WO1989010903A1 - Article de verre - Google Patents

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Publication number
WO1989010903A1
WO1989010903A1 PCT/AU1989/000196 AU8900196W WO8910903A1 WO 1989010903 A1 WO1989010903 A1 WO 1989010903A1 AU 8900196 W AU8900196 W AU 8900196W WO 8910903 A1 WO8910903 A1 WO 8910903A1
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WO
WIPO (PCT)
Prior art keywords
glass
coating composition
article
glass coating
approximately
Prior art date
Application number
PCT/AU1989/000196
Other languages
English (en)
Inventor
Lawrence David Mccarthy
Henry John Rossell
Michael Vincent Swain
Original Assignee
Commonwealth Scientific And Industrial Research Or
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Commonwealth Scientific And Industrial Research Or filed Critical Commonwealth Scientific And Industrial Research Or
Publication of WO1989010903A1 publication Critical patent/WO1989010903A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/28—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material
    • C03C17/32—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material with synthetic or natural resins

Definitions

  • the present invention relates to glass articles including toughened glass articles and to a method of preparing such glass articles.
  • Silica based glasses including the widely-used soda-lime container glass, are isotropic elastic solids. They are chemically homogeneous, with all the constituent atoms strongly bonded to one another, but with no long-range or periodic order. Estimates based on the nature of the interatomic forces indicate that strains of up to 20% should occur before rupture occurs: this is equivalent to strengths in the range 10-20 GPa. For normal samples, observed strengths usually are less than one hundredth of this theoretical level; moreover, samples which have received nominally identical treatment show a wide variation in their individual strengths.
  • Such surface inclusions may be airborne dust particles present during the heat treatment of the glass, and temperatures well below the softening point of the glass will suffice to develop strongly-bonded inclusions, which then act as significant strength-limiting flaws.
  • atmospheric moisture acts detrimentally on a glass surface, producing corrosion products; these are a form of foreign inclusion, and have the same strength-limiting effect.
  • the sodium in the surface layer of glass is exchanged for potassium in a molten salt bath. Since the potassium ions occupy a greater volume than the sodium ions they have replaced, the surface layer is placed under a compressive stress. This procedure is costly, however, and cannot be applied reasonably to glass containers that are made in large numbers.
  • a glass coating composition including an effective amount of at least one inorganic or organic polymeric component; and at least one reinforcing component incorporated
  • the glass coating composition according to the present invention when coated on a glass article, strengthens and toughens the article.
  • the coating 0 advantageously adheres strongly to the glass substrate and possesses a high tensile strength of itself.
  • the coating formed from the glass coating composition lies across any pre-existing, strength-limiting 5 flaws in the glass surface. Under the action of any applied tensile load, the stress across any flaw would then be carried by the coating. Thus, extra work would have to be done before the load carrying effect of the coating broke down, which would then allow the microcracks in the glass to o widen and cause failure of the glass.
  • the coating formed from the glass coating composition may protect the glass surface from abrasion, indentation, or any other such damage leading to the production of strength limiting flaws.
  • the at least one inorganic or organic polymeric component of the glass coating composition may be of any suitable type which will provide the required high tensile strength.
  • a water soluble or water insoluble polymer may be used. Where a water soluble polymer is used the coating composition may be rendered water resistant as discussed below.
  • a natural or synthetic organic polymer may be used as the polymeric component.
  • a synthetic organic polymer may be selected from acrylic polymers including acrylate and methacrylate polymers or copolymers, acrylamide or methacrylamide polymers or copolymers thereof, urethane polymers or copolymers thereof, alkyd resins, or mixtures thereof.
  • Preferred acrylic polymers include polyacrylamide and polymethylmethacrylate.
  • Alkyd resins (“Glyptal” resins), may be used alone, or with the inclusion of one or more copolymers to modify their properties in a manner known per se. These resins may be provided in a form that is soluble in common organic 5 ' solvents such as alcohol", applied to the glass, dried, then converted to the final crosslinked or cured form thermally at temperatures near 200°C ("stoving varnishes"), or crosslinked with reagents such as melamine to further modify the properties according to known art. Alkyd resins are ⁇ obtainable commercially in an extremely wide range of formulations, and admixtures with copolymers and crosslinking agents.
  • the preferred polyurethanes may be selected from the large range of formulations available commercially.
  • Polyurethane is known to have excellent adhesion to glass, and has been proposed as a useful coating (e.g. Vaporcure process).
