USRE36573E - Method for producing thick ceramic films by a sol gel coating process - Google Patents
Method for producing thick ceramic films by a sol gel coating process Download PDFInfo
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- USRE36573E USRE36573E US08/938,996 US93899697A USRE36573E US RE36573 E USRE36573 E US RE36573E US 93899697 A US93899697 A US 93899697A US RE36573 E USRE36573 E US RE36573E
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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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62218—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining ceramic films, e.g. by using temporary supports
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
- C23C18/1208—Oxides, e.g. ceramics
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1225—Deposition of multilayers of inorganic material
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1229—Composition of the substrate
- C23C18/1241—Metallic substrates
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1254—Sol or sol-gel processing
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1262—Process of deposition of the inorganic material involving particles, e.g. carbon nanotubes [CNT], flakes
- C23C18/127—Preformed particles
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1295—Process of deposition of the inorganic material with after-treatment of the deposited inorganic material
Definitions
- This invention relates to the production of thick ceramic films, including composite films, on selected substrates, using a sol-gel coating technique. More particularly this invention relates to a technique for depositing polycrystalline ceramic films such as lead zirconate titanate and partially stabilized zirconia, in thicknesses greater than 10 ⁇ m.
- Ceramic coatings can be prepared by thermal or plasma spraying and physical vapour deposition (PVD) techniques.
- PVD physical vapour deposition
- a bulk powder is passed through a plasma and directed towards a substrate where it cools on contact. Films up to 10 mm thick can be produced in this way but usually need post-deposition heating as the deposited film tends to be porous (10% porosity is considered good).
- Another drawback of the plasma spray technique is that only line of sight geometries can be successfully coated.
- PVD expensive vacuum systems are required to coat high quality ceramic films of less than 10 ⁇ m. In addition this technique is also limited to line of sight geometries.
- sol-gel processing An alternative method, which has gained considerable ground and credibility in recent years, is sol-gel processing.
- Organo-metallic precursor compounds of the desired ceramic oxides are mixed and dissolved in a suitable solvent.
- the resultant solution is then hydrolysed to form a structured solution or gel containing organo-metallic polymers or macroclusters.
- Additives can be added to control the viscosity and surface tension of the sol gel solution.
- Films are prepared by either spin, dip or spray coating or painting onto an appropriate substrate.
- the coated substrate is then fired to remove the organic material and a post-fire heating step is usually performed to fully develop the final ceramic structure.
- the sol gel process has several advantages over other fabrication methods. It is simple, more economically feasible and permits coating of complex geometries, not necessarily line of sight.
- Ceramic films up to about 0.5 ⁇ m can be deposited in a single layer but films up to about 3.0 ⁇ m have been produced using a complex vacuum controlled firing treatment. Thicker films, up to about 10 ⁇ m in thickness have been produced by successive coatings in 0.1 ⁇ m layers. Clearly a 10 ⁇ m film made 0.1 ⁇ m at a time is a very time consuming and laborious process. In order to exploit the desired properties of the ceramic, it is essential that the ceramic film should be crack-free. Sol Gel films are, however, very susceptible to substrate interaction, defects and stresses within the film. Generally the thinner the film the lower the internal stresses and the number of defects.
- Solvents and organics can escape from 0.1 ⁇ m layers relatively easily but for thicker layers this is not so resulting in defects which can act as nucleation centres for crack propagation.
- Sol gel films are also substrate dependent and most films are limited to metallized silicon or other highly polished substrates. Conventional sol gel technology cannot, therefore, be used to produce thick, large area sol gel films.
- An object of the present invention is to provide an improved method for applying adherent ceramic films to metallic substrates in thicknesses greater than 5 ⁇ m and at least up to 200 ⁇ m without cracking.
- Another object is to provide an improved sol-gel process for producing polycrystalline ceramic coatings on a wide range of substrates.
- a process for producing a crack-free crystalline film selected from stabilized zirconia .[.or.]. .Iadd.and .Iaddend.titania on a substrate selected from aluminum foil and stainless steel comprising:
- sol gel mixture selected from titania and zirconia and a solution of a metal salt with up to 90% by weight of yttria or ceria stabilized zirconia powder or pure titania powder in a size range between .1 and 10 microns so as to produce a stable dispersion.
- sol-gel processing techniques first require the preparation of an organo-metallic solution of the desired ceramic oxide precursors in an organic solvent, followed by hydrolysation and pyrolysation to remove the organic phase. Similar techniques are followed in the present invention with the important distinction that the primary organo-metallic solution is mixed with ceramic particles and subjected to ultrasonic mixing to form a sol gel based paint which can be deposited on simple or complex geometry substrates by either spin, dip or spray coating or painting, followed by hydrolysation, pyrolysation and heating in air. Typical formulations are described below and it is emphasized that these formulations are not critical but may be varied widely.
- Zirconium propoxide, acetylacetone and methoxyethanol were mixed in a molar ratio of 1:1:4. Water, glycerol and ethylene glycol were then added to adjust viscosity.
- Ceramic powders were added to the solutions (a)-(f) above and mixed ultrasonically to provide uniform stable dispersions.
- Ceramic powders may be selected from a wide range of materials, including alumina, silica titania, zirconia, silicon carbide, titanium carbide and PZT. Preferred ceramic powders in selected sol gel solutions are shown in Table 1 below.
- the paints prepared above may be applied to any suitable substrate either by dipping, spin coating or spraying or painting as any conventional sol gel is used.
- Planar, coaxial and complex geometry substrates can be readily coated. Examples of these include metals, inside and outside of tubes, complex objects such as steel nuts and orthopaedic implants.
- Films of greater than 5 ⁇ m and up to at least 200 ⁇ m in thickness can be applied by spin coating multiple layers. A single layer up to 6 ⁇ m in thickness can be deposited without cracking.
- the ceramic/sol gel paint Following deposition of the ceramic/sol gel paint on the substrate, it is heated in air to a temperature between 400° C. and 700° C., depending upon the particular substrate and coating, for a period of 1 to 30 minutes so as to remove the organic materials and form the oxide compounds. After the first firing, additional layers may be deposited and fired until the desired thickness has been obtained. Thereafter, the films may be heated at a temperature between 400° C. and 1000° C., preferably about 550° C. for a period of up to about 4 hours, preferably about 1 hour.
