USRE32449E - Ceramic body of zirconium dioxide (ZrO2) and method for its preparation - Google Patents

Ceramic body of zirconium dioxide (ZrO2) and method for its preparation Download PDF

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Publication number
USRE32449E
USRE32449E US06/821,650 US82165086A USRE32449E US RE32449 E USRE32449 E US RE32449E US 82165086 A US82165086 A US 82165086A US RE32449 E USRE32449 E US RE32449E
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oxide
mole
ceramic body
rare earth
yttrium
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US06/821,650
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Nils Claussen
Manfred Ruhle
Gunter Petzow
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Max Planck Gesellschaft zur Foerderung der Wissenschaften eV
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Max Planck Gesellschaft zur Foerderung der Wissenschaften eV
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/02Inorganic materials
    • A61L27/04Metals or alloys
    • A61L27/047Other specific metals or alloys not covered by A61L27/042 - A61L27/045 or A61L27/06
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/48Shaped 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
    • C04B35/486Fine ceramics
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/48Shaped 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
    • C04B35/486Fine ceramics
    • C04B35/488Composites
    • C04B35/4885Composites with aluminium oxide
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5025Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with ceramic materials
    • C04B41/5042Zirconium oxides or zirconates; Hafnium oxides or hafnates
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81Coating or impregnation
    • C04B41/85Coating or impregnation with inorganic materials
    • C04B41/87Ceramics
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00241Physical properties of the materials not provided for elsewhere in C04B2111/00
    • C04B2111/0025Compositions or ingredients of the compositions characterised by the crystal structure
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00836Uses not provided for elsewhere in C04B2111/00 for medical or dental applications