  • a useful coating e.g. Vaporcure process
  • a commercial two-part coating material was purchased (Epiglass reaction lacquer) . Preliminary trials showed that this coating formed hard adherent films on freshly fired slides.
  • Polyurethanes are produced from a reaction between a polyhydroxyl compound (polyol) and a polyfunctional isocyanate.
  • Typical reactants could be propylene glycol and toluene diisocyanate with a catalyst of tin octoate.
  • the commercial two-part PU coatings contain partly polymerised polyol/diisocyanate: one part has unreacted hydroxyl groups and catalyst, the other part has an excess of isocyanate.
  • the two components When the two components are mixed they react to form a gelatinous solid in about an hour; reaction then continues to form a rigid polymer.
  • Complete reaction at room temperature takes about 3 days. The period of 3 days required to achieve complete reaction was inconvenient, so further investigations have been conducted at various temperatures and times to investigate thermal acceleration of the polymerization. It was found that heating to 80°C for 2 hours was sufficient to give a tough adherent film.
  • a protein polymer for example a casein polymer may be used as a natural polymeric component.
  • a low melting silicon polymer may be used.
  • a low melting glass may be used.
  • the at least one polymeric component may be present in any suitable effective amounts.
  • the polymeric component may comprise from approximately 40 to 95% by weight, based on the total weight of the glass coating composition. A polymeric component content of about 50 to 95% by weight is preferred.
  • the at least one reinforcing component of the glass coating composition may have a platelet-type structure.
  • the reinforcing component having platelet-type structure may be a silicon carbide or vermiculite product, for example an exfoliated vermiculite.
  • the reinforcing component may alternatively or in addition include a component having a fibrous structure, organic, inorganic or mineral fibres, preferably high-modulus 0 whiskers or fibres.
  • the reinforcing component having a fibrous structure may include silicon carbides, silicon nitrides, alumina, metals or mixtures thereof.
  • silicon carbide (SiC) including silicon carbide whiskers are not used in r _r conjunction with polyacrylate polymers, alkyd resins.
  • a vermiculite product has the advantage that the particles are platelets typically approximately 5 m diameter and about 3nm thick, which do not represent any biological hazard, as may be encountered with product having a fibrous
  • flakes would all lie parallel in a coating and be bonded to each other, and to the glass surface by the polymeric component.
  • whiskers or fibres these may be in any suitable configuration including felts, oriented weaves and. lay-ups so as to provide desired
  • the reinforcing component may be present in the glass coating composition in any suitable effective amount.
  • the reinforcing component may be present in amounts of from approximately 5 to 60% by weight, based on the total weight of the glass coating composition.
  • a reinforcing component of approximately 5 to 40% by weight based on the total weight of the glass coating composition is preferred.
  • the glass coating composition may further include an effective amount of at least one coupling agent.
  • the at least one coupling agent may function to improve adhesion of the polymeric component to the reinforcing component and/or to the glass substrate when, in use, the coating composition is coated onto such a substrate.
  • the coupling agent may also function to improve the water resistance of the coating on curing.
  • the at least one coupling agent may be a silane product.
  • An amino silane product may be used. (N,N-diethyl- 3-aminopropyl)trimethoxysilane is preferred.
  • the at least one coupling agent may be present in the glass coating composition in any suitable effective amount.
  • the at least one silane coupling agent may be present in an amount of from approximately 0.1 to 1% by weight based on the total weight of the glass coating, composition.
  • the glass coating composition may further include an effective amount of at least one cross-linking agent.
  • the cross-linking agent may be a heat-, or radiation-curable cross-linking agent.
  • a cross-linking agent such as a glyoxal formaldehyde may be used.
  • the at least one cross-linking agent may be present in the glass coating composition in any suitable effective amount.
  • the cross-linking agent may be present in amount of from 0 to approximatley 50%, preferably approximately 5 to 50%, more preferably approximately 7.5% to 10% by weight based on the total weight of the glass coating composition.
  • the glass coating composition according to the present invention may further include other compounding ingredients.
  • Compounding ingredients such as colourants, fillers, solvents, dispersants, surfactants, extenders, and the like may be included.
  • the glass coating composition may be provided in the form of a solution or dispersion in a suitable solvent.
  • An aqueous solvent or organic solvent or mixtures thereof may be used.
  • An alcohol solvent, e.g. methanol or ethanol may be used.
  • An aqueous solution is preferred.
