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US3956150A Expired / Lapsed US ⏱️ 0.0 years remaining

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
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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)

US3518199A Cited
US3528918A Cited
US3595795A Cited
US3669887A Cited

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

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