WO2004110959A1 - Uniformly coloured ceramic framework and ceramic colouring solution - Google Patents
Uniformly coloured ceramic framework and ceramic colouring solution Download PDFInfo
- Publication number
- WO2004110959A1 WO2004110959A1 PCT/EP2004/006220 EP2004006220W WO2004110959A1 WO 2004110959 A1 WO2004110959 A1 WO 2004110959A1 EP 2004006220 W EP2004006220 W EP 2004006220W WO 2004110959 A1 WO2004110959 A1 WO 2004110959A1
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- WIPO (PCT)
- Prior art keywords
- solution
- ceramic framework
- ceramic
- polyethylene glycol
- anyone
- Prior art date
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Classifications
-
- 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
-
- 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating 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
- C04B41/5007—Coating 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 salts or salty compositions, e.g. for salt glazing
-
- 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
-
- 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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
- C04B2111/00836—Uses not provided for elsewhere in C04B2111/00 for medical or dental applications
Definitions
- the present invention relates to a colouring solution for ceramic framework, the ceramic framework coloured with the solution as well as a process for obtaining a uniformly coloured ceramic framework.
- Ceramic framework is usually coloured with metal salt solutions. For that purpose salt solutions are applied on the ceramic or the framework itself is dipped into the solution. The framework is dried afterwards and fired to fix the colour.
- DE 196 19 168 A1 describes a ceramic colouring solution consisting essentially of water and a palladium containing compound dissolved therein.
- the solution might further contain cosolvents such as alcohols, glycols, glycol ether or polyethylene glycol.
- DE 196 19 165 C1 A1 refers to a similar solution containing a mixture of Ti and Fe components.
- WO 00/46168 A1 refers to colouring ceramics by way of ionic or complex- containing solutions containing defined concentrations of at least one salts or complexes of the rare earth elements or of the elements of the subgroups.
- the solution might contain additives like stabilizers, complex builders, pigments and beating additives.
- One way to prevent migrations of that type might be the addition of soluble substances of high molecular weight. This usually affects the diffusion of all ingredients and thereby leads to the desired effect.
- polymeric additives may decrease the solubility of metal ions by binding great portions of the water available and also may decrease the shelf live stability of the solution by facilitating precipitation or being prone to degradation.
- Any additive must also be thermally degradable during the firing process without leaving ay residue or affecting the composition and integrity of the ceramic framework.
- a further object is to provide a colouring solution for ceramic framework that prevents the disadvantageous separation tendencies, however, maintaining all other desired properties of the system.
- Still a further object is to provide a colouring solution leading to less sintering deformation of ceramic framework after firing.
- Still a further object is to provide a colouring solution leading to a uniformly coloured ceramic framework.
- a stabilizer wherein the polyethylene glycol is present in an amount of about 0,5 to about 10 % by weight of the total composition addresses the problems mentioned above.
- the present invention relates to a solution for colouring ceramic framework, ceramic framework coloured with said solution and a process for colouring a ceramic framework.
- polyethylene glycol or derivatives thereof surprisingly shows no detrimental effect on the viscosity and does not affect the shelf life stability of the solution.
- a further positive and surprising effect using polyethylene oxides and derivatives thereof is the positive influence on the deformation occurring during the sintering process.
- inventive colouring solution it is thus possible to improve the fit of wide spanning frameworks (more than 3 units).
- inventive solution can be applied to presintered ceramic bodies of various compositions, especially such comprising or preferably consisting essentially of ZrO 2 and/or AI 2 O 3 , respectively.
- compositions are known to the skilled person in the art (cf. for example WO 00/4618 A1).
- the ZrO 2 is preferably stabilized with Y 2 O 3 .
- Useful metal salts useful for the colouring purpose are described e.g. in WO 00/46168 A1 especially on page 3.
- Useful metal salts are preferably selected from rare earth elements or of the subgroups of the rare earth elements like La, Pr and/or Er.
- Useful are also salts of transition metals of the groups MIA, IVA, VA, VIA, VIIA, VIIIA, IB, HB, especially Fe, Co, Ni, Cu and Mn.
