DE2940393A1 - Piezoelectric ceramic based on lead titanate zirconate - contg. copper, niobium and manganese for frequency stable oscillator - Google Patents

Piezoelectric ceramic based on lead titanate zirconate - contg. copper, niobium and manganese for frequency stable oscillator

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Publication number
DE2940393A1
DE2940393A1 DE19792940393 DE2940393A DE2940393A1 DE 2940393 A1 DE2940393 A1 DE 2940393A1 DE 19792940393 DE19792940393 DE 19792940393 DE 2940393 A DE2940393 A DE 2940393A DE 2940393 A1 DE2940393 A1 DE 2940393A1
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Prior art keywords
piezoelectric ceramic
contg
niobium
manganese
copper
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Granted
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DE19792940393
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German (de)
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DE2940393C2 (en
Inventor
Ing.(grad.) Walter 8505 Röthenbach Christoffers
Helmut 7440 Nürtingen Hanisch
Hermann Dr.-Ing. 7146 Tamm Schichl
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Alcatel Lucent Deutschland AG
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Standard Elektrik Lorenz AG
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Priority to DE19792940393 priority Critical patent/DE2940393A1/en
Publication of DE2940393A1 publication Critical patent/DE2940393A1/en
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Publication of DE2940393C2 publication Critical patent/DE2940393C2/de
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
    • C04B35/49—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates
    • C04B35/491—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates based on lead zirconates and lead titanates, e.g. PZT
    • C04B35/493—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates based on lead zirconates and lead titanates, e.g. PZT containing also other lead compounds
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N30/00—Piezoelectric or electrostrictive devices
    • H10N30/80—Constructional details
    • H10N30/85—Piezoelectric or electrostrictive active materials
    • H10N30/853—Ceramic compositions

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Composite Materials (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

Piezoelectric ceramic (I) based on a solid soln. of Pb titanate and Pb zirconate has the formula Pb(Cu one quarter Nb three quarters)x(Mn one third Nb two thirds)y(TizZru03 (in which x+y+z+u is 1 and x is 0.01-0.34, y is 0.01-0.34, x+y is 0.02-0.35 and z is 0.1-0.75). The ceramic is specified for use as frequency-stable oscillator, i.e. with little variation of resonance frequency with time and low temp. coefft. of resonance frequency.

Description

Piezoelektrische Keramik Piezoelectric ceramics

Die Erfindung bezieht sich auf eine piezoelektrische Keramik auf der Basis einer festen Lösung von Bleititanat und Bleizirkonat.The invention relates to a piezoelectric ceramic on the Base of a solid solution of lead titanate and lead zirconate.

Piezoelektrische Keramiken auf der Basis einer festen Lösung von Bleititanat und Bleizirkonat sind in vielfacher Zusammensetzuno bekannt. Solche Massen werden in an sich bekannter Weise durch Pressen und Sintern der gut gemischten Ausgangssubstanzen hergestellt und anschließend durch Anlegen einer Gleichspannung zwischen Elektroden polarisiert, um ihnen die für die Verwenduno erforderlichen Eigenschaften zu verleihen. Neben einer möglichst geringen Porosität der Endprodukte, die insbesondere durch eine Sinteruna unter vermindertem Druck erzielt werden kann, sind, je nach dem Verwendungszweck, die verschiedenen elektrischen Eigenschaften der Keramik von besonderer Bedeutung.Piezoelectric ceramics based on a solid solution of lead titanate and lead zirconate are known in a variety of compositions. Such crowds will be in a manner known per se by pressing and sintering the well mixed starting substances and then by applying a DC voltage between electrodes polarized in order to give them the properties required for their use. In addition to the lowest possible porosity of the end products, in particular through Sinteruna can be achieved under reduced pressure, depending on the intended use, the various electrical properties of ceramics are of particular importance.

