about 400°C than the sintering temperature, maintaining said heat treating for from about 1 hour to about 60 hours, and then cooling the material subjected to said heat treatment at a cooling rate from about 300°C per hour to about 10°C per hour, so as to increase the tensile strength and decrease the resonant impedance of said ceramics.
Claim 5
Independent Claim
129 words
A method of preparing ferroelectric ceramics comprising the material system Pb(Ni 1/3 Nb 2/3 )O 3 -PbTiO 3 -PbZrO 3 in solid solution, said method comprising: calcining at 700° to 900°C a powdered mixture of the oxides, hydroxides or carbonates of the metals to be contained in the ceramics, to form a solid solution and then sintering at 1200° to 1300°C, then heat treating at a temperature lower by about 100° to about 400°C than the sintering temperature, maintaining said heat treatment for from about 1 hour to about 60 hours, and cooling the material subjected to said heat treatment at a cooling rate from about 300° per hour to about 10°C per hour, so as to increase the tensile strength and decrease the resonant impedance of said ceramics.
Claim 6
Independent Claim
129 words
A method of preparing ferroelectric ceramics comprising the material system Pb(Ni 1/3 Nb 2/3 )O 3 -PbTiO 3 -PbZrO 3 in solid solution, said method comprising: calcining at 700° to 900°C a powdered mixture of the oxides, hydroxides or carbonates of the metals to be contained in the ceramics, to form a solid solution and then sintering at 1200° to 1300°C, then heat treating at a temperature lower by about 100° to about 400°C than the sintering temperature, maintaining said heat treatment for from about 1 hour to about 60 hours, and cooling the material subjected to said heat treatment at a cooling rate from about 300° per hour to about 10°C per hour, so as to increase the tensile strength and decrease the resonant impedance of said ceramics.
Claim 7
Independent Claim
135 words
A method of preparing ferroelectric ceramics comprising the material system Pb(Mg 1/3 Nb 2/3 )O 3 -Pb(Mn 1/3 Nb 2/3 )O 3 -PbTiO 3 -PbZrO 3 in solid solution, said method comprising: calcining at 700° to 900°C a powdered mixture of the oxides, hydroxides or carbonates of the metals to be contained in the ceramics, to form a solid solution and then sintering at 1200° to 1300°C, then heat treating at a temperature lower by about 100° to about 400°C than the sintering temperature, maintaining said heat treatment for from about 1 hour to about 60 hours, and cooling the material subjected to said heat treatment at a cooling rate from about 300°C per hour to about 10°C per hour so as to increase the tensile strength and decrease the resonant impedance of said ceramics.
Claim 8
Independent Claim
135 words
A method of preparing ferroelectric ceramics comprising the material system Pb(Mg 1/3 Nb 2/3 )O 3 -Pb(Mn 1/3 Nb 2/3 )O 3 -PbTiO 3 -PbZrO 3 in solid solution, said method comprising: calcining at 700° to 900°C a powdered mixture of the oxides, hydroxides or carbonates of the metals to be contained in the ceramics, to form a solid solution and then sintering at 1200° to 1300°C, then heat treating at a temperature lower by about 100° to about 400°C than the sintering temperature, maintaining said heat treatment for from about 1 hour to about 60 hours, and cooling the material subjected to said heat treatment at a cooling rate from about 300°C per hour to about 10°C per hour so as to increase the tensile strength and decrease the resonant impedance of said ceramics.
Claim 9
Independent Claim
132 words
A method of preparing ferroelectric ceramics comprising the material system Pb(Li 1/4 Nb 3/4 )O 3 -PbTiO 3 -PbZrO 3 plus MnO 2 in solid solution, said method comprising: calcining at 700° to 900°C a powdered mixture of the oxides, hydroxides or carbonates of the metals to be contained in the ceramics, to form a solid solution and then sintering at 1200° to 1300°C, then heat treating at a temperature lower by about 100° to about 400°C than the sintering temperature, maintaining said heat treatment for from about 1 hour to about 60 hours, and cooling the material subjected to said heat treatment at a cooling rate from about 300° per hour to about 10°C per hour, so as to increase the tensile strength and decrease the resonant impedance of said ceramics.
Claim 10
Independent Claim
132 words
A method of preparing ferroelectric ceramics comprising the material system Pb(Li 1/4 Nb 3/4 )O 3 -PbTiO 3 -PbZrO 3 plus MnO 2 in solid solution, said method comprising: calcining at 700° to 900°C a powdered mixture of the oxides, hydroxides or carbonates of the metals to be contained in the ceramics, to form a solid solution and then sintering at 1200° to 1300°C, then heat treating at a temperature lower by about 100° to about 400°C than the sintering temperature, maintaining said heat treatment for from about 1 hour to about 60 hours, and cooling the material subjected to said heat treatment at a cooling rate from about 300° per hour to about 10°C per hour, so as to increase the tensile strength and decrease the resonant impedance of said ceramics.