- a combination of Fe, Mn and Er is particularly preferred (cf. Table of Periodic Properties of the Elements; SARGENT- WELCH Scientific Company; Illinois 60077; 1980).
- metal salts soluble in the solvent used can be used.
- the metal ions are contained in the solution in an amount sufficient to achieve an adequate colouring of the ceramic framework. Good results can be achieved e.g. with amounts in the range of about 0,01 to about 15,0 % by weight of metal ions, preferably in the range of about 0,1 to about 10,0 % by weight, more preferably in the range of about 0,1 to about 7,0 % by weight.
- Polyethylene oxide or derivatives of polyethylene oxide in the meaning of the present invention are generally prepolymeric polyethers predominantly comprising -(CH 2 -CH 2 -O)- groups.
- the polyethylene glycol should preferably be dissolvable or dispersible in the solvent containing appropriate amounts of metal ions as mentioned above.
- metal ions i.g., sodium sulfate, sodium sulfate, sodium sulfate, sodium sulfate, sodium sulfate, sodium sulfate, sodium sulfate, sodium sulfate, sodium sulfate, sodium sulfate, sodium sulfate, sodium sulfate, sodium sulfate, sodium sulfate, sodium sulfate, sodium sulfate, sodium sulfate, sodium sulfate, sodium sulfate, sodium sulfate, sodium sulfate, sodium sulfate, sodium sulfate, sodium sulfate, sodium sulfate, sodium sulfate, sodium sulfate, sodium sulfate, sodium sulfate, sodium sulfate, sodium
- Mn (substance) is the average molecular weight of the respective polyether oxide or ethoxylated compound used. While simple polyethylene glycols show the highest water solubility, segmented derivatives may add tensidic characteristics, if desired.
- polyethylene also mixtures of polyethylene and the derivatives can be used.
- Preferred examples for the polyethylene oxides mentioned above are:
- the inventive colouring solution also comprises a solvent.
- the solvent should preferable be able to dissolve the metal ion(s) used.
- Typical solvents are water, alcohols like methyl alcohol, ethyl alcohol, iso-propyl alcohol, n-propyl alcohol, ketones like aceton and mixtures of water with alcohols and/or ketones and/or ethylene glycol and/or glycerol.
- the number average molecular weight (Mn) of the polyethylene oxide should be in the range of about 1.000 to about 200.000, preferably in the range of about 10.000 to about 100.000, more preferably in the range of about 20.000 to about 50.000.
- the Mn is in the range of about 500 or below, the content of the polyethylene glycol used has to be increased. If the Mn is above about 200.000, the polyethylene glycol used might be not sufficiently soluble in the solution and a homogeneous mixture is difficult to obtain.
- Mn The number average molecular weight (Mn) can be determined according to procedures known to a person skilled in the art as described for example in Arndt/M ⁇ ller, Polymer charactermaschine, Hanse Verlag, 1996. Depending on the molecular weight to be determined, it might be necessary to apply different measurement methods (see below).
- the polyethylene oxide should be added in an amount so that the desired effect can be obtained and the ceramic framework obtained after firing is uniformly coloured.
- the polyethylene oxide can be added in an amount in the range of about 0,5 to about 10 % by weight of the colouring solution, preferably in an amount in the range of about 1 to about 8 % by weight or in an amount in the range of about 1 to about 5 % by weight, or in an amount in the range of about 4 to about 8 % by weight.
- the colour value might be to bright.
- the colour value might be not homogenous.
- Further additives can be added to the colouring solution like stabilizers such as methoxy phenol hydrochinone, Topanol A, ascorbic acid, complex builders such as EDTA, NTA, citric acid, lactic acid and beating additives such as temporary binders, buffers such as acetate or amino buffers and thixotropic substances like polysaccharides, poly vinyl alcohols, cellulose derivatives, carraghenanes, polyvinyl pyrollidone.
- stabilizers such as methoxy phenol hydrochinone, Topanol A, ascorbic acid, complex builders such as EDTA, NTA, citric acid, lactic acid and beating additives
- temporary binders such as acetate or amino buffers and thixotropic substances like polysaccharides, poly vinyl alcohols, cellulose derivatives, carraghenanes, polyvinyl pyrollidone.
