US3464785A - Process for producing ordered complex perovskite-type crystals with high dielectric constants - Google Patents

Process for producing ordered complex perovskite-type crystals with high dielectric constants Download PDF

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US3464785A
US3464785A US513735A US3464785DA US3464785A US 3464785 A US3464785 A US 3464785A US 513735 A US513735 A US 513735A US 3464785D A US3464785D A US 3464785DA US 3464785 A US3464785 A US 3464785A
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crystals
dielectric constants
high dielectric
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type crystals
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Salvatore F Galasso
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RTX Corp
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Definitions

  • Perovskite-type single crystals of the formula 'o.3a o.s7) s wherein A is barium or strontium and B is magnesium, calcium, zinc, nickel or cobalt are prepared by mixing powders of a compound yielding the oxide of A with Ta O and the B metal oxide and then mixing the powders with a flux of the formula AF wherein A is as defined above. The resulting mixture is heated to a temperature above the melting point of the flux and after holding for at least 0.5 hours is gradually cooled to effect crystal formation.
  • This invention relates in general to materials characterized by high, temperature-stable dielectric constants. It contemplates the production of ordered complex perovskite-type crystals with dielectric constants which are relatively unaffected thermally up to temperatures as high as 800 C.
  • capacitor compounds which are dielectnically temperaturestable, exhibit dielectric constants on the order of approximately 10.
  • ferroelectrics such as barium titanate, which possess dielectric constants several orders of magnitude larger than the usual capacitor compounds, are known to be temperature sensitive.
  • capacitor insulators displaying both high dielectric constants and reasonable thermal stability, particularly in the higher temperature ranges.
  • a further object of this invention is to provide ordered complex perovskite-type crystals characterized by high dielectric constants which are substantially independent of their environment up to temperatures of 800 C.
  • An additional object is to provide methods of producing crystals of high electrical resistivity from compounds identified by the formula A(B B )O particularly those characterized by the formula A(B Ta )O
  • FIGURE 1 is a graph of log resistivity versus temperature for a representative Ba(Mg Ta )O single crystal.
  • FIGURE 2 is a graph of dielectric constant versus temperature for a Ba(Mg Ta )O single crystal.
  • the perovskite structure is recognized in the art as that adopted by many ABOg-type compounds in which large A ions and oxygen ions form close-packed layers with small B ions in the octahedral holes between the oxygen ions. Investigations have been made of a large number of new compounds of the general formula A(B' B" )O where B and B are two different elements in the octahedrally coordinated cation position of the perovskite structure. Experiments have confirmed that many com- Patented Sept. 2, 1969 pounds indentified by the formula A(-B' B )O form in an ordered perovskite structure. Inorganic Chemistry, 2, 482 (1963).
  • A is a barium ion and B is a magnesium ion
  • this crystal is characterized by a dielectric constant of approximately 500 which is relatively independent of temperature over the above-mentioned temperature range. This was completely unexpected inasmuch as similar electrical resistivity measurements in powder compacts of substantially the same composition did not display equivalent electrical properties. While the exact reasons for the superior electrical properties of the crystal are not known, a comparison of the respective X-ray patterns associated with the various crystals showed that the perovskite pseudo-cells were less distorted in the crystal. It is postulated that the presence of a small amount of fluoride ion in the crystals produced, the fluoride ion being present in the flux in which the crystals were grown, is a contributing factor.
  • the preferred technique for growing crystals of the A(B Ta )O' type is as follows, the production of the Ba(Mg Ta )O crystals being specified for the sake of simplicity:
  • Reagent grade BaCO Ta O and MgO were dry-mixed in the approximate proportions to obtain stoichiometric compositions with the amount of fluoride flux as indicated in- Table II;
  • the fluoride flux, BaF was selected in the preparation of the-Ba(B' Ta )O3 type crystals, instead of the more commonly used KF, PbO- or P130- PbF fluxes, in order to minimize the amount of cation impurities introduced into the' crystals.
  • BaCOg was used in the preparation of the crystalsdiscussed, other compounds; such as Ba'NO from which barium oxide may be derived, are use'able in the process.
  • the mixtures were placed in 50ml. covered platinum crucibles and heated to a temperature approximately 100 C. above the meltingpointof. the flux. Soaking at temperature was'efiec'tedfor periods ranging from 0.5 to 8.5 hours, depending on the composition of the mixture.
  • the-crucibles and contained samples were gradually cooled over a temperature range of approximately 400 CI. and. the resulting crystals-Were mechanically extracted from the flux.
  • the specific soaking temperatures, soaking times, sample Weights, flux rates and cooling rates are given in' Table IT. While the tabled conditions represent the best of numerous experiments designed to increase the size of the crystals, it will be. understood that these conditions are representative only.
  • Crystals prepared in accordance with the abovedescribed' techniques were'nearly cubic in shape and varied in color from yellow to" green.
  • Selected crystals from each batch were analyzed using X-ray diffraction tech-- niques and photographs: were taken using a 57.3 min; radius Philips X-ray' camera and" high intensity copper Ka radiation, and the presence of ordering and cell sizes were determined.