Definitions

  • Finely granular zirconium dioxide bodies partially stabilized with yttrium oxide, cerium dioxide and/or other rare earth oxides, and coarsely granular zirconium dioxide bodies partially stabilized with magnesium oxide or calcium oxide pertain to the polycrystalline ceramics which have the highest strengths and resistance to fracture which have been measured up to now. The chief reason for this lies in the tension-induced transformation of the tetragonal lattice modification to the monoclinic room-temperature modification.
  • bodies containing yttrium oxide are sintered, hot-pressed or hot-isostatically pressed ("hipped") usually with an yttrium oxide content between 1 and 6 mole-%, either in the tetragonal monophasic field or in the cubic/tetragonal two-phase region, at temperatures between 1400° and 1550° C.
  • Their structure then consists of a fine-grained (0.1-1.0 micrometer), tetragonal content (up to 100%) and somewhat coarser, cubic grains (1-10 micrometers) (3.5-6.0 mole-% for high yttrium oxide contents).
  • the bodies can contain aluminum oxide in larger amounts.
  • Zirconium oxide bodies containing magnesium oxide or calcium oxide are usually sintered in the cubic monophasic region at temperatures between 1690° and 1800° C.; they are therefore more coarse-grained (50 to 70 micrometers).
  • TZP Tetragonal Zirconia Polycrystals.
  • a bibliography on TZP ceramics is contained in the book, "Science and Technology of Zirconia II", Advances in Ceramics, Vol. 11, 1984) suitable for use in air only for application temperatures up to about 200° C., although such ceramics would offer substantial advantages for use in internal combustion engines.
  • This phenomenon would also be disadvantageous for use as a bioceramic (hip joint replacement).
  • the invention is based on it--that in sintered specimens which have been heat treated in a milieu rich in yttrium oxide, cerium oxide, magnesium oxide or calcium oxide, e.g., a powder bed of yttrium oxide or magnesium oxide, this degradation process does not occur, or occurs to a lesser degree.
  • the invention is therefore based on the problem of reducing or eliminating the above-described loss of strength or surface degradation in ceramic bodies of zirconium dioxide.
  • a ceramic body partially stabilized with yttrium oxide and/or cerium oxide and/or one or more rare earth oxides and/or magnesium oxide and possibly containing aluminum oxide which is characterized by being partially stabilized with 0.5 to 5 mole-% of yttrium oxide and/or 2 to 12 mole-% of magnesium oxide and/or calcium oxide and one or more rare earth oxides (e.g., cerium oxide), is 30 to 100% in the tetragonal lattice modification, and has in the surface region a content of yttrium oxide or rare earth oxide and/or magnesium oxide and/or calcium oxide, such that the body is covered by a thin layer that is mostly in the cubic lattice form or in a more highly stabilized tetragonal lattice form.
  • a partially stabilized cubic layer can be transformed by tempering (peak aging) at temperatures commonly used in PSZ (1100°-1420° C.) to a PSZ-like layer (i.e., cubic grains having tetragonal segregations).
  • thin surface layer in the sense of the invention, is to be understood to mean a layer with a thickness of 0.1 to 200 micrometers, preferably 0.3 to 30 micrometers.
  • the body on the basis of zirconium dioxide in accordance with the invention is prepared by firing it in a milieu which is rich in yttrium oxide, cerium oxide, magnesium oxide, calcium oxide and/or rare earth oxides.
  • the invention is explained hereinbelow on the basis of the use of yttrium oxide, cerium oxide, magnesium oxide and calcium oxide. It is to be understood, however, that it applies likewise to other rare earth oxides.
  • This surface stabilization or annealing is likewise advantageous for conventional zirconia ceramics partially stabilized with magnesium oxide or calcium oxide.
  • the ceramic body in accordance with the invention it is possible to set out either from the finished sintered or hipped ceramic or from a green body presolidified at relatively low temperature (e.g., room temperature).
  • the ceramic or the green body is now provided with a surface of yttrium oxide, cerium oxide, magnesium oxide, calcium oxide, etc., either in the form of a pressed-on layer of powder or of a slip containing yttrium oxide or magnesium oxide, which can be sprayed on, for example, or applied in the form of a bath for impregnating the surface.
  • the bodies thus treated are then fired or sintered at temperatures between 1000° and 1600° C., the length of the treatment being able to be between about 10 minutes and about 100 hours.
  • the desired surface stabilization is also achieved to special advantage by firing or sintering the ceramic or green body in a powder bed of yttrium oxide and/or cerium oxide and/or magnesium oxide and/or calcium oxide. Those conditions are preferred in which the desired diffusion is achieved in the shortest possible time, while at the same time achieving a PSZ-like layer.
  • the body can be performed either by mixing the oxides, or by wet chemical methods such as sol gel, coprecipitation, spray reaction of aqueous solutions, or from fine, homogeneous powders obtained by fusion and prealloyed with yttrium oxide, cerium oxide, magnesium oxide and/or calcium oxide, and then sintering or hipping, or sintered and then hipped, at temperatures generally between 1350° and 1550° C.
  • the finished ceramic is then, as mentioned above, coated with yttrium oxide, cerium oxide, magnesium oxide, calcium oxide, etc., or fired in a corresponding powder bed, until the surface layer enriched with yttrium, cerium, magnesium, or calcium oxide etc. is formed.