- the present invention is also directed to a process comprising the steps:
- Colouring the ceramic framework can be achieved by dipping the framework into the solution.
- the solution can also be applied to the framework by spraying, brushing or by using a sponge or fabric.
- the ceramic framework usually is treated with the solution for about 1 to about 5 minutes, preferably about 2 to about 3 minutes at room temperature. Preferably no pressure is used.
- Drying the coloured ceramic framework is not absolute necessary, but preferred to reduce the time needed for firing and to avoid unwanted inhomogenous colour effects.
- the firing conditions are dependant on the ceramic material used.
- the firing usually takes place for a ZrO 2 based ceramic at a temperature above about 1300 °C, preferably above about 1400 0 C, more preferably above about 1450 °C and lasts for at least about 0,5 h, preferably for at least about 1 h, more preferably for at least about 2 h.
- the firing usually takes place for a AI 2 O 3 based ceramic at a temperature above about 1350 °C, preferably above about 1450 0 C 1 more preferably above about 1650 °C and lasts for at least about 0,5 h, preferably for at least about 1 h, more preferably for at least about 2 h.
- the present invention relates also to ceramic framework coloured with the inventive solution, and to ceramic framework obtainable by a process as described above.
- the coloring solution of the present invention does not necessarily comprise any organic colorants or coloring means that will only tint the surface but not the bulk, like pigments.
- Titroprozessor As an apparatus a Titroprozessor (TIP) is used with a Pt-titrode and a high Ohm reference electrode; chemical agents to be used are: 2 N KOH/methanol; 2,5 ml acetic anhydrid solved in 50,0 ml DMF; 2,5 g 4-Dimethylaminopyridin solved in 100 ml DMF (catalytic solvent); THF, H 2 O. All substances should be water free ( ⁇ 0,01 % water).
- TIP Titroprozessor
- a specific amount of the substance to be analyzed is put in a vessel and solved in 20 ml THF, if necessary by warming up. After addition of 10,0 ml catalytic solvent and 5,0 ml acetic anhydride reagent the mixture is stirred in the sealed vessel for 30 min at RT. Thereafter 2,0 ml H 2 O is added and the mixture is stirred for another 10 min at RT. The titration is done with 0,2 N KOH/methanol. Three blank values are determined to be used to determine the average value. The calculation is done as follows:
- SEC size exclusion chromatography
- the polymer is dissolved in tetrahydrofuran as mobile phase(THF, p.a., stabilized with BHT) and then analyzed by SEC with a differential refractometer detector.
- Molecular weight characterization is achieved by regression analysis of external polyethylene glycol (PEG) standards (8 SEC standards, 420 to 108.000 g/mol, e.g. from Fluka).
- the analysis is done with a liquid chromatograph being able to deliver a constant longterm flow of 1.0 ml/min equipped with a differential refractometer (refractive index detector) and an electronic integrator, together with a column SDV, 8.0 mm x 30 cm with particle size of 5 microns, columns with 10.000 A, 500 ⁇ and 100 A; from PSS, Mainz, Germany, and a pre-column SDV, 8.0 x 50 mm with particle size of 10 microns, 100 A; from PSS, Mainz, Germany.
- the flow rate should be 1.0 mi/min.
- WinGPC Size Exclusion Chromatography software from PSS, Mainz, Germany can be used to analyze the data obtained.
- the average retention times for all the PEG standards is calculated, as well as the log 10 MW for all the PEG standards.
- a PEG Molecular Weight (MW) calibration curve is constructed and the average retention times are plotted vs. log-
- the correlation coefficient (R2) should be > 0.99.
- the molecular weight of the PEG sample using the SEC software is calculated. Values for Peak MW (MP), Weight Average MW (MW), Number Average MW (MN), and Polydispersity (DP) can be obtained.
- MP Peak MW
- MW Weight Average MW
- MN Number Average MW
- DP Polydispersity
- Figure 1 shows a typical test bar used for evaluating the deformation of the coloured ceramic framework after firing.