- Titania films using both the calcium zirconate and calcium titanate sol gel could be deposited onto stainless steel and fired at 700° C. and could be heated at 900° C. However upon cooling from 900° C. to room temperature, the substrate began to bow and the titania coating began to "pop off". The failure of the titania film is believed due to the thermal expansion mismatch between the ceramic and the substrate. Zirconia films were prepared in similar manner as the titania but did not fail. Therefore, it appears that zirconia does not suffer from thermal expansion mismatch as greatly as the titania.
- YSZ and CSZ films were prepared using a calcium modified zirconia sol gel solution and were deposited onto soft steel, stainless steel, inconel and carbon/carbon composite. Spin coated films produced excellent results and provided films which were adherent. The surface morphology of these coatings was rough and irregular. However, when electroded with silver paint the films were found to be insulating indicating that they are pin hole and crack-free. Polishing the sample with 0.3 ⁇ m diamond paste resulted in smooth and shiny surface on the ceramic. Scanning electrode microscopy observation of the polished sample did not disclose any holes, pores or defects in the sample. Film thicknesses were determined by mounting the sample edgewise in epoxy resin, polishing the edge and comparing the sample to a grid within an optical microscope.
- the film thickness of a 20 layer coating was 60 ⁇ m.
- CSZ films (20 layers) were prepared by spin coating onto a 2 cm by 3.5 cm inconel coupon, firing at 700° C. and heated overnight at 900° C. The sample was then thermal cycled 10 times from room temperature to 1300° C. The sample showed no delamination or spalling after the test.
- YSZ and CSZ films were successfully coated onto a variety of substrates, these include soft steel, stainless steel, inconel and carbon/carbon composites coupons and soft steel, stainless steel and inconel rods.
- the PZT films produced according to the present invention find industrial application in the production of integrated sensor and actuator devices in which the piezoelectric device and semiconductor circuitry are deposited on the same chip to form so called “smart structures".
- Piezoelectric PZT films deposited on optical fibres may be used as integrated optical phase modulators or to produce steerable optical fibres.
- the zirconia and alumina coatings have structural applications. Examples of these are:
- Thermal barrier coatings where the ceramic is used to provide a thermal gradient between the surface of the film and the metal substrate. This allows metallic components in turbine engines and heat exchanger to be operated at high temperatures.
- Films were deposited onto planar substrates by spin coating and subsequently fired at 400° C. Thicker films were achieved by repeating the sequence until the desired thickness was obtained. The films were then heated at 650° C. for 1 hour. Fibres and wires were coated using an automated dipping system.
- PZT films deposited onto planar substrates produced crack free films that were 9-60 ⁇ m thick.
- the films were found insulating indicating that they were pinhole free. Under observation by scanning electron microscopy, the films appeared .Iadd.to be .Iaddend.dense.
- the dielectric and piezoelectric properties obtained for these films was comparable to bulk material. In fact these films were found to be of sufficient quality to produce piezoelectric cantilevers which were 4 cm long and 0.5 cm wide and, at the fundamental resonance frequencies, vibrate with deflections observable with naked eye (0.8 mm).
- PZT coatings on fibres and wires achieved coatings of 10-30 ⁇ m in thickness. These coatings were also of high enough quality to produce an "In-line Optic Phase Modular" device where the PZT was 30 ⁇ m thick.
- the development of zirconia and titania films was carried out in two stages.
- the first stage involved the fabrication of zirconia and titania films without adding inorganic additives to the sol gel solution and the second investigated the use of inorganic additives to improve both the distribution of the particles within the film and its adhesion to substrates.
- Titania and zirconia sol gel mixtures were prepared by mixing 4 g of either zirconium propoxide or titanium isopropoxide with 3 g acetic acid, 2 g DDW, 0.5 g polyethylene glycol and 0.5 g glycerol. Either 4 g of yttria partially stabilized zirconia or titania powder was added to the appropriate sol gel solution and the mixture sonified for at least 5 min. The films were then deposited onto aluminium foil and stainless steel coupons by spin coating and firing at 500° C. Films heated above 600° C. tended not to adhere to the substrate and could be rubbed off.
- Modified sol gel mixtures were made by adding a metal salt.
- 2 g of a metal salt (either lead nitrate, lead acetate, calcium nitrate, calcium acetate, strontium acetate, strontium nitrate cerium acetate, cerium nitrate and yttrium acetate and yttrium nitrate) was dissolved in 4 g of acetic acid.
- acetic acid 8 g of zirconium propoxide or titanium isopropoxide or a mixture of zirconium propoxide (6 g) and titanium isopropoxide (4 g) was added along with 2.5 g DDW, 1 g polyethylene glycol and 1 g glycerol.
- Ceramic powder (4 g), either yttria or ceria partially stabilized zirconia (YSZ or CSZ) or titania was added to the solution and sonified for at least 5 min. The films were then deposited on to stainless steel coupons as in the previous example and were found to have excellent adhesion. Without wishing to be bound by this explanation it is believed that the added metal cation suppresses the disruptive tetragonal to monoclinic phase change which occurs in zirconia. Sol gel zirconia undergoes a number of phase changes as a result of changes in temperature. Conventional sol gel films (ones prepared without the addition of ceramic powders) are amorphous when deposited at room temperatures. The material becomes tetragonal when heated to between 400-600° C.
- This phase persists when the material is cooled back down to room temperatures. However, if the film is heated above 600° C. and cooled back to room temperature, the monoclinic phase is also present in the material. This monoclinic phase is 5 volume % larger than the tetragonal. The corresponding variations in the volume throughout the multiphase material causes the ceramic to break apart (resulting in poor adhesion). However, when metal cations such as calcium, magnesium, cerium or yttrium are added to conventional zirconia sol gel solutions, this tetragonal to monoclinic phase transformation is suppressed and the integrity of the ceramic body is maintained throughout the temperature range below 2300° C.
