DE1926812A1 - Piezoelectric ceramic mass used in manufacture of - wave filters and electromechanical converters - Google Patents
Piezoelectric ceramic mass used in manufacture of - wave filters and electromechanical convertersInfo
- Publication number
- DE1926812A1 DE1926812A1 DE19691926812 DE1926812A DE1926812A1 DE 1926812 A1 DE1926812 A1 DE 1926812A1 DE 19691926812 DE19691926812 DE 19691926812 DE 1926812 A DE1926812 A DE 1926812A DE 1926812 A1 DE1926812 A1 DE 1926812A1
- Authority
- DE
- Germany
- Prior art keywords
- pbtio3
- pbzro3
- zno
- tho2
- mol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000919 ceramic Substances 0.000 title claims abstract description 42
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 9
- 229910003781 PbTiO3 Inorganic materials 0.000 claims abstract description 15
- 229910020698 PbZrO3 Inorganic materials 0.000 claims abstract description 15
- 239000000203 mixture Substances 0.000 claims abstract description 15
- 239000006104 solid solution Substances 0.000 claims abstract description 9
- 229910052745 lead Inorganic materials 0.000 claims abstract description 5
- 229910052776 Thorium Inorganic materials 0.000 claims abstract description 4
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 4
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 4
- 229910017052 cobalt Chemical group 0.000 claims abstract description 3
- 239000010941 cobalt Chemical group 0.000 claims abstract description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical group [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical group [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract 4
- 229910052759 nickel Inorganic materials 0.000 claims abstract 2
- 238000010586 diagram Methods 0.000 claims description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- 239000011651 chromium Substances 0.000 claims description 5
- 239000011701 zinc Substances 0.000 claims description 5
- ZSLUVFAKFWKJRC-IGMARMGPSA-N 232Th Chemical compound [232Th] ZSLUVFAKFWKJRC-IGMARMGPSA-N 0.000 claims description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 2
- 229910052715 tantalum Inorganic materials 0.000 claims description 2
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 2
- 238000007792 addition Methods 0.000 abstract description 14
- 229910052748 manganese Inorganic materials 0.000 abstract description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 62
- 229910004369 ThO2 Inorganic materials 0.000 description 53
- ZCUFMDLYAMJYST-UHFFFAOYSA-N thorium dioxide Chemical compound O=[Th]=O ZCUFMDLYAMJYST-UHFFFAOYSA-N 0.000 description 50
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 description 41
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 30
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 20
- 230000008878 coupling Effects 0.000 description 15
- 238000010168 coupling process Methods 0.000 description 15
- 238000005859 coupling reaction Methods 0.000 description 15
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 11
- 239000000047 product Substances 0.000 description 9
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 description 6
- 239000000654 additive Substances 0.000 description 5
- 230000000996 additive effect Effects 0.000 description 4
- 230000008020 evaporation Effects 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 4
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 description 4
- 229910000464 lead oxide Inorganic materials 0.000 description 3
- HTUMBQDCCIXGCV-UHFFFAOYSA-N lead oxide Chemical compound [O-2].[Pb+2] HTUMBQDCCIXGCV-UHFFFAOYSA-N 0.000 description 3
- 230000010287 polarization Effects 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000008186 active pharmaceutical agent Substances 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 101100215147 Caenorhabditis elegans aco-1 gene Proteins 0.000 description 1
- 101100298998 Caenorhabditis elegans pbs-3 gene Proteins 0.000 description 1
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- 241001503987 Clematis vitalba Species 0.000 description 1
- 101000746263 Conus leopardus Conotoxin Lp5.1 Proteins 0.000 description 1
- 241001669680 Dormitator maculatus Species 0.000 description 1
- 241000277307 Esox Species 0.000 description 1
- 101100057143 Schizosaccharomyces pombe (strain 972 / ATCC 24843) cta3 gene Proteins 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 241001122767 Theaceae Species 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000004873 anchoring Methods 0.000 description 1