Die elektrischen Eigenschaften von piezoelektrischer Keramik hängen sehr wesentlich von der Zusammensetzung der Keramik ab. Dabei spielen die Art und der Anteil der in der Masse vorhandenen chemischen Elemente eine große Rolle. Es sind bereits piezoelektrische Keramiken der unterschiedlichsten Zusammensetzung bekannt, die jeweils unterschiedliche elektrische Eigenschaften haben. Aufgrund einer bekannten chemischen Zusammensetzung lassen sich jedoch die elektrischen Eigenschaften nicht voraussagen, wie auch umgekehrt es nicht möglich ist, bestimmte elektrische Eigenschaften planmäßig durch Auswahl einer bestimmten Zusammensetzung zu erzielen. Da sich eine große Anzahl von chemischen Elementen als Bestandteil für piezoelektrische Keramik eignet und schon deren Kombinationsmöglichkeit sehr groß ist, und außerdem bei vorgegebenen chemischen Bestandteilen die Variationsmöglichkeit der Anteile der einzelnen Bestandteile wiederum sehr groß ist, ist es nicht möglich, durch eine begrenzte Anzahl von Versuchen piezoelektrische Keramiken bestimmter Eigenschaften zu erhalten.The electrical properties of piezoelectric ceramics depend on it depends very much on the composition of the ceramic. The kind and play the proportion of the chemical elements present in the mass plays a major role. It are already piezoelectric ceramics of the most varied of compositions known, each of which has different electrical properties. Because of However, the electrical properties can be determined from a known chemical composition not predict just as vice versa it is not possible to determine certain electrical properties planned by selecting a certain composition to achieve. Because there are a large number of chemical elements as a constituent suitable for piezoelectric ceramics and the possibility of combining them is very good is large, and also the possibility of variation with given chemical constituents the proportions of the individual components is again very large, it is not possible by a limited number of experiments piezoelectric ceramics determined Properties.

Aufgabe der Erfindung ist es, eine piezoelektrische Keramik zu schaffen, die sich insbesondere für frequenzstabile Schwinger eignet, d.h. eine piezoelektrische Keramik mit geringer zeitlicher änderung der Resonanzfrequenz und einem geringen Temperaturkoeffizienten der Resonanzfrequenz.The object of the invention is to create a piezoelectric ceramic, which is particularly suitable for frequency-stable transducers, i.e. a piezoelectric Ceramic with a low change in the resonance frequency over time and a low one Temperature coefficient of the resonance frequency.

Diese Aufgabe wird durch die im Anspruch 1 angegebene Zusammensetzung der piezoelektrischen Keramik gelöst.This object is achieved by the composition specified in claim 1 solved the piezoelectric ceramic.

Aus der DE-OS 1 646 740 und aus der DE-AS 1 646 823 sind bereits piezoelektrische Keramiken der Zusammensetzung Pb(Mnl/3Nb2/3)TiZrO3 bekannt. Weiter ist aus der DE-AS 1 950 317 eine piezoelektrische Keramik der Zusammensetzung Pb(Cu1#4Nb314)TiZr03 bekannt.From DE-OS 1 646 740 and from DE-AS 1 646 823 piezoelectric Ceramics of the composition Pb (Mnl / 3Nb2 / 3) TiZrO3 are known. Next is from the DE-AS 1 950 317 a piezoelectric ceramic of the composition Pb (Cu1 # 4Nb314) TiZr03 known.

Es war jedoch nicht vorauszusehen, daß eine piezoelektrische Keramik, welche durch bestimmte Kombination der genannten bekannten Zusammensetzungen erhalten wird, gerade eine Resonanzfrequenz mit geringer zeitlicher änderung und mit einem geringen Temperaturkoeffizienten haben wird.However, it was not foreseeable that a piezoelectric ceramic, which by certain combination of known compositions mentioned is obtained, just a resonance frequency with little change over time and with a low temperature coefficient will have.

Außerdem war es für den Fachmann nicht naheliegend gewesen, gerade aus diesen beiden bekannten Zusammensetzungen einen neuen Stoff zu schaffen, da es noch sehr viele andere tflönlichkeiten gibt, aus bekannten Zusamrnensetzuncien eine neue Zusammensetzung zu bilden. Schließlich war es auch nicht naheliegend, die Anteile der einzelnen Bestandteile der neuen piezoelektrischen Keramik gerade in dem im Anspruch 1 angegebenen enoenvernltnir zu wählen.Besides, it hadn't been obvious to the specialist, especially to create a new substance from these two known compositions, since There are a great many other personalities from known compositions to form a new composition. After all, it wasn't obvious either the proportions of the individual components of the new piezoelectric ceramic straight in the enoenvernltnir specified in claim 1 to choose.