- metal cations such as calcium, magnesium, cerium or yttrium
- metal cations discussed calcium is preferred because of its high solubility in all of the solvents used to make the sol gel solutions.
- Other metal cations, while also capable of suppressing the tetragonal to monoclinic phase change, are not as soluble as calcium and are more difficult to work with.
- Modified sol gel dispersions of CSZ and YSZ were either spin or dip coated onto soft steel, stainless steel, Inconel® and carbon/carbon composite.
- the dispersions were prepared by dissolving 2 g of calcium nitrate in 4 g of acetic acid. To the resulting solution 8.5 g of zirconium propoxide, 2.5 g DDW and 1 g each of polyethylene glycol and glycerol. Ceramic powder (4 g) was added as before. Coatings on soft steel were fired and heated for at least 8 hours at 500° C. Coatings on stainless steel and Inconel® were fired at 700° C. and heated for at least 8 hours at 700° C. and 900° C. respectively. Coatings on carbon/ carbon composites were fired at 450° C. Rods of carbon steel, stainless steel and inconel were dip coated and fired and heated in a manner similar to the coupons.
- Calcium zirconate coatings were deposited onto stainless steel coupons by spin coating, firing at 700° C. and heating at 900° C. for at least 8 hours.
- the calcium zirconate sol gel was prepared by dissolving propoxide (8.5 g), DDW (2.5 g) and 1 g each of polyethylene glycol and glycerol. Calcium zirconate powder (4 g) was added to the resulting solution and dispersed by sonifying for at least 5 minutes.
- Dielectric coatings have been fabricated by dip and spin coating multiple layers of either ceria stabilized zirconia (CSZ) or alumina films onto alumina substrates. These coatings which range from 10-60 ⁇ m in thickness have withstood RF voltages of up to 3.2 kV.
- CSZ ceria stabilized zirconia
- CSZ films have been deposited on stainless and carbon steel nuts by painting multiple layers and heating to 500° C. for 24 hours.
- a 11/2 inch diameter carbon steel tube was coated on both the inside and outside with CSZ by dip coating multiple layers.
- the fired coating improved extrusion speed and surface equality of polymers produced, as compared to uncoated capillary dies.
- High frequency transducers which exhibit thickness mode resonance in the frequency range 35-60 MHz have been fabricated by depositing PZT coatings on aluminum substrates.
- Silicon carbide (4 g) (1-10 micron, Johnson Mathey) as added to a solution of Ca(NO 3 ) 2 (2 g), acetic acid (3 g), zirconium isopropoxide (8 g), water (1 g), glycerol (1 g) and poly(ethylene glycol)(1 g).
- Ten layers were deposited on a silicon substrate by spin coating and fired at 600° C. between each coating. The film was then heated overnight at 600° C. The resulting films were adherent and SEM analysis showed them to be dense and approximately 12-15 ⁇ m in thickness.
- Ten layers were deposited on a silicon substrate by spin coating and fired at 600° C. between each coating. The film was then heated overnight at 600° C. The resulting films were adherent and SEM analysis showed them to be dense and approximately 12 ⁇ m in thickness.
- a silicon carbide paint and titanium nitride paint were prepared as in Examples 11 and 12 respectively. Alternating layers were applied by spin coating and fired at 600° C. between each coating. The film was then heated overnight at 600° C. The resulting films were adherent and SEM analysis showed them to be dense and approximately 12 ⁇ m in thickness.
Abstract
Description
TABLE 1 ______________________________________ Nickel Zinc Powder PZT.sup.1 Zirconia.sup.2 Alumina.sup.3 Silica.sup.4 Ferrite.sup.5 Titania.sup.6 ______________________________________ (Yttria) Yes Yes Yes Yes No Yes Zirconia (Ceria) Yes Yes Yes Yes No Yes Zirconia PZT Yes Yes Yes Yes No No Alumina Yes Yes Yes Yes No No Titania Yes Yes Yes Yes No Yes Calcium Yes Yes No No No Yes Zirconate Silica No Yes Yes Yes No No Silicon No Yes Yes No No No Carbide Titanium No Yes Yes No No No Nitride Calcium No Yes Yes No No No Hydroxy- apatite Nickel No No No No Yes No Zinc Ferrite ______________________________________
Claims (17)
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US08/938,996 USRE36573E (en) | 1995-03-22 | 1997-09-26 | Method for producing thick ceramic films by a sol gel coating process |
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US08/409,127 US5585136A (en) | 1995-03-22 | 1995-03-22 | Method for producing thick ceramic films by a sol gel coating process |
US08/938,996 USRE36573E (en) | 1995-03-22 | 1997-09-26 | Method for producing thick ceramic films by a sol gel coating process |
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US08/409,127 Ceased US5585136A (en) | 1995-03-22 | 1995-03-22 | Method for producing thick ceramic films by a sol gel coating process |
US08/938,996 Expired - Lifetime USRE36573E (en) | 1995-03-22 | 1997-09-26 | Method for producing thick ceramic films by a sol gel coating process |
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EP (1) | EP0815285B1 (en) |
JP (1) | JPH11502262A (en) |
KR (1) | KR100390037B1 (en) |
AT (1) | ATE204617T1 (en) |
AU (1) | AU4617496A (en) |
CA (1) | CA2213209C (en) |
DE (1) | DE69614673T2 (en) |
DK (1) | DK0815285T3 (en) |
ES (1) | ES2159716T3 (en) |