- 229910001422 barium ion Inorganic materials 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(II) oxide Inorganic materials [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007850 degeneration Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 150000002611 lead compounds Chemical class 0.000 description 1
- XMFOQHDPRMAJNU-UHFFFAOYSA-N lead(II,IV) oxide Inorganic materials O1[Pb]O[Pb]11O[Pb]O1 XMFOQHDPRMAJNU-UHFFFAOYSA-N 0.000 description 1
- 210000004072 lung Anatomy 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N nickel(II) oxide Inorganic materials [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229910001427 strontium ion Inorganic materials 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 230000035922 thirst Effects 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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Abstract
Description
"Piezoelelctrische keraullsche Massen und ihre Verwendung zur Herstellung von Wellenfiltern und elektromechanischen Wandlern" Priorität: 27. Mai 1968, Japan, Nr. 35 918/68 24. September 1968, Japan, Nr. 68 859 Nr. 68 860, Nr. 68 861, Nr.68 862."Piezoelectric Keraulic masses and their use for production of wave filters and electromechanical converters "Priority: May 27, 1968, Japan, No. 35 918/68 September 24, 1968, Japan, No. 68 859 No. 68 860, No. 68 861, No. 68 862
Nr. 68 863 und Nr. 68 864 Elektromechanische Wandler, wie Tonabnehmer und Mikrophone, erfordern eine große Ausgangsleistung und einen flachen Anstieg der Frequenzcharakteristiken. Es ist deshalb erwünscht, daß piezoelektrische Massen einen großen elektromechanischen Kopplungskoeffizienten (z.B. 30 % oder größer) und auch eine große Dielektrizitätskonstante aufweisen. Elektromechanische Wellenfilter für Radioemnfänger und Fernsehgeräte sollen einen genau bestimmten Wert des Kopplungskoeffizienten, einen niedrigen Resonanzwiderstand und einen großen mechanischen Gütefaktor haben Die Wandler erfordern außerdem eine große Temperatur- und Zeitstabilität der Resonanzfrequenz und anderer elektrischer Eigenschaften. Weiterhin ist es für den Gebrauch bei hohen Temperaturen erwünscht, daß keramische Massen einen hohen Curiepunkt haben. No. 68 863 and No. 68 864 Electromechanical converters, such as pickups and microphones, require a large output power and a flat slope the frequency characteristics. It is therefore desirable that piezoelectric masses a large electromechanical coupling coefficient (e.g. 30% or greater) and also have a large dielectric constant. Electromechanical wave filters for radio receivers and television sets, a precisely determined value of the coupling coefficient, have a low resonance resistance and a large mechanical quality factor The transducers also require a high temperature and time stability of the resonance frequency and other electrical properties. Furthermore, it is for use at high levels Temperatures desirable that ceramic Masses a high Curie point to have.
Es sind bereits keramische Nassen für die vorgenannten Zwecke bekannt, die als Hauptkomponente Bleititanatzirkonat oder Bariumtitanat aufweisen. Ein Teil des Bleies im Bleititanatzirkonat kann z.B. durch Bariumionen, Strontiumionen oder Calciumionen ersetzt werden. Es können auch ein oder mehrere Metalloxyde zu dem Bleititanatzirkonat hinzugefügt werden, um so die piezoelektrischen und die Sinterungscharakteristiken zu verbessern. Ceramic wetnesses are already known for the aforementioned purposes, which have lead titanate zirconate or barium titanate as their main component. A part of the lead in lead titanate zirconate can e.g. be replaced by barium ions, strontium ions or Calcium ions are replaced. There can also be one or more metal oxides to the Lead titanate zirconate can be added to improve the piezoelectric and sintering characteristics to improve.
Keramische Massen auf der Grundlage von Barlumtitanat haben einen kleinen elektromechanischen Kopplungskoeffizienten und einen niedrigen Curiepunkt bei etwa 120° C. Die Keramiken sollen deswegen nur in niedrigen Temperaturbereichen verwendet werden. Andererseits habenkermische Massen auf der Grundlage von Bleltitanatzirmonat einen relativ hohen Curiepunkt, der den Gebrauch bei hohen Temperaturen zuläßt, weisen aber gewöhnlich durch die genannten. Ceramic bodies based on barlum titanate have one small electromechanical coupling coefficient and a low Curie point at around 120 ° C. The ceramics should therefore only be used in low temperature ranges be used. On the other hand, have ceramic masses based on bleltitanate fermonth a relatively high Curie point, which allows use at high temperatures, but usually indicate by the named.