- Figure 2 shows a typical ceramic disc (Zirconia) used for evaluating the results of the homogeneity of the colouring process.
- the rod-shaped samples (dimensions h * w * l: 3 * 4 * 48 [mm]; before sintering) were processed similar to a LavaTM bridge (milling, dyeing and sintering) with a commercial LavaTM equipment:
- the presintered Zirconia (a LavaTM Frame blank for bridges) were milled, thereafter the dust was removed with microbrushes and compressed air.
- the milled sample was dipped in one of the LavaTM frame shade dying liquids (F5,
- the solution FS 5 comprised 1 ,9 % by weight metal ions, 1 ,5 % by weight organic binder.
- the frame shade solutions used are nominated as FS 4 and 6 (solution not containing polyethylene glycol) and FS 4 * and 6* (solution containing polyethylene glycol).
- the solution FS 4 comprised 5,0 % by weight metal ions, 1 ,5 % by weight organic binder.
- the solution FS 6 comprised 1 ,4 % by weight metal ions, 1 ,5 % by weight organic binder.
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- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Inorganic Chemistry (AREA)
- Dental Preparations (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Paints Or Removers (AREA)
- Cosmetics (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Sampling And Sample Adjustment (AREA)
- Liquid Crystal (AREA)
Abstract
Description
Claims
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2006515864A JP4949020B2 (en) | 2003-06-13 | 2004-06-09 | Evenly colored ceramic framework and ceramic coloring solution |
CA2529110A CA2529110C (en) | 2003-06-13 | 2004-06-09 | Uniformly coloured ceramic framework and ceramic colouring solution |
US10/560,702 US20060117989A1 (en) | 2003-06-13 | 2004-06-09 | Uniformly coloured ceramic framework and colouring solution |
AU2004247376A AU2004247376B2 (en) | 2003-06-13 | 2004-06-09 | Uniformly coloured ceramic framework and ceramic colouring solution |
US12/610,745 US20100047438A1 (en) | 2003-06-13 | 2009-11-02 | Uniformly coloured ceramic framework and colouring solution |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP03013513.1 | 2003-06-13 | ||
EP03013513A EP1486476B1 (en) | 2003-06-13 | 2003-06-13 | Uniformly coloured ceramic framework and colouring solution |
Related Child Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US12/610,745 Division US20100047438A1 (en) | 2003-06-13 | 2009-11-02 | Uniformly coloured ceramic framework and colouring solution |
Publications (1)
Publication Number | Publication Date |
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WO2004110959A1 true WO2004110959A1 (en) | 2004-12-23 |
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Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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PCT/EP2004/006220 WO2004110959A1 (en) | 2003-06-13 | 2004-06-09 | Uniformly coloured ceramic framework and ceramic colouring solution |
Country Status (9)
Country | Link |
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US (2) | US20060117989A1 (en) |
EP (1) | EP1486476B1 (en) |
JP (1) | JP4949020B2 (en) |
CN (1) | CN100556856C (en) |
AT (1) | ATE309182T1 (en) |
AU (1) | AU2004247376B2 (en) |
CA (1) | CA2529110C (en) |
DE (1) | DE60302225T2 (en) |
WO (1) | WO2004110959A1 (en) |
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Also Published As
Publication number | Publication date |
---|---|
AU2004247376A1 (en) | 2004-12-23 |
AU2004247376B2 (en) | 2009-11-12 |
CN1805913A (en) | 2006-07-19 |
CN100556856C (en) | 2009-11-04 |
EP1486476A1 (en) | 2004-12-15 |
ATE309182T1 (en) | 2005-11-15 |
JP4949020B2 (en) | 2012-06-06 |
DE60302225D1 (en) | 2005-12-15 |
EP1486476B1 (en) | 2005-11-09 |
JP2006527156A (en) | 2006-11-30 |
US20060117989A1 (en) | 2006-06-08 |
US20100047438A1 (en) | 2010-02-25 |
CA2529110A1 (en) | 2004-12-23 |
CA2529110C (en) | 2012-01-31 |
DE60302225T2 (en) | 2006-08-10 |
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