Claim 11
Independent Claim
139 words
A method of preparing ferroelectric ceramics comprising the material system Pb(Zn 1/3 Nb 2/3 )O 3 -Pb(Sn 1/3 Nb 2/3 )O 3 -PbTiO 3 -PbZrO 3 plus MnO 2 in solid solution, said method comprising: calcining at 700° to 900°C a powdered mixture of the oxides, hydroxides or carbonates of the metals to be contained in the ceramics to form a solid solution and then sintering at 1200° to 1300°C, then heat treating at a temperature lower by about 100°C to about 400°C than the sintering temperature, maintaining said heat treatment for from about 1 hour to about 60 hours, and then cooling said material subjected to said heat treatment at a cooling rate from about 300°C per hour to about 10°C per hour, so as to increase the tensile strength and decrease the resonant impedance of said ceramics.
Claim 12
Independent Claim
139 words
A method of preparing ferroelectric ceramics comprising the material system Pb(Zn 1/3 Nb 2/3 )O 3 -Pb(Sn 1/3 Nb 2/3 )O 3 -PbTiO 3 -PbZrO 3 plus MnO 2 in solid solution, said method comprising: calcining at 700° to 900°C a powdered mixture of the oxides, hydroxides or carbonates of the metals to be contained in the ceramics to form a solid solution and then sintering at 1200° to 1300°C, then heat treating at a temperature lower by about 100°C to about 400°C than the sintering temperature, maintaining said heat treatment for from about 1 hour to about 60 hours, and then cooling said material subjected to said heat treatment at a cooling rate from about 300°C per hour to about 10°C per hour, so as to increase the tensile strength and decrease the resonant impedance of said ceramics.
Claim 13
Independent Claim
212 words
A method of preparing ferroelectric ceramics comprising one material selected from the group consisting of Pb(Ni 1/3 Nb 2/3 ) 0 .37 Ti 0 .36 Zr 0 .27 O 3 , Pb(Mg 1/3 Nb 2/3 ) O .06 (Mn 1/3 Nb 2/3 ) 0 .06 Ti 0 .44 Zr 0 .44 O 3 , Pb(Li 1/4 Nb 3/4 ) 0 .1 Ti 0 .43 Zr 0 .47 O 3 +0.8 wt% MnO 2 , and Pb(Zn 1/3 Nb 2/3 ) 0 .05 (Sn 1/3 Nb 2/3 ) 0 .05 Ti 0 .44 Zr 0 .46 O 3 +1 wt% MnO 2 , said method comprising: calcining at 700° to 900°C a powder mixture of the oxides, hydroxides or carbonates of the metals to be contained in the ceramics to form a solid solution and then sintering at 1200° to 1300°C, then heat treating at a temperature lower by about 100° to about 400°C than the sintering temperature of said ceramics, maintaining said heat treatment for from about 1 hour to about 60 hours, and then cooling said material subjected to said heat treatment at a cooling rate from about 300°C per hour to about 10°C per hour, so as to increase the tensile strength and decrease the resonant impedance of said ceramics.
Claim 14
Independent Claim
212 words
A method of preparing ferroelectric ceramics comprising one material selected from the group consisting of Pb(Ni 1/3 Nb 2/3 ) 0 .37 Ti 0 .36 Zr 0 .27 O 3 , Pb(Mg 1/3 Nb 2/3 ) O .06 (Mn 1/3 Nb 2/3 ) 0 .06 Ti 0 .44 Zr 0 .44 O 3 , Pb(Li 1/4 Nb 3/4 ) 0 .1 Ti 0 .43 Zr 0 .47 O 3 +0.8 wt% MnO 2 , and Pb(Zn 1/3 Nb 2/3 ) 0 .05 (Sn 1/3 Nb 2/3 ) 0 .05 Ti 0 .44 Zr 0 .46 O 3 +1 wt% MnO 2 , said method comprising: calcining at 700° to 900°C a powder mixture of the oxides, hydroxides or carbonates of the metals to be contained in the ceramics to form a solid solution and then sintering at 1200° to 1300°C, then heat treating at a temperature lower by about 100° to about 400°C than the sintering temperature of said ceramics, maintaining said heat treatment for from about 1 hour to about 60 hours, and then cooling said material subjected to said heat treatment at a cooling rate from about 300°C per hour to about 10°C per hour, so as to increase the tensile strength and decrease the resonant impedance of said ceramics.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1979-05-11 | 1979-11-10 | 1980-05-11 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1983-05-11 | 1983-11-10 | 1984-05-11 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1987-05-11 | 1987-11-10 | 1988-05-11 | $7700.00 | Window Closed / Lapsed |