Zusätze verursachte Entartungen auf. Zur Herstellung von keramischen Massen auf der Grundlage von Bleititanatzirkonat, die zur Erzielung einer hohen Dichte gut gesintert sind, ist es oft erforderlich, die Keramiken bei einer Temperatur oberhalb 13000 C zu brennen. Während des Brennens bei solch einer hohen Temperatur ist aber eine beträchtliche Verdampfung des Bleioxyds unvermeidbar. In diesem Zusammenhang ist eine Vielzahl von Verfahren zur Verhinderung der Verdampfung des PbO vorgeschlagen worden. Es ist aber schwierig, nach diesen bekannten Verfahren Keramiken herzustellen, die die erwünschten piezoelektrischen Charakteristiken haben. Außerdem müssen die herkömmlichen Keramiken um einen grossen elektromechanischen Kopplungskoeffizient zu erhalten, unter Anwendung einer nachteiligent hohen Gleichspannung von 40 kV/cm bis 50kV/cm polarisiert werden. Additions caused degeneration. For the production of ceramic Materials based on lead titanate zirconate, which are used to achieve a high Density are well sintered, it is often necessary to keep the ceramics at one temperature to burn above 13000 C. While burning at such a high temperature but considerable evaporation of the lead oxide is unavoidable. In this context a variety of methods for preventing evaporation of the PbO are proposed been. However, it is difficult to manufacture ceramics using these known methods, which have the desired piezoelectric characteristics. In addition, the conventional ceramics by a large electromechanical coupling coefficient to get under Use of a disadvantageously high DC voltage be polarized from 40 kV / cm to 50 kV / cm.
Es ist deshalb eine Aufgabe der Erfindung, neue und verbesserte piezoelektrische keramische Massen zu schaffen, die die oben beschriebenen, bestimmten Eigenschaften aufweisen, die durch einen großen piezoelektrischen Kopplungskoeffizienten und durch eine große Dielektrizitätskonstante gekennzeichnet sind, die bei der Betriebstemperatur nicht schwanken und die ferner durch einen grossen mechanischen Gütefaktor, einen niedrigen Resonanzwiderstand und einen großen piezoelektrischen Kopplungskoeffizienten gekennzeichnet sind0 Diese Aufgaben werden durch die Erfindung gelöst, Gegenstand der Erfindung ist somit eine piezoelektrische keramische Masse, bestehend aus einer ternären festen Lösung, die als Grundkomponenten 2.5 Mol-% bis 60,0 Mol-% Pb(M1/3Mb2/3)O3, wobei M Mikkel oder Kobalt bedeutet, nicht mehr als 60,0 Mol-% PbTiO3 und nicht mehr als 80 Mol-% PbZrO3 enthält. Zusätzlich zu den genannten wesentlichen Komponenten kann sie weinigstens ein Oxyd von Mangan, Zink, Chrom, Eisen, Tantal oder Thorium als Zusatz bzw. Zusätze zur Reduzierung des Resonanzwiderstandes, zur Erhöhung des mechantschen Gütefaktors und zur Erniedrigung der Variationen der Resonanzfrequenz mit der Temperatur enthalten. Die Menge des Zusatzes soll nicht mehr als 3 Gew.-% der Zusammengesetzung des maßgeblichen ternären Systems betragen.It is therefore an object of the invention to provide new and improved piezoelectric To create ceramic masses that have the specific properties described above have, by a large piezoelectric coupling coefficient and by a large dielectric constant which are characterized at the operating temperature do not fluctuate and furthermore by a large mechanical quality factor, a low resonance resistance and a large piezoelectric coupling coefficient are characterized0 These objects are achieved by the invention, subject matter the invention is thus a piezoelectric ceramic mass, consisting of a ternary solid solution containing as basic components 2.5 mol% to 60.0 mol% Pb (M1 / 3Mb2 / 3) O3, where M is Mikkel or cobalt, not more than 60.0 mol% and not PbTiO3 contains more than 80 mol% PbZrO3. In addition to the essential components mentioned it can be at least an oxide of manganese, zinc, chromium, iron, tantalum, or thorium as an additive or additives to reduce the resonance resistance, to increase the mechanical quality factor and to reduce the variations in the resonance frequency with the temperature included. The amount of the additive should not be more than 3% by weight the composition of the relevant ternary system.