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Cited By (15)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6426114B1 (en) | 2000-05-02 | 2002-07-30 | The University Of British Columbia | Sol-gel calcium phosphate ceramic coatings and method of making same |
US6432238B1 (en) * | 1998-12-30 | 2002-08-13 | Samsung Electro-Mechanicals Co., Ltd. | Method for fabricating piezoelectric/electrostrictive thick film using seeding layer |
US20020127335A1 (en) * | 2001-03-12 | 2002-09-12 | Lee Yong-Kyun | Method for preparing and forming a thick coating of PZT using sol-gel process |
WO2002072495A3 (en) * | 2001-03-09 | 2002-11-14 | Datec Coating Corp | Sol-gel derived resistive and conductive coating |
US6770325B2 (en) | 2000-05-19 | 2004-08-03 | The University Of British Columbia | Process for making chemically bonded composite hydroxide ceramics |
US20040247791A1 (en) * | 2003-06-03 | 2004-12-09 | United States Department Of Energy | Method for preparing nanocrystalline ceramic thin films |
US20040258611A1 (en) * | 2003-06-23 | 2004-12-23 | Mark Barrow | Colloidal composite sol gel formulation with an expanded gel network for making thick inorganic coatings |
US20060127294A1 (en) * | 2004-12-14 | 2006-06-15 | Feng-Yun Wang | New method for preparing pure, thermally stable and high surface area ceria |
US20060134496A1 (en) * | 2004-12-13 | 2006-06-22 | Applied Materials, Inc. | Fuel cell conditioning layer |
US20060293164A1 (en) * | 2003-02-03 | 2006-12-28 | Reinhard Nesper | Method for production of a b/n/c/si ceramic from a borazine precursor, ceramics made by said method and use of the ceramic made by said method |
WO2007094019A1 (en) * | 2006-02-17 | 2007-08-23 | Nm Tech Ltd. Nanomaterials And Microdevices Technology | A method for preparing nanocrystalline transparent films of tungsten oxide |
US20070224359A1 (en) * | 2006-03-22 | 2007-09-27 | Burin David L | Method for preparing strain tolerant coatings by a sol-gel process |
US20070228033A1 (en) * | 2004-05-19 | 2007-10-04 | Koninklijke Philips Electronics N.V. | Layer for Use in a Domestic Appliance |
US20080078503A1 (en) * | 2006-10-03 | 2008-04-03 | National University Corporation Tohoku University | Mechanical pump operating well for a long term and method of manufacturing the same |
WO2013007254A1 (en) | 2011-07-08 | 2013-01-17 | Scheer Heizsysteme & Produktionstechnik Gmbh | Thick ceramic coating |
Families Citing this family (73)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US7166470B2 (en) * | 1994-10-18 | 2007-01-23 | Symyx Technologies, Inc. | Formation of combinatorial arrays of materials using solution-based methodologies |
US5585136A (en) * | 1995-03-22 | 1996-12-17 | Queen's University At Kingston | Method for producing thick ceramic films by a sol gel coating process |
US5955140A (en) * | 1995-11-16 | 1999-09-21 | Texas Instruments Incorporated | Low volatility solvent-based method for forming thin film nanoporous aerogels on semiconductor substrates |
JP3327149B2 (en) * | 1995-12-20 | 2002-09-24 | セイコーエプソン株式会社 | Piezoelectric thin film element and ink jet recording head using the same |
US6117294A (en) | 1996-01-19 | 2000-09-12 | Micron Technology, Inc. | Black matrix material and methods related thereto |
US6670050B2 (en) * | 1997-05-30 | 2003-12-30 | Honeywell International Inc. | Titanium-based heat exchangers and methods of manufacture |
US6165553A (en) * | 1998-08-26 | 2000-12-26 | Praxair Technology, Inc. | Method of fabricating ceramic membranes |
US6977095B1 (en) * | 1997-10-01 | 2005-12-20 | Wright Medical Technology Inc. | Process for producing rigid reticulated articles |
DE19817482C2 (en) * | 1998-04-20 | 2003-07-03 | Fraunhofer Ges Forschung | Process for producing thick layers of ferroelectric ceramics |
IT1306214B1 (en) * | 1998-09-09 | 2001-05-30 | Gel Design And Engineering Srl | PROCESS FOR THE PREPARATION OF THICK GLASS FILMS OF SILIC OXIDE ACCORDING TO THE SOL-GEL TECHNIQUE AND THICK FILMS SO OBTAINED. |
US20020024270A1 (en) * | 1998-10-14 | 2002-02-28 | Sumsung Electro-Mechanics Co. | Piezoelectric/electrostrictive film element formed at low temperature using electrophoretic deposition |
US6251473B1 (en) | 1999-05-12 | 2001-06-26 | The Trustees Of The University Of Pennsylvania | Preparation of ceramic thin films by spray coating |
US6409813B1 (en) | 1999-05-18 | 2002-06-25 | Durga P. Beesabathina | Glass-release coating, coating process, and coated parts for manufacturing glass |
US6284682B1 (en) * | 1999-08-26 | 2001-09-04 | The University Of British Columbia | Process for making chemically bonded sol-gel ceramics |
US6750023B2 (en) * | 1999-09-02 | 2004-06-15 | Corning Incorporated | Porous inorganic substrate for high-density arrays |
DE19943789A1 (en) * | 1999-09-13 | 2001-03-15 | Fraunhofer Ges Forschung | Process for the deposition of zirconium oxide layers using soluble powders |
FR2801135B1 (en) * | 1999-11-12 | 2002-02-08 | Univ Claude Bernard Lyon | PROCESS FOR PRODUCING A TRANSMISSION CATHODE USING THE SOL-GEL TECHNIQUE AND CATHODE OBTAINED BY SUCH A METHOD |
US6627571B1 (en) | 2000-03-01 | 2003-09-30 | Symyx Technologies, Inc. | Method and system for the situ synthesis of a combinatorial library of supported catalyst materials |
EP1156024A1 (en) * | 2000-05-19 | 2001-11-21 | "VLAAMSE INSTELLING VOOR TECHNOLOGISCH ONDERZOEK", afgekort "V.I.T.O." | Composite ceramic precursors and layers |
US20040161789A1 (en) * | 2000-08-30 | 2004-08-19 | Tanner Cameron W. | Porous inorganic substrate for high-density arrays |