Die piezoelektrische Keramik gemäy der Erfindung wird in an sich bekannter Weise so hergestellt, daß die Ausgangssubstanzen, und zwar die Carbonate und Oxide der einzelnen Bestandteile, im entsprechenden Mennenverhaltnis bis zur Homogenisierung gemahlen und gemischt und bei einer TemDeratur von 700 - 900 0C kalziniert werden. Anschließend wird nochmals gemahlen und das so erhaltene Pulver durch einen isostatischen Preßvorganq bei Paumtemperatur mit einem Druck von etwa 3,6 ~ 108N/qm zu Körpern gepreßt, die einer Sinterung zwischen 1250 und 1300 0C unterworfen werden. Der erste Teil der Sinterung ird unter vermindertem Druck vorgenommen und der zweite Teil der Sinterung bei Normaldruck in oxidierender Atmosphäre. Hierbei werden weitgehend porenfreie Körper hoher Dichte erhalten.The piezoelectric ceramic according to the invention is known per se Way made so that the starting substances, namely the carbonates and oxides of the individual components, in the appropriate proportion up to homogenization ground and mixed and calcined at a temperature of 700 - 900 ° C. It is then ground again and the powder obtained in this way through an isostatic Pressing process at Paum temperature with a pressure of about 3.6 ~ 108N / qm to form bodies pressed, which are subjected to sintering between 1250 and 1300 0C. The first Part of the sintering is carried out under reduced pressure and the second part sintering at normal pressure in an oxidizing atmosphere. Here are largely Obtain high density non-porous bodies.

In den nachfolgenden Tabellen sind Beisoiele für Zusammensetzungen gemäß der Erfindung und deren elektrische Ei den schaften angegeben.The following tables are examples of compositions according to the invention and their electrical egg specified the shafts.

In den Tabellen bedeuten: x : Molarer Anteil an Pb(Cu114Nb314)03 y : Molarer Anteil an Pb(Mn113Nb213)03 z : Molarer Anteil an PbTiO3 u : Molarer Anteil an PbZr03 fs : Die Resonanzfrequenz in kHz tan X : Der Verlustfaktor bei 1 kHz kr Der Kopplungsfaktor der Radialschwinguno : : die Permitivität TEE : Der Temperaturkoeffizient der Permitivität TK : Der Temperaturkoeffizient der Resonanzfrequenz O : Die Güte 9 : Die Dichte N : Die Schaltgeschwindigkeit Aus den Tabellen kann entnommen werden, daß der Temperaturkoeffizient der Resonanzfrequenz sehr kleine, teils negative und teils positive Werte hat, so daß durch Auswahl einer geeigneten dazwischenliegenden Zusammensetzung praktisch ein Temperaturkoeffizient Null erzielt werden kann. Die Dichte ist sehr hoch und liegt fast beim theoretischen Wert. Die zeitliche Anderung der Resonanzfrequenz ist sehr gering und ist kleiner oder gleich 0,1 # pro Zeitdekade. Der Temperaturkoeffizient der Resonanzfrequenz liegt unter 30 ppm pro OC.In the tables: x: molar proportion of Pb (Cu114Nb314) 03 y : Molar fraction of Pb (Mn113Nb213) 03 z: Molar fraction of PbTiO3 u: Molar fraction an PbZr03 fs: The resonance frequency in kHz tan X: The loss factor at 1 kHz kr The coupling factor of the radial oscillation:: the permittivity TEE: the temperature coefficient the permittivity TK: the temperature coefficient of the resonance frequency O: the quality 9: The density N: The switching speed From the tables it can be seen that the temperature coefficient of the resonance frequency is very small, partly negative and partly has positive values, so that by choosing a suitable one in between Composition practically a temperature coefficient of zero can be achieved. the Density is very high and is almost the theoretical value. The change in time the resonance frequency is very low and is less than or equal to 0.1 # per decade of time. The temperature coefficient of the resonance frequency is below 30 ppm per OC.

Zusätzlich wird eine hohe piezoelektrische Aktivität erhalten, so daß die piezoelektrische Keramik gemäß der Erfindung sich nicht nur für Schwinger für frequenzstabile Oszillatoren eignet, sondern auch sehr gut für Filteranwendungen geeignet ist.In addition, a high piezoelectric activity is obtained, see above that the piezoelectric ceramic according to the invention is not only suitable for vibrators suitable for frequency-stable oscillators, but also very good for filter applications suitable is.

Wie aus den Tabellen weiterhin entnommen werden kann, können Gütewerte bis 4500 erreicht werden.As can also be seen from the tables, quality values until 4500 can be reached.