Die keramische Masse der Erfindung kann in einfacher Weise hergestellt werden und zur Herstellung von Wellenfiltern und anderer Gegenstände verwendet werden0 Wie oben erwähnt, ißt die beträcht liche Verdampfung des Bleioxyds beim Brennen bei Temperaturen oberhalb 13000 C ein Problem bei der Sinterung von Bleiverbindungen wie Bleititanatzirkonat0 Bei der keramischen Masse der Erfindung tritt ein geringerer Verlust an Bleioxyd durst. Verdampfung ein als bei Bleititanatzirkonat, weil die Masse bei Temperaturen unterhalb 13000 C gebrannt wird. Das ternäre System kann ohne eine besondere Kontrolle der PbO-Atmosphäre gebrannt werden.The ceramic mass of the invention can be produced in a simple manner and for the manufacture of wave filters and others Objects As mentioned above, the considerable evaporation of lead oxide eats away a problem with the sintering of when firing at temperatures above 13000 C Lead compounds such as lead titanate zirconate in the ceramic mass of the invention there is less loss of lead oxide thirst. Evaporation as with lead titanate zirconate, because the mass is fired at temperatures below 13000 C. The ternary system can be fired without special control of the PbO atmosphere.
Keramische Körper, die gemäß der Erfindung hergestellt sind, weisen einen planaren piezoelektrischen Kopplungskoeffizienten grös ser als 30 % auf und sind deshalb zur Verwendung bei elektromechanischen Wandlern, wie Tonabnehmern und Mikrophonen, geeignet.Ceramic bodies made according to the invention have a planar piezoelectric coupling coefficient greater than 30% and are therefore for use in electromechanical transducers such as pickups and Microphones, suitable.
Die keramischen Massen der Erfindung weisen im Temperaturbereich von -20° C bis 600 G eine Veränderung der Resonanzfrequenz von weniger als 9 x 10-6/°C auf und sind somit als Wellenfilter brauchbar.The ceramic compositions of the invention have in the temperature range of -20 ° C to 600 G a change in the resonance frequency of less than 9 x 10-6 / ° C and can therefore be used as a wave filter.
Die Veränderung der Resonanz frequenz (T.K) errechnet sich nach der Pormel: T.K = fr(60° C) - fr(-20° C) 80fr(20° C) in der fr(600 C), fr(200 C) und fr(-20° C) die Resonanzfrequenz bei 60° Cbzw. bei 200 C oder -20° C sind.The change in the resonance frequency (T.K) is calculated according to the Pormel: T.K = fr (60 ° C) - fr (-20 ° C) 80fr (20 ° C) in the fr (600 C), fr (200 C) and fr (-20 ° C) is the resonance frequency at 60 ° C or are at 200 C or -20 ° C.
Die Erfindung wird im folgenden anhand der Zeichnungen näher beschrieben. Im einzelnen zeigen: Fig. 1 ein gemäß der Erfindung verwendetes Dreiecksdiagramm eines ternären Systems xPb(Ni1/3Nb2/3)O3-yPbTiO3-zPbZrO3.The invention is described in more detail below with reference to the drawings. Show in detail: Fig. 1 shows a used according to the invention Triangle diagram of a ternary system xPb (Ni1 / 3Nb2 / 3) O3-yPbTiO3-zPbZrO3.