FR2813602B1 (en) * | 2000-09-07 | 2003-09-26 | Armines Ass Pour La Rech Et Le | COATING COMPOSITION AND METHOD FOR COATING A SURFACE OF A SUBSTRATE |
KR100379771B1 (en) * | 2000-10-06 | 2003-04-11 | 한국과학기술연구원 | Fabricating Method of Ferroelectric Thick Film Using Polymer Composites |
KR100406646B1 (en) * | 2000-10-07 | 2003-11-21 | 한국과학기술연구원 | Fabricating Method of Thick Film Using Compound of Relaxer Ferroelectric Ceramics and Polymer Matrix |
US20040219423A1 (en) * | 2001-04-27 | 2004-11-04 | Tunney Cathal Joseph | Metal-supported solid electrolyte electrochemical cell and multi cell reactors incorporating same |
US6544589B2 (en) * | 2001-08-20 | 2003-04-08 | Northrop Grumman Corporation | Method of controlling drying stresses by restricting shrinkage of ceramic coating |
EP1340541A1 (en) | 2002-02-28 | 2003-09-03 | Corning Incorporated | Structured catalysts incorporating thick washcoats and method of preparation thereof |
DE10225972B3 (en) * | 2002-06-11 | 2004-03-04 | Fachhochschule Kiel | Process for spin coating a thick ceramic layer using a sol-gel process |
CA2499559A1 (en) * | 2002-10-03 | 2004-04-15 | Alberta Research Council Inc. | Protective ceramic coating |
EP1566078B1 (en) | 2002-11-22 | 2006-09-13 | Koninklijke Philips Electronics N.V. | Sol-gel based heating element |
US6936561B2 (en) | 2002-12-02 | 2005-08-30 | Corning Incorporated | Monolithic zeolite coated structures and a method of manufacture |
US6964201B2 (en) * | 2003-02-25 | 2005-11-15 | Palo Alto Research Center Incorporated | Large dimension, flexible piezoelectric ceramic tapes |
US6895645B2 (en) * | 2003-02-25 | 2005-05-24 | Palo Alto Research Center Incorporated | Methods to make bimorph MEMS devices |
US7089635B2 (en) | 2003-02-25 | 2006-08-15 | Palo Alto Research Center, Incorporated | Methods to make piezoelectric ceramic thick film arrays and elements |
DE10322701B4 (en) * | 2003-05-20 | 2006-12-28 | Humboldt-Universität Zu Berlin | Sample carriers using a porous film comprising metal oxide particles, methods for producing a sample carrier, use of the sample carrier and methods for the selective detection of phosphorylated / sulfated biopolymers, in particular peptides / proteins |
JP4825955B2 (en) * | 2003-06-13 | 2011-11-30 | 独立行政法人産業技術総合研究所 | Biological implant material and method for producing the same |
US7300702B2 (en) * | 2003-08-18 | 2007-11-27 | Honeywell International, Inc. | Diffusion barrier coating for Si-based components |
DE10355160B4 (en) * | 2003-11-26 | 2008-04-03 | Schott Ag | Coated glass ceramic plate, method for its production and hob with such a glass ceramic plate |
EP1547675A1 (en) * | 2003-12-24 | 2005-06-29 | Corning Incorporated | Coated microstructures and methods of coating same |
FR2865219B1 (en) * | 2004-01-20 | 2006-03-31 | Peugeot Citroen Automobiles Sa | METHOD FOR DEPOSITING A METAL OXIDE COATING ON A SUBSTRATE |
US7384779B2 (en) * | 2004-04-12 | 2008-06-10 | Corning Incorporated | Porous substrate plates and the use thereof |
DE102004052135A1 (en) * | 2004-06-07 | 2005-12-29 | Fachhochschule Schmalkalden | Coated metal substrate especially a hard metal with a wear protection layer consisting of high purity Al2O3 nanocrystals and containing residual pressure stresses useful in tool production |
DE102004041695A1 (en) * | 2004-08-26 | 2006-03-02 | Schott Ag | Colored coating for glass or glass/ceramic plates, for domestic appliances, is a sol-gel network with colored pigments within shroudings to prevent a catalytic reaction |
DE102005018246A1 (en) * | 2005-04-19 | 2006-10-26 | Schott Ag | Glass or glass ceramic articles with decorative coating |
EP1808511A1 (en) * | 2006-01-16 | 2007-07-18 | Siemens Aktiengesellschaft | Method of coating a compressor |
JP2008094972A (en) | 2006-10-12 | 2008-04-24 | Adeka Corp | Coating liquid and manufacturing method of titanic acid-based ceramic film using the coating liquid |
US9431598B2 (en) * | 2006-11-06 | 2016-08-30 | Drexel University | Sol-gel precursors and methods for making lead-based perovskite films |
US20090239061A1 (en) * | 2006-11-08 | 2009-09-24 | General Electric Corporation | Ceramic corrosion resistant coating for oxidation resistance |
DE102007015635A1 (en) * | 2007-03-31 | 2008-10-02 | Schaeffler Kg | Coating of a hardened steel component and method of applying the coating |
WO2008147359A1 (en) * | 2007-05-31 | 2008-12-04 | Carrier Corporation | Deactivation resistant photocatalyst and method of preparation |
CN102067719B (en) | 2008-04-22 | 2014-07-16 | 达泰克涂料股份公司 | Thick film high temperature thermoplastic insulated heating element |
WO2010009234A1 (en) * | 2008-07-16 | 2010-01-21 | Wisconsin Alumni Research Foundation | Metal substrates including metal oxide nanoporous thin films and methods of making the same |
DE102009023628A1 (en) | 2009-05-27 | 2010-12-02 | Siemens Aktiengesellschaft | A method of forming a layer of absorber particles for energy radiation |
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US20130112910A1 (en) * | 2011-05-06 | 2013-05-09 | Seiko Epson Corporation | Precursor solution for piezoelectric films, method for manufacturing the same, and method for manufacturing piezoelectric film |
DE102011077021A1 (en) * | 2011-06-07 | 2012-12-13 | Schaeffler Technologies AG & Co. KG | Method for producing electrically-insulated ceramic coating on piston or bearing component i.e. rolling body, of needle cage, involves applying mixture on component, and drying mixture with temperature between specific degrees Celsius |