Tabelle 1 Zusammensetzung fs 0> 0 x y z u E##zJ k r 1 0,06 0,06 0,38 0,50 170,18 0,0014 45,78 2 0,06 0,06 0,33 0,55 176,15 0,0011 39,53 3 0,06 0,06 0,28 0,60 180,64 0,0011 32,96 4 0,06 0,06 0,23 0,65 182,39 0,0013 26,63 5 0,06 0,06 0,18 0,70 180,10 0,0020 21,06 6 0,06 0,06 0,13 0,75 180,86 0,0013 16,74 7 0,03 0,03 0,44 0,5Q 162,12 0,0008 55,43 8 0,03 0,03 0,39 0,55 171,08 0,0008 45,13 9 9 0,03 0,03 0,34 0,60 177,43 0,0012 35,76 10 0,03 0,03 0,29 0,65 179,77 0,0014 29,63 11 0,03 0,03 0,2t 0,70 179,02 0,0015 21,12 Tabelle 2 = TK c T t3 fs 0 lo 3 1C## 1 412 5,32 -255 2428 8,02 2 363 5,50 -208 23P0 8,01 3 330 5,80 -175 3360 8,00 4 309 5,64 - 78 4543 7,99 5 298 6,10 200 3700 7,99 6 291 7,20 270 3307 7,99 7 505 5,3 -339 1452 8,02 8 380 4,8 -235 1826 8,02 9 349 a,8 -165 2126 8,01 10 322 5,0 + 10 2310 7,99 11 310 5,2 385 3075 7,99 Tabelle 3 = Zusammensetzung N 0> x y z u m/sek k ç o 12 0,06 G,065 0,43 0,445 1720 30,3 600 13 0,06 0,065 0,44 0,435 1630 32,6 990 14 0,0 0,065 0,45 0,425 1615 31,3 1180 15 0,06 0,065 0,46 0,415 1660 27,0 1140 16 0,06 0,065 0,47 0,405 1665 26,6 1110 17 0,06 0,065 0,48 0,395 1690 25,1 1040 18 ~ 0,0 0,065 0,50 0,375 1773 20,4 790 9 0.06 0,065 0,55 0,325 1850 14,5 540 Tabelle 4 z 0> fs 0 10 1O 12 6,20 -420 1650 8,028 13 5,50 -350 1280 7,96 14 3,15 - 90 1300 8,02 15 2,28 + 20 1800 1 8,01 16 2,30 + 25 1930 7,99 17 2,45 + 11 2050 7,99 18 2,7 - 45 2500 8,01 19 2,9 -145 3000 8,01 Table 1 Composition fs 0> 0 xyzu E ## zJ kr 1 0.06 0.06 0.38 0.50 170.18 0.0014 45.78 2 0.06 0.06 0.33 0.55 176.15 0.0011 39.53 3 0.06 0.06 0.28 0.60 180.64 0.0011 32.96 4 0.06 0.06 0.23 0.65 182.39 0.0013 26.63 5 0.06 0.06 0.18 0.70 180.10 0.0020 21.06 6 0.06 0.06 0.13 0.75 180.86 0.0013 16.74 7 0.03 0.03 0.44 0.5Q 162.12 0.0008 55.43 8 0.03 0.03 0.39 0.55 171.08 0.0008 45.13 9 9 0.03 0.03 0.34 0.60 177.43 0.0012 35.76 10 0.03 0.03 0.29 0.65 179.77 0.0014 29.63 11 0.03 0.03 0.2t 0.70 179.02 0.0015 21.12 Table 2 = TK c T t3 fs 0 lo 3 1C ## 1 412 5.32 -255 2428 8.02 2,363 5.50 -208 23P0 8.01 3 330 5.80 -175 3360 8.00 4,309 5.64-78 4543 7.99 5 298 6.10 200 3700 7.99 6 291 7.20 270 3307 7.99 7,505 5.3 -339 1,452 8.02 8 380 4.8 -235 1826 8.02 9 349 a, 8 -165 2126 8.01 10 322 5.0 + 10 2310 7.99 11 310 5.2 385 3075 7.99 Table 3 = Composition N 0> xyzum / sec k ç O 12 0.06 G, 065 0.43 0.445 1720 30.3 600 13 0.06 0.065 0.44 0.435 1630 32.6 990 14 0.0 0.065 0.45 0.425 1615 31.3 1180 15 0.06 0.065 0.46 0.415 1660 27.0 1140 16 0.06 0.065 0.47 0.405 1665 26.6 1110 17 0.06 0.065 0.48 0.395 1690 25.1 1040 18 ~ 0.0 0.065 0.50 0.375 1773 20.4 790 9 0.06 0.065 0.55 0.325 1850 14.5 540 Table 4 z 0> fs 0 10 1O 12 6.20 -420 1650 8.028 13 5.50 -350 1280 7.96 14 3.15 - 90 1300 8.02 15 2.28 + 20 1800 1 8.01 16 2.30 + 25 1930 7.99 17 2.45 + 11 2050 7.99 18 2.7 - 45 2500 8.01 19 2.9 -145 3000 8.01