Fig. 2 ein gemaß der Erfindung verwendetes Dreiecksdiagramm eines ternären Systems xPb(Co1/3Nb2/3)O3-yPbTiO3-zPbZrO3 und Fig. 3 eine graphische Darstellung der Temperaturabhängigkeit der Dielektrizitätskonstanten einer beispielhaften Grundmasse Pb(Co1/3Nb2/3)O3-PbTiOZrO3 gemäß der Erfindung mit einem Zusatz von MnO2. Figure 2 is a triangular diagram of a used in accordance with the invention ternary system xPb (Co1 / 3Nb2 / 3) O3-yPbTiO3-zPbZrO3 and FIG. 3 shows a graph the temperature dependence of the dielectric constant of an exemplary matrix Pb (Co1 / 3Nb2 / 3) O3-PbTiOZrO3 according to the invention with an addition of MnO2.
In Fig. 1, die ein Dreiecksdiagramm einer ternaren festen Lösung Pb(Ni1/3Nb2/3)O3-PbTiO3-PbZrO3 darstellt> weist das System in dem Polygon ABCDEF einen planaren Kopplungskoeffizienten von ungefähr 20 % oder größer auf. Innerhalb des Polygons ABCDEF umfaßen die keramischen Massen 2,5 Mol-% bis 62,5 Mol-% von Pb(Ni1/3Nb2/3)O3, nicht mehr als 75,0 Mol-% PbTiO3 und nicht mehr als 87,5 Mol-% PbZrO3. Innerhalb des Polygons GHIJKL weisen die keramischen Massen einen planaren Kopplungskoeffizienten von ungefähr 30 % oder größer auf. Die genannten Erzeugnisse, insbesondere die letzteren, sind wertvolle elektromechanische Wandler. Die keramischen Erzeugnisse innerhalb des Polygons LMNOBAKPQ weisen in dem Temperaturbereich von -20° C bis 600 C eine Veränderung der llesonanzfre quenz unterhalb 90 x 10-6/° C auf, und sind so besonders wertvoll als piezoelektrische keramische Massen, z.B. als keramische Filter. Weiterhin weisen die Zusammensetzungen innerhalb des Polygons ABCDEF, die einen Zusatz oder Zusätze wle MnO2 usw. enthalten, einen kleinen planaren Kopplungskoeffizienten und eine geringe Veränderung der Resonanzfrequenz auf, In der Pig.2, die ein Dreiecksdiagramm einer ternären festen Lösung Pb(Co1/3Nb2/3)O3-PbTiO3-PbZrO3 darstellte weist das System innerhalb des Polygons ABCDEF einen planaren Kopplungskoeffizienten von ungefähr 20 % oder größer auf. Die keramischen Erzeugnisse innerhalb des Polygons ABCDEF umfassen 2,0 Mol-% bis 60,0 Mol-% Pb(Co1/3Nb2/3)O3, nicht mehr als 60,0 Mol-% PbTiO3 und nicht mehr als 80,0 Mol-.% PbZrO3e Die keramischen Erzeugnisse innerhalb des Polygons GHIJKL weisen einen planaren Kopplungskoeffizienten von ungefähr 40 ß oder größer auf. Die genannten Erzeugnisse, insbesondere die letzteren, sind wertvolle elektromechanische Wandler. Die keramischen Erzeugnisse innerhalb des Polygons GHIJKL Weisen im Temperaturbereich von 200 C bis 600 C eine Änderung der Resonanzfrequenz unterhalb 90 x 10-6/° C auf> und sind somit besonders wertvoll als piezoelektrische keramische Massen, z.B. als keramische Filter. Weiterhin weisen die Zusammensetzungen in dem Polygon ABCDEF, die einen Zusatz oder Zusätze wie NnO2 usw. enthalten, einen kleinen planaren Kopplungskoeffi zienten und eine geringe Änderung der Resonanzfrequenz auf, Praktische Beispiele Zur Herstellung der keramischen Nasse der Erfindung müssen die wesentlichen Ausgangsstoffe (d.h. PbO oder Pb3O4. NiO oder CoO, Nb2O5, TiO2 und ZrOz) und die gegebenenfalls weiter zuzusetzenden Bestandteile, d.h. MnO2, ZnO, Cr2O3, Fe2O3, Ta2O5 oder ThO2, mit destilliertem Wasser 10 bis 15 Stunden lang in einer mit Gummi ausgekleidaten Kugelmühle innig vermischt werden Danach wird die Mischung getrocknet und unter einem Druck von 1000 kg/cm² in die gewünschte Form gepreßt. Die geformten Stücke werden 2 Stunden bei 8500. C bis. 900° C kalziniert, in liner Kugelmühle feucht pulverisiert und getrocknet. Das trockene Produkt* daß eine kleine Menge destillierten Wassers enthält, wird unter einem Druck von 1000 kg/cm² in Scheiben von 8 mm Durchmesser und 2 mm Dicke gepreßt. Die gepreßten Scheiben werden 1 Stunde bei 11900 C bis 12500 C gebrannt. Die gesinterten keramischen Erzeugnisse werden auf beiden Seiten bis zu einer Dicke von 0,4 mm poliert. Zur