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US8716053B2 (en) * | 2012-02-16 | 2014-05-06 | E I Du Pont De Nemours And Company | Moisture barrier for photovoltaic cells |
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FR3013996B1 (en) | 2013-12-02 | 2017-04-28 | Office National Detudes Et De Rech Aerospatiales Onera | PROCESS FOR THE LOCAL REPAIR OF THERMAL BARRIERS |
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WO2020145366A1 (en) * | 2019-01-10 | 2020-07-16 | 日本碍子株式会社 | Composite member |
CN111393153A (en) * | 2020-03-22 | 2020-07-10 | 浙江宇达新材料有限公司 | Method for preparing ceramic membrane |
US11818955B2 (en) | 2021-08-26 | 2023-11-14 | City University Of Hong Kong | Method for forming piezoelectric films on surfaces of arbitrary morphologies |
WO2023250355A1 (en) * | 2022-06-21 | 2023-12-28 | Covalent Coating Technology, Inc. | Fusion of glass/ceramic to industrial metallic substrates |
CN115121131B (en) * | 2022-07-25 | 2024-04-16 | 浙江汇甬新材料有限公司 | Silicon-rich zeolite molecular sieve membrane and preparation method thereof |
Citations (40)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3936383A (en) * | 1973-05-14 | 1976-02-03 | Nobutoshi Daimon | Sol of ultra-fine particles of synthetic hectorite |
US3975165A (en) * | 1973-12-26 | 1976-08-17 | Union Carbide Corporation | Graded metal-to-ceramic structure for high temperature abradable seal applications and a method of producing said |
US4460630A (en) * | 1978-03-15 | 1984-07-17 | Matsushita Electric Industrial Co., Ltd. | Method of forming porcelain enamels on aluminized steel |
US4460639A (en) * | 1983-04-06 | 1984-07-17 | Dow Corning Corporation | Fiber reinforced glass matrix composites |
US4476156A (en) * | 1983-03-10 | 1984-10-09 | The United States Of America As Represented By The United States Department Of Energy | Low temperature process for obtaining thin glass films |
US4726099A (en) * | 1986-09-17 | 1988-02-23 | American Cyanamid Company | Method of making piezoelectric composites |
US4738896A (en) * | 1986-09-26 | 1988-04-19 | Advanced Technology Materials, Inc. | Sol gel formation of polysilicate, titania, and alumina interlayers for enhanced adhesion of metal films on substrates |
US4788046A (en) * | 1987-08-13 | 1988-11-29 | Ceramics Process Systems Corporation | Method for producing materials for co-sintering |
US4814202A (en) * | 1986-05-30 | 1989-03-21 | Centre Meridional D'oenologie | Processes for manufacturing thin membranes composed of an organic lattice of titanium and silicon oxides and powder composed of submicronic grains of mixed titanium and silicon oxides |
US4859525A (en) * | 1985-02-25 | 1989-08-22 | University Of Florida | Method for low temperature processing of lightweight SiC/SiO2 composites and products |
JPH01275765A (en) * | 1988-04-28 | 1989-11-06 | Seiko Epson Corp | Production of implant material |
US4921731A (en) * | 1986-02-25 | 1990-05-01 | University Of Florida | Deposition of ceramic coatings using sol-gel processing with application of a thermal gradient |
US4946710A (en) * | 1987-06-02 | 1990-08-07 | National Semiconductor Corporation | Method for preparing PLZT, PZT and PLT sol-gels and fabricating ferroelectric thin films |
US4970182A (en) * | 1986-12-17 | 1990-11-13 | Nippondenso Co., Ltd. | Method for producing multi-component ceramics |
US4990324A (en) * | 1986-12-17 | 1991-02-05 | Nippondenso Co., Ltd. | Method for producing two-component or three-component lead zirconate-titanate |
EP0433915A1 (en) * | 1989-12-20 | 1991-06-26 | Central Glass Company, Limited | Method of forming metal oxide film by using metal alkoxide solution |
US5053251A (en) * | 1989-05-26 | 1991-10-01 | Shinko Pantec Co., Ltd. | Method for repairing glass-lined equipment by sol-gel process |
US5066617A (en) * | 1986-07-23 | 1991-11-19 | Nippon Steel Corporation | Method for producing plzt powder |
US5091348A (en) * | 1988-04-22 | 1992-02-25 | Alcan International Limited | Sol-gel method of making ceramics |
US5106828A (en) * | 1987-07-20 | 1992-04-21 | North American Philips Corporation | Method for fabricating superconductors by sol-gel process |
EP0482659A1 (en) * | 1990-10-25 | 1992-04-29 | Sumitomo Electric Industries, Limited | Process for producing thin glass film by sol-gel method |
US5147515A (en) * | 1989-09-04 | 1992-09-15 | Dipsol Chemicals Co., Ltd. | Method for forming ceramic films by anode-spark discharge |
US5173331A (en) * | 1986-08-01 | 1992-12-22 | International Business Machines Corporation | Zirconia toughening of glass-ceramic materials |
US5185177A (en) * | 1988-02-08 | 1993-02-09 | Mitsubishi Kasei Corporation | Producing a ceramic implant by coating a powder mixture of zirconia and either tricalcium phosphate or hydroxyapatite on a molded unsintered body of partially stabilized zirconia and then sintering the article |
US5198269A (en) * | 1989-04-24 | 1993-03-30 | Battelle Memorial Institute | Process for making sol-gel deposited ferroelectric thin films insensitive to their substrates |
US5204140A (en) * | 1986-03-24 | 1993-04-20 | Ensci, Inc. | Process for coating a substrate with tin oxide |
US5219611A (en) * | 1991-09-30 | 1993-06-15 | Cornell Research Foundation, Inc. | Preparing densified low porosity titania sol gel forms |