  • the body When a stabilizer-rich coating is applied to a green body, the body is commonly preformed at a low pressure, say of about 100 MPa, and then pressed again at higher pressure, e.g., 200 to 650 MPa. In most cases, however, the preferred method is the sintering of the pressed body or the firing of a finish-sintered and processed body in a powder bed containing magnesium oxide or yttrium oxide and/or cerium oxide.
  • the ceramic bodies of the invention in comparison to specimens prepared under otherwise equal conditions but without the above-described surface treatment, in a treatment for accelerated aging, consisting of four hours of firing at temperatures between 250° C. and 400° C. at steam pressures of 4 to 15 bar, show scarcely any effect.
  • the thin surface layer was produced by firing the ready-sintered samples in magnesium oxide, yttrium oxide, cerium oxide or calcium oxide powder, or by treatment with yttrium oxide powder or a zirconium powder containing at least 12 mole-% of yttrium oxide, the surface layer being pressed onto the zirconium oxide compacts stabilized by a small addition (0.5 to 5, preferably 2 to 4 mole-%) of yttrium oxide, or being applied as an aqueous suspension of powder and sintered.
  • a small addition 0.5 to 5, preferably 2 to 4 mole-%
  • This layer can also contain aluminum oxide for fining the grain. Presumably other rare earth oxides produce a similarly positive effect, as previously mentioned.
  • this layer represents primarily a thermally stable protection for TZP ceramics, but also for conventional zirconium oxide partially stabilized with magnesium or calcium (Mg-, Ca-PSZ).
  • Example 1 Samples of a powder which was prepared and treated as in Example 1, but contained only 2 mole-% of yttrium oxide by volume, were formed as in Example 1.
  • An aqueous suspension of yttria powder was applied to the cylindrical compacts and some of it penetrated into the surface pores; then the coated compacts (type I) were sintered at 1500° C. for 2 hours, and then subjected to the autoclaving described in Example 1, together with identical samples with no coating (type II).
  • type I showed only tetragonal and cubic X-ray reflections, but type II showed tetragonal and large monoclinic X-ray reflections which indicates the thermal degradation of the uncoated samples.
  • Example 1 Samples from the powder of Example 1 were isostatically pressed at a pressure of 100 MPa, and then sprayed with a suspension of 12 mole-% zirconia powder containing 12 mole-% of yttrium oxide (coating thickness approx. 40 to 200 micrometers), then pressed again isostatically at 630 MPa, and sintered as in Example 1. After the autoclaving treatment (as in Example 1), no thermal degradation of the surface could be detected.
  • Example 2 Samples in accordance with Example 2 were coated with the same suspension, but this time with the addition of 20% alumina by volume, and otherwise treated as in Example 1. Here, again, no degradation could be detected after the heat treatment in the autoclave.
  • Example 6 50 volume-percent of alumina powder (Pechinee Ugine Kuhlman, A6) [was added] to the powder from Example 1 and ground in the attrition mill as in Example 1.
  • Isostatically pressed cylinders (approx. 1 ⁇ 1 cm diameter) were sintered at 1500° C., some with (type I) and some without (type II) a slip of 50 wt.-% of yttrium oxide and 50 wt.-% of cerium oxide.
  • type I contained on the polished surface only tetragonal zirconium oxide plus aluminum oxide (measured by X-ray analysis), while type II additionally contained cubic forms.
  • the surface of type I had a high content of monoclinic zirconium oxide, while type II showed no measurable change.
  • a coprecipitated zirconia powder containing 2.2 mole-% of yttrium oxide was pressed isostatically at 620 MPa; the samples were then sintered in air for 2 hours at 1500° C.
  • the bodies thus prepared contained exclusively tetragonal grains of an average size of 0.4 micrometers (material type A).
  • a similarly made commercial material with 3 mole-% of yttrium oxide contained approximate 80% of tetragonal grains (approximately 0.4 micrometers) and approximately 20% cubic grains (about 5 micrometers) (material type B).
  • Material types A and B were subjected to an autoclave test with a steam pressure of 5 bar at 250° C. for 2 hours, and both types degrade greatly, i.e., show mostly monoclinic reflections at the surface; type A was even completely decomposed.
  • Types A and B were then fired each for 2 hours in powder beds of yttrium oxide, cerium oxide, titanium oxide, magnesium oxide and calcium oxide, at different temperatures.
  • the heat treatment temperatures and the results of the autoclave test that followed are listed in Table 1. From this it appears that, with the exception of titanium oxide, all the other oxides have a positive effect, especially at higher temperatures.
  • a firing in a magnesium oxide powder bed is effective even at relatively low temperatures (1120° C.).
  • Types A and B in the form of unsintered compacts, were sintered for 2 h at 1500° C. in powder beds of yttrium oxide, cerium oxide, calcium oxide and magnesium oxide (in air). The above-described autoclave test again showed no surface degradation.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Composite Materials (AREA)
  • Inorganic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Manufacturing & Machinery (AREA)
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US06/821,650 1983-06-16 1986-01-23 Ceramic body of zirconium dioxide (ZrO2) and method for its preparation Expired - Fee Related USRE32449E (en)

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DE3321857 1983-06-16
DE3321857 1983-06-16
DE3345659 1983-12-16
DE19833345659 DE3345659A1 (de) 1983-06-16 1983-12-16 Keramikkoerper aus zirkoniumdioxid (zro(pfeil abwaerts)2(pfeil abwaerts)) und verfahren zu seiner herstellung

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US06/619,939 Reissue US4525464A (en) 1984-06-12 1984-06-12 Ceramic body of zirconium dioxide (ZrO2) and method for its preparation

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