Ausbildung Ton Elektroden wird die polierte Scheibe auf beiden Seiten mit. Silberfarbe überzogen und bei 6000 0 gebrannt. Zur Polarisation werden die Proben in ein Silikonälbad von 1000 C eingetaucht, 1 Stunde mit einer Gleichspannung von 15 kV/mm beaufschlagt und innerhalb 30 Minuten im elektrischen Feld auf Raumtemperatur abgekühlt. Die dielektrischen und piezoelektrischen Eigenschaften der polarisierten Proben sind gemessen und in den Tabellen 1 und II aufgeführt.In Fig. 1, which is a triangular diagram of a ternary solid solution Pb (Ni1 / 3Nb2 / 3) O3-PbTiO3-PbZrO3 represents> the system has a planar coupling coefficient in the polygon ABCDEF of about 20% or greater. Inside the polygon include ABCDEF the ceramic ones Masses 2.5 mol% to 62.5 mol% of Pb (Ni1 / 3Nb2 / 3) O3, not more than 75.0 mol% PbTiO3 and not more than 87.5 mol% PbZrO3. Point within the polygon GHIJKL the ceramic masses have a planar coupling coefficient of approximately 30% or bigger on. The products mentioned, especially the latter, are valuable electromechanical converters. The ceramic products within the polygon LMNOBAKPQ show a change in the resonance frequency in the temperature range from -20 ° C to 600 ° C frequency below 90 x 10-6 / ° C, and are particularly valuable as piezoelectric ceramic masses, e.g. as ceramic filters. Continue to show the compositions within the polygon ABCDEF that have an additive or additions wle contain MnO2, etc., a small planar coupling coefficient and a small change in the resonance frequency on, In the Pig.2, which is a triangle diagram a ternary solid solution Pb (Co1 / 3Nb2 / 3) O3-PbTiO3-PbZrO3 shows that System within the polygon ABCDEF has a planar coupling coefficient of approximately 20% or greater. The ceramic products inside the polygon ABCDEF comprise 2.0 mol% to 60.0 mol% Pb (Co1 / 3Nb2 / 3) O3, not more than 60.0 mol% PbTiO3 and not more than 80.0 mol.% PbZrO3e. The ceramic products within the Polygons GHIJKL have a planar coupling coefficient of approximately 40 ß or bigger on. The products mentioned, especially the latter, are valuable electromechanical converters. Ceramic products inside polygon GHIJKL Show a change in the resonance frequency in the temperature range from 200 C to 600 C. below 90 x 10-6 / ° C to> and are therefore particularly valuable as piezoelectric ceramic masses, e.g. as ceramic filters. Furthermore, the compositions in the polygon ABCDEF, which contain an additive or additions such as NnO2 etc., one small planar Kopplungskoeffi cients and a small change in the resonance frequency on, Practical Examples To prepare the ceramic paste of the invention must the essential starting materials (i.e. PbO or Pb3O4, NiO or CoO, Nb2O5, TiO2 and ZrOz) and the possibly further constituents to be added, i.e. MnO2, ZnO, Cr2O3, Fe2O3, Ta2O5 or ThO2, with distilled water for 10 to 15 hours are then intimately mixed in a rubber-lined ball mill the mixture is dried and made into the desired one under a pressure of 1000 kg / cm² Pressed shape. The molded pieces are heated to 8500 ° C for 2 hours. 900 ° C calcined, pulverized moist in a liner ball mill and dried. The dry product * that Containing a small amount of distilled water is under a pressure of 1000 kg / cm² pressed into disks of 8 mm in diameter and 2 mm in thickness. The pressed discs are fired for 1 hour at 11900 C to 12500 C. Sintered ceramic products are polished on both sides to a thickness of 0.4 mm. For training clay The polished disk is using electrodes on both sides. Silver color plated and burned at 6000 0. For polarization, the samples are placed in a silicone bath immersed at 1000 C, applied with a direct voltage of 15 kV / mm for 1 hour and cooled to room temperature within 30 minutes in an electric field. the dielectric and piezoelectric properties of the polarized samples are measured and listed in Tables 1 and II.