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3951874A (en) * 1974-07-10 1976-04-20 International Telephone And Telegraph Corporation Method for preparing electron emissive coatings
US4121941A (en) * 1977-11-10 1978-10-24 Matsushita Electric Industrial Co., Ltd. Low microwave loss ceramics and method of manufacturing the same
US4216103A (en) * 1978-04-13 1980-08-05 Tdk Electronics Co., Ltd. High dielectric constant type ceramic composition consisting essentially of Pb(Fe1/2 Nb1/2)O3 -Pb(Mg1/3 Ta2/3)O3
US4216102A (en) * 1978-04-10 1980-08-05 Tdk Electronics Co., Ltd. High dielectric constant type ceramic composition consisting essentially of Pb(Fe1/2 Nb1/2)O3 -Pb(Mg1/3 Nb2/3)O3
US4287075A (en) * 1978-04-17 1981-09-01 Tdk Electronics Co., Ltd. High dielectric constant type ceramic composition consisting essentially of Pb(Fe1/2 Nb1/2)O3 -Pb(Mg1/3 Nb2/3)O3 -Pb(Mg1/2 W1/2)O3
EP0095338A1 (en) * 1982-05-26 1983-11-30 Nippon Hoso Kyokai Low-loss microwave dielectric material
DE3331610A1 (de) * 1982-09-06 1984-03-08 Murata Manufacturing Co., Ltd., Nagaokakyo, Kyoto Dielektrische keramische zusammensetzung
US4829032A (en) * 1986-01-16 1989-05-09 Ngk Spark Plug Co., Ltd. Dielectric ceramic composition
US4853199A (en) * 1987-01-08 1989-08-01 Matsushita Electric Industrial Co., Ltd. Method for producing crystalline complex perovskite compounds
US6593263B2 (en) * 2000-08-24 2003-07-15 Amotech Co., Ltd. Method for preparing dielectric ceramic compositions
CN112707728A (zh) * 2021-01-27 2021-04-27 南方科技大学 微波介质陶瓷材料及其制备方法和电子器件

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1223744B (de) * 1962-03-05 1966-08-25 Max Schmidt Verfahren zum Herstellen von zylinderfoermigen Verpackungsbehaeltnissen und zum Fuellen derselben mit Dekorationshohlkoerpern, z. B. Christbaumkugeln od. dgl.
DE3530571A1 (de) * 1985-08-27 1987-03-05 Siemens Ag Dielektrisches keramikmaterial
DE3530570A1 (de) * 1985-08-27 1987-03-05 Siemens Ag Dielektrisches keramikmaterial

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2812234A (en) * 1953-11-23 1957-11-05 Sprague Electric Co Titanate compositions
US3340074A (en) * 1964-03-16 1967-09-05 Corning Glass Works Barium titanate materials

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2812234A (en) * 1953-11-23 1957-11-05 Sprague Electric Co Titanate compositions
US3340074A (en) * 1964-03-16 1967-09-05 Corning Glass Works Barium titanate materials

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3951874A (en) * 1974-07-10 1976-04-20 International Telephone And Telegraph Corporation Method for preparing electron emissive coatings
US4121941A (en) * 1977-11-10 1978-10-24 Matsushita Electric Industrial Co., Ltd. Low microwave loss ceramics and method of manufacturing the same
US4216102A (en) * 1978-04-10 1980-08-05 Tdk Electronics Co., Ltd. High dielectric constant type ceramic composition consisting essentially of Pb(Fe1/2 Nb1/2)O3 -Pb(Mg1/3 Nb2/3)O3
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GB1156199A (en) 1969-06-25
FR1509999A (fr) 1968-01-19
DE1671173B2 (enrdf_load_stackoverflow) 1971-01-28
DE1671173A1 (de) 1970-02-19

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