Claims (5)

Ansprüche 1.) Piezoelektrische Keramik auf der Basis einer festen Lösung von Bleititanat und Bleizirkonat, g e k e n n z e i c h n e t d u r c h die allgemeine Formel Pb(Cu1/4Nb3/4)x(Mn1/3Nb2/3)y TizZruO3, worin x + y + z + u = 1 und x = 0,01 - 0,34, y = 0,01 - 0,34, x + y = 0,02 - 0,35 und z = 0,1 - 0,75.Claims 1.) Piezoelectric ceramic based on a solid Solution of lead titanate and lead zirconate general formula Pb (Cu1 / 4Nb3 / 4) x (Mn1 / 3Nb2 / 3) y TizZruO3, where x + y + z + u = 1 and x = 0.01-0.34, y = 0.01-0.34, x + y = 0.02-0.35 and z = 0.1-0.75. 2.) Piezoelektrische Keramik nach Anspruch 1, dadurch gekennzeichnet, daß x und y gleich oder fast gleich sind.2.) Piezoelectric ceramic according to claim 1, characterized in that that x and y are equal or almost equal. 3.) Piezoelektrische Keramik nach Anspruch 2, dadurch gekennzeichnet, daß x = y = 0,06.3.) Piezoelectric ceramic according to claim 2, characterized in that that x = y = 0.06. 4.) Piezoelektrische Keramik nach AnsDruch 2, dadurch gekennzeichnet, daß x = y = 0,03.4.) Piezoelectric ceramic according to AnsDruch 2, characterized in that that x = y = 0.03. 5.) Piezoelektrische Keramik nach Anspruch 2, dadurch gekennzeichnet, daß x = 0,06 und y = 0,065.5.) Piezoelectric ceramic according to claim 2, characterized in that that x = 0.06 and y = 0.065.
DE19792940393 1979-10-05 1979-10-05 Piezoelectric ceramic based on lead titanate zirconate - contg. copper, niobium and manganese for frequency stable oscillator Granted DE2940393A1 (en)

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DE19792940393 DE2940393A1 (en) 1979-10-05 1979-10-05 Piezoelectric ceramic based on lead titanate zirconate - contg. copper, niobium and manganese for frequency stable oscillator

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0780350A1 (en) * 1995-12-20 1997-06-25 Murata Manufacturing Co., Ltd. Piezoelectric ceramic composition
DE102016107405A1 (en) * 2016-04-21 2017-10-26 Epcos Ag Piezoceramic, method for its production and electroceramic device comprising the piezoceramic

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1646823B1 (en) * 1966-12-29 1971-06-16 Nippon Electric Co PIEZOELECTRIC CERAMIC FABRIC
DE1646740A1 (en) * 1967-06-29 1971-08-26 Matsushita Electric Ind Co Ltd Piezoelectric ceramic masses
DE1950317B2 (en) * 1968-10-01 1971-11-25 Matsushita Electric Industrial Co. Ltd., Kadoma, Osaka (Japan) PIEZOELECTRIC CERAMICS
DE2456050A1 (en) * 1973-11-24 1975-05-28 Matsushita Electric Ind Co Ltd METHOD OF MANUFACTURING FERROELECTRIC CERAMICS

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1646823B1 (en) * 1966-12-29 1971-06-16 Nippon Electric Co PIEZOELECTRIC CERAMIC FABRIC
DE1646740A1 (en) * 1967-06-29 1971-08-26 Matsushita Electric Ind Co Ltd Piezoelectric ceramic masses
DE1950317B2 (en) * 1968-10-01 1971-11-25 Matsushita Electric Industrial Co. Ltd., Kadoma, Osaka (Japan) PIEZOELECTRIC CERAMICS
DE2456050A1 (en) * 1973-11-24 1975-05-28 Matsushita Electric Ind Co Ltd METHOD OF MANUFACTURING FERROELECTRIC CERAMICS

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0780350A1 (en) * 1995-12-20 1997-06-25 Murata Manufacturing Co., Ltd. Piezoelectric ceramic composition
US5798052A (en) * 1995-12-20 1998-08-25 Murata Manufacturing Co., Ltd. Piezoelectric ceramic composition
DE102016107405A1 (en) * 2016-04-21 2017-10-26 Epcos Ag Piezoceramic, method for its production and electroceramic device comprising the piezoceramic

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