Die Nummern der Proben in den Tabellen I und II und die Bereiche der Zusammensetzung der Massen der Erfindung sind in den Figuren 1 und 2 gezeigt. Zusammensetzungen, die durch das Polygon ABCDEF in den Figuren 1 und 2 definiert sind, haben die oben. beschriebenen und im einzelnen in den Tabellen I und II gezeigten Eigenschaften. Bei keramischen Massen, die mehr als 62,5 Mol-% Pb(Ni1/3Nb2/3)O3 oder mehr als 60 Mol-% Pb(Co1/3Nb2/3)O3 enthalten, ist die Piezoelektrizität schwach und der planare Kopplungskoeffizient klein. Bei Massen, die weniger als 2,5 Mol Pb(Ni1/3Nb2/3)O3 oder weniger als 2,0 Mol-% Pb(Co1/3Nb2/3)O3 enthalten, sind die piezoelektrischen Eigenschaften ungenügend. The sample numbers in Tables I and II and the ranges the composition of the compositions of the invention are shown in FIGS. Compositions defined by the polygon ABCDEF in Figures 1 and 2 are have the above. and shown in detail in Tables I and II Properties. For ceramic masses that are more than 62.5 mol% Pb (Ni1 / 3Nb2 / 3) O3 or contain more than 60 mol% of Pb (Co1 / 3Nb2 / 3) O3, the piezoelectricity is weak and the planar coupling coefficient is small. For masses less than 2.5 moles Pb (Ni1 / 3Nb2 / 3) O3 or less than 2.0 mol% of Pb (Co1 / 3Nb2 / 3) O3 are the piezoelectric properties insufficient.
Andererseits können Massen, die im Falle von Pb(Ni1/3Nb2/3)O3 75,0 Mol-% oder mehr Mol-% PbTiO3 oder imi Falle von Pb(Co1/3Nb1/3)O3 60,0 Mol-% oder mehr Mol-% PbTiO3 enthalten, nicht zu keramischen Erzeugnissen gesintert werden. Ferner weisen Massen, die im Falle von Pb(Ni1/3Nb2/3)O3 87,5 Mol-% oder mehr Mol-% oder im Falle von Pb(Co1/3Nb2/3)O3 80,0 Mol-% oder mehr Mol-% PbZrO3 enthalten, bei Raumtemperatur nur eine schwache Piezoelektrizität auf. On the other hand, masses which in the case of Pb (Ni1 / 3Nb2 / 3) O3 can be 75.0 Mol% or more mol% of PbTiO3 or in the case of Pb (Co1 / 3Nb1 / 3) O3 60.0 mol% or contain more mol% PbTiO3, cannot be sintered into ceramic products. Furthermore, masses which, in the case of Pb (Ni1 / 3Nb2 / 3) O3, are 87.5 mol% or more mol% or in the case of Pb (Co1 / 3Nb2 / 3) O3 contain 80.0 mol% or more mol% of PbZrO3, only weak piezoelectricity at room temperature.