US5242631A (en) * | 1992-01-13 | 1993-09-07 | Westinghouse Electric Corp. | Method for coating nuclear fuel pellets |
EP0564866A2 (en) * | 1992-04-06 | 1993-10-13 | Motorola, Inc. | Method for making a semiconductor device having an anhydrous ferroelectric thin film |
US5260094A (en) * | 1991-09-30 | 1993-11-09 | Cornell Research Foundation, Inc. | Preparing densified low porosity titania sol-gel forms |
US5266360A (en) * | 1991-12-20 | 1993-11-30 | United Technologies Corporation | Inhibiting coke formation by coating gas turbine elements with silica |
US5281405A (en) * | 1992-02-19 | 1994-01-25 | E. I. Du Pont De Nemours And Company | Optically useful compositions and a sol-gel process for their production |
US5308807A (en) * | 1992-07-15 | 1994-05-03 | Nalco Chemical Company | Production of lead zirconate titanates using zirconia sol as a reactant |
US5352481A (en) * | 1992-05-29 | 1994-10-04 | Hughes Aircraft Company | Process for forming particles having a uniform size distribution |
US5506061A (en) * | 1989-07-06 | 1996-04-09 | Forskningscenter Riso | Method for the preparation of metal matrix composite materials |
US5558701A (en) * | 1993-01-08 | 1996-09-24 | British Technology Group Limited | Sol-gel composition for producing glassy coatings |
US5585136A (en) * | 1995-03-22 | 1996-12-17 | Queen's University At Kingston | Method for producing thick ceramic films by a sol gel coating process |
US5662824A (en) * | 1988-05-24 | 1997-09-02 | Alfa Biotech Spa | Magnetically attractable particles and method |
US5676745A (en) * | 1995-06-07 | 1997-10-14 | The United States Of America, As Represented By The Secretary Of Commerce | Pre-ceramic polymers in fabrication of ceramic composites |
US5759376A (en) * | 1994-09-07 | 1998-06-02 | Dot Dunnschicht- Und Oberflaechen-Technologie Gmbh | Method for the electrodeposition of hydroxyapatite layers |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5885657A (en) * | 1994-06-23 | 1999-03-23 | Creavis Gesellschaft Fur Technologie Und Innovation Mbh | Production of ceramic layers and their use |
-
1995
- 1995-03-22 US US08/409,127 patent/US5585136A/en not_active Ceased
-
1996
- 1996-02-13 AU AU46174/96A patent/AU4617496A/en not_active Abandoned
- 1996-02-13 WO PCT/CA1996/000088 patent/WO1996029447A1/en active IP Right Grant
- 1996-02-13 ES ES96901675T patent/ES2159716T3/en not_active Expired - Lifetime
- 1996-02-13 PT PT96901675T patent/PT815285E/en unknown
- 1996-02-13 DE DE69614673T patent/DE69614673T2/en not_active Expired - Lifetime
- 1996-02-13 DK DK96901675T patent/DK0815285T3/en active
- 1996-02-13 JP JP8527922A patent/JPH11502262A/en active Pending
- 1996-02-13 EP EP96901675A patent/EP0815285B1/en not_active Expired - Lifetime
- 1996-02-13 AT AT96901675T patent/ATE204617T1/en active
- 1996-02-13 CA CA002213209A patent/CA2213209C/en not_active Expired - Lifetime
- 1996-02-13 KR KR1019970706610A patent/KR100390037B1/en not_active IP Right Cessation
-
1997
- 1997-09-26 US US08/938,996 patent/USRE36573E/en not_active Expired - Lifetime
-
1998
- 1998-07-07 HK HK98109000A patent/HK1007889A1/en not_active IP Right Cessation
Patent Citations (42)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3936383A (en) * | 1973-05-14 | 1976-02-03 | Nobutoshi Daimon | Sol of ultra-fine particles of synthetic hectorite |
US3975165A (en) * | 1973-12-26 | 1976-08-17 | Union Carbide Corporation | Graded metal-to-ceramic structure for high temperature abradable seal applications and a method of producing said |
US4460630A (en) * | 1978-03-15 | 1984-07-17 | Matsushita Electric Industrial Co., Ltd. | Method of forming porcelain enamels on aluminized steel |
US4476156A (en) * | 1983-03-10 | 1984-10-09 | The United States Of America As Represented By The United States Department Of Energy | Low temperature process for obtaining thin glass films |
US4460639A (en) * | 1983-04-06 | 1984-07-17 | Dow Corning Corporation | Fiber reinforced glass matrix composites |
US4859525A (en) * | 1985-02-25 | 1989-08-22 | University Of Florida | Method for low temperature processing of lightweight SiC/SiO2 composites and products |
US4921731A (en) * | 1986-02-25 | 1990-05-01 | University Of Florida | Deposition of ceramic coatings using sol-gel processing with application of a thermal gradient |
US5204140A (en) * | 1986-03-24 | 1993-04-20 | Ensci, Inc. | Process for coating a substrate with tin oxide |
US4814202A (en) * | 1986-05-30 | 1989-03-21 | Centre Meridional D'oenologie | Processes for manufacturing thin membranes composed of an organic lattice of titanium and silicon oxides and powder composed of submicronic grains of mixed titanium and silicon oxides |
US5066617A (en) * | 1986-07-23 | 1991-11-19 | Nippon Steel Corporation | Method for producing plzt powder |
US5173331A (en) * | 1986-08-01 | 1992-12-22 | International Business Machines Corporation | Zirconia toughening of glass-ceramic materials |
US4726099A (en) * | 1986-09-17 | 1988-02-23 | American Cyanamid Company | Method of making piezoelectric composites |
US4738896A (en) * | 1986-09-26 | 1988-04-19 | Advanced Technology Materials, Inc. | Sol gel formation of polysilicate, titania, and alumina interlayers for enhanced adhesion of metal films on substrates |
US4990324A (en) * | 1986-12-17 | 1991-02-05 | Nippondenso Co., Ltd. | Method for producing two-component or three-component lead zirconate-titanate |
US4970182A (en) * | 1986-12-17 | 1990-11-13 | Nippondenso Co., Ltd. | Method for producing multi-component ceramics |
US5116643A (en) * | 1987-06-02 | 1992-05-26 | National Semiconductor Corporation | Method for preparing PLZT, PZT and PLT sol-gels and fabricating ferroelectric thin films |
US5028455A (en) * | 1987-06-02 | 1991-07-02 | National Semiconductor Corporation | Method for preparing plzt, pzt and plt sol-gels and fabricating ferroelectric thin films |
US4946710A (en) * | 1987-06-02 | 1990-08-07 | National Semiconductor Corporation | Method for preparing PLZT, PZT and PLT sol-gels and fabricating ferroelectric thin films |
US5106828A (en) * | 1987-07-20 | 1992-04-21 | North American Philips Corporation | Method for fabricating superconductors by sol-gel process |
US4788046A (en) * | 1987-08-13 | 1988-11-29 | Ceramics Process Systems Corporation | Method for producing materials for co-sintering |
US5185177A (en) * | 1988-02-08 | 1993-02-09 | Mitsubishi Kasei Corporation | Producing a ceramic implant by coating a powder mixture of zirconia and either tricalcium phosphate or hydroxyapatite on a molded unsintered body of partially stabilized zirconia and then sintering the article |
US5091348A (en) * | 1988-04-22 | 1992-02-25 | Alcan International Limited | Sol-gel method of making ceramics |
JPH01275765A (en) * | 1988-04-28 | 1989-11-06 | Seiko Epson Corp | Production of implant material |
US5662824A (en) * | 1988-05-24 | 1997-09-02 | Alfa Biotech Spa | Magnetically attractable particles and method |
US5198269A (en) * | 1989-04-24 | 1993-03-30 | Battelle Memorial Institute | Process for making sol-gel deposited ferroelectric thin films insensitive to their substrates |
US5053251A (en) * | 1989-05-26 | 1991-10-01 | Shinko Pantec Co., Ltd. | Method for repairing glass-lined equipment by sol-gel process |
US5506061A (en) * | 1989-07-06 | 1996-04-09 | Forskningscenter Riso | Method for the preparation of metal matrix composite materials |
US5147515A (en) * | 1989-09-04 | 1992-09-15 | Dipsol Chemicals Co., Ltd. | Method for forming ceramic films by anode-spark discharge |
EP0433915A1 (en) * | 1989-12-20 | 1991-06-26 | Central Glass Company, Limited | Method of forming metal oxide film by using metal alkoxide solution |
EP0482659A1 (en) * | 1990-10-25 | 1992-04-29 | Sumitomo Electric Industries, Limited | Process for producing thin glass film by sol-gel method |
US5260094A (en) * | 1991-09-30 | 1993-11-09 | Cornell Research Foundation, Inc. | Preparing densified low porosity titania sol-gel forms |
US5219611A (en) * | 1991-09-30 | 1993-06-15 | Cornell Research Foundation, Inc. | Preparing densified low porosity titania sol gel forms |
US5266360A (en) * | 1991-12-20 | 1993-11-30 | United Technologies Corporation | Inhibiting coke formation by coating gas turbine elements with silica |
US5242631A (en) * | 1992-01-13 | 1993-09-07 | Westinghouse Electric Corp. | Method for coating nuclear fuel pellets |
US5281405A (en) * | 1992-02-19 | 1994-01-25 | E. I. Du Pont De Nemours And Company | Optically useful compositions and a sol-gel process for their production |
EP0564866A2 (en) * | 1992-04-06 | 1993-10-13 | Motorola, Inc. | Method for making a semiconductor device having an anhydrous ferroelectric thin film |
US5352481A (en) * | 1992-05-29 | 1994-10-04 | Hughes Aircraft Company | Process for forming particles having a uniform size distribution |
US5308807A (en) * | 1992-07-15 | 1994-05-03 | Nalco Chemical Company | Production of lead zirconate titanates using zirconia sol as a reactant |
US5558701A (en) * | 1993-01-08 | 1996-09-24 | British Technology Group Limited | Sol-gel composition for producing glassy coatings |
US5759376A (en) * | 1994-09-07 | 1998-06-02 | Dot Dunnschicht- Und Oberflaechen-Technologie Gmbh | Method for the electrodeposition of hydroxyapatite layers |
US5585136A (en) * | 1995-03-22 | 1996-12-17 | Queen's University At Kingston | Method for producing thick ceramic films by a sol gel coating process |
US5676745A (en) * | 1995-06-07 | 1997-10-14 | The United States Of America, As Represented By The Secretary Of Commerce | Pre-ceramic polymers in fabrication of ceramic composites |
Non-Patent Citations (6)
Title |
---|
Abstract No. 1 275765(A) of JP Application No. 63 106057, Nov. 6, 1989. * |
Abstract No. 1-275765(A) of JP Application No. 63-106057, Nov. 6, 1989. |
Guglielmi, M. et al., "Precursors for sol gel prepaarations", J. Non-Cryst. Solids 100:16-30 (1988). |
Guglielmi, M. et al., Precursors for sol gel prepaarations , J. Non Cryst. Solids 100:16 30 (1988). * |
Yi et al., "Sol-Gel Processing of Complex Oxide Films," Ceramic Bulletin vol. 70 No. 7 1991 pp. 1173-1179. |
Yi et al., Sol Gel Processing of Complex Oxide Films, Ceramic Bulletin vol. 70 No. 7 1991 pp. 1173 1179. * |
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DK0815285T3 (en) | 2001-10-08 |
ATE204617T1 (en) | 2001-09-15 |
EP0815285B1 (en) | 2001-08-22 |
HK1007889A1 (en) | 1999-04-30 |
KR100390037B1 (en) | 2003-10-22 |
US5585136A (en) | 1996-12-17 |
DE69614673T2 (en) | 2002-06-27 |
AU4617496A (en) | 1996-10-08 |
EP0815285A1 (en) | 1998-01-07 |
CA2213209C (en) | 2003-10-21 |
JPH11502262A (en) | 1999-02-23 |
WO1996029447A1 (en) | 1996-09-26 |
PT815285E (en) | 2001-12-28 |
ES2159716T3 (en) | 2001-10-16 |
KR19980703207A (en) | 1998-10-15 |
DE69614673D1 (en) | 2001-09-27 |
CA2213209A1 (en) | 1996-09-26 |
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