Die Tabellen 1 und II zeigen die keramischen Eingenschaften der Iteramischen Massen ohne oder mit dem Oxyd von Mn, Zn, Cr, Fe, Ta oder Th in einer Menge bis zu 3 Gew.-% der Zusammensetzung des maßgeblichen ternären Systems. Der Zusatz von Oxyd zu den Grundkomponenten verringert augenscheinlich ihren Resonanzwiderstand in einem wesentlichen Ausmaß. Der Zusatz bewirkt auch eine Erhöhung des mechanischen Gütefaktors und eine Verbesserung ihres planaren Kopplungskoeffizienten. Der Zusatz verringert weiterhin die Veränderung ihrer Resonanzfrequenz mit der Temperatur. Der Zusatz von Manganoxyd fördert besonders die oben beschriebenen erwünschten Wirkungen. Tables 1 and II show the ceramic properties of the Iteramic Masses without or with the oxide of Mn, Zn, Cr, Fe, Ta or Th in an amount up to at 3% by weight of the composition of the relevant ternary system. The addition of Oxide to the basic components apparently reduces their resonance resistance to a substantial extent. The addition also causes an increase in the mechanical Figure of merit and an improvement in their planar coupling coefficient. The addition further reduces the change in their resonance frequency with temperature. The addition of manganese oxide particularly promotes the desired effects described above.
Figur 3 zeigt die Temperaturveränderung der Dielektrizitätskonstanten
von keramischen Massen gemäß der Erfindung mit eines 2usatz
von
MnO2. Aus Figur 3 sieht man, daß keramische Massen gemäß der Erfindung eine relativ
hohe Curietemperatur haben. Fast alle keramischen Massen gemäß der Erfindung weisen
einen großen planaren Kopplungskoeffizienten auf, und insbesondere weisen die im
Bereich der morphotropischen Übergangsgrenze hohe Werte von 50 % bis 55 % auf,
Tabelle
I
Tabelle I (Forts.)
Tabelle II (Forts.)
Tabelle II (Forts.)
Tabelle II (Forts.)
Claims (1)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19691926812 DE1926812A1 (en) | 1968-05-27 | 1969-05-27 | Piezoelectric ceramic mass used in manufacture of - wave filters and electromechanical converters |
Applications Claiming Priority (8)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP3591868 | 1968-05-27 | ||
JP6886068 | 1968-09-24 | ||
JP6886168 | 1968-09-24 | ||
JP6886268 | 1968-09-24 | ||
JP6886468 | 1968-09-24 | ||
JP6886368 | 1968-09-24 | ||
JP6885968 | 1968-09-24 | ||
DE19691926812 DE1926812A1 (en) | 1968-05-27 | 1969-05-27 | Piezoelectric ceramic mass used in manufacture of - wave filters and electromechanical converters |
Publications (1)
Publication Number | Publication Date |
---|---|
DE1926812A1 true DE1926812A1 (en) | 1970-02-05 |
Family
ID=27564408
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
DE19691926812 Pending DE1926812A1 (en) | 1968-05-27 | 1969-05-27 | Piezoelectric ceramic mass used in manufacture of - wave filters and electromechanical converters |
Country Status (4)
Country | Link |
---|---|
DE (1) | DE1926812A1 (en) |
FR (1) | FR2009956A1 (en) |
GB (1) | GB1275961A (en) |
SE (1) | SE359978B (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3767579A (en) * | 1971-02-25 | 1973-10-23 | Nippon Electric Co | Piezoelectirc ceramics |
-
1969
- 1969-05-23 FR FR6917020A patent/FR2009956A1/en active Granted
- 1969-05-23 GB GB26349/69A patent/GB1275961A/en not_active Expired
- 1969-05-23 SE SE07340/69A patent/SE359978B/xx unknown
- 1969-05-27 DE DE19691926812 patent/DE1926812A1/en active Pending
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3767579A (en) * | 1971-02-25 | 1973-10-23 | Nippon Electric Co | Piezoelectirc ceramics |
Also Published As
Publication number | Publication date |
---|---|
GB1275961A (en) | 1972-06-01 |
SE359978B (en) | 1973-09-10 |
FR2009956A1 (en) | 1970-02-13 |
FR2009956B1 (en) | 1974-09-20 |
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