  • the glass coating composition includes approximately 40 to 70% by weight of polyacrylamide; approximately 30 to 60% by weight of vermiculite; and approximately 0.1% to approximately 0.5% by weight of (N,N-diethyl-3-aminopro ⁇ yl)trimethoxysilane.
  • the glass coating composition may include approximately 80 to 95% by weight of a polyurethane polymer; and approximately 5 to 15% by weight silicon carbide.
  • a toughened article including a glass, article, and a glass coating on at least one surface thereof. formed from a glass coating composition including an effective amount of at least one inorganic or organic polymeric component; and at least one reinforcing agent incorporated therein; the glass coating being such that when coated on the glass article, it strengthens and toughens the article.
  • the glass article may be formed from a silica based glass.
  • the glass article may be formed from a soda-lime type glass.
  • the glass article may be a shaped article.
  • the glass article may be a container such as a bottle, jar or like vessel.
  • the glass article may be subjected to a surface purification step prior to application of the coating.
  • the glass article may be prepared for coating by way of a cleaning or other step as discussed below.
  • the glass coating composition may include approximately 40 to 70% by weight of polyacrylamide; approximately 30 to 60% of vermiculite; and approximately 0.1% to approximately 0.5% by weight of a coupling agent, preferably (N,N-diethyl-3-amino ⁇ ropyl)- trimethoxysilane.
  • a coupling agent preferably (N,N-diethyl-3-amino ⁇ ropyl)- trimethoxysilane.
  • the glass coating composition may include approximately 80 to 95% by weight of a polyurethane polymer; and approximately 5 to 15% silicon carbide.
  • a process for preparing a toughened article including providing a glass article; and a glass coating composition including an effective amount of at least one inorganic or organic polymeric component; and at least one reinforcing component incorporated therein; the glass coating composition being such that when coated on a glass substrate it strengthens and toughens the article; contacting the surface of the glass article with the glass coating composition; and drying the coated glass article so formed.
  • the glass article may be a glass container, preferably a soda-lime type glass container as discussed above.
  • the glass coating composition may be provided in the form of an aqueous solution.
  • the glass coating composition may further include at least one coupling agent.
  • the process for preparing a toughened article may include the preliminary step of mixing the coupling agent with the polymeric component and at least one reinforcing component for a time sufficient to allow the coupling agent to hydrolyse and/or to interact with the reinforcing component prior to contact with the surface of the glass article.
  • the at least one reinforcing agent of the glass coating composition includes
  • the process for preparing a toughened article may further include the preliminary step of subjecting the vermiculite to a conversion process to produce an exfoliated vermiculite.
  • the vermiculite may first be reacted with sodium chloride to form a sodium vermiculite.
  • the sodium vermiculite may then be reacted with an N-butylamine hydrochloride to form the final exfoliated product.
  • the process for preparing the toughened article may include the preliminary step of subjecting the glass article to a surface preparation step.
  • the surface preparation step may include a physical or chemical cleaning step.
  • Various solvents, acidic or basic polishers or etchers may be used.
  • an electrical discharge treatment may be included.
  • the most effective surface preparation step includes a heat treatment step.
  • the glass article is subjected to a firing in air at elevated temperature for a time sufficient to clean the surface.
  • the heated glass may be then subjected to slow cooling, for example at room temperature.
  • the heat treatment step may be conducted at temperatures of approximately 350 to 450 C and above. Preferably a temperature of 400°C is preferred. Lower firing temperatures were found to be ineffective. Similarly, temperatures significantly higher than 450°C are to be avoided as there is a risk of compositional changes in the surface.
  • the glass articles may be stored under dry nitrogen after cleaning.
  • the glass coating composition may preferably be provided in the form of an aqueous solution.
  • the aqueous solution of the glass coating composition may be coated onto the surface of the glass article in any suitable manner.
  • the glass coating composition may be coated onto the surface as a film for example using kiss coating, doctor rolls, gravure rolls, immersion coating techniques or similar techniques.
  • the glass coating composition may be sprayed onto the glass surface in any known manner.
  • the film so formed may then be dried to remove excess solvent. Drying times and temperatures will vary depending, for example, on the composition of the composition and thickness of coating.
  • the drying step may be conducted in air at room temperature for a period of approximately 12 to 48 hours, preferably for approximately 24 hours.
  • the process of preparing the toughened article may further include the further step of curing the coated glass article.
  • the curing step may take any suitable form depending on the cross-linking agent present. Where the natural or synthetic organic polymer is a curable polymer, the curing step may include heating the coated glass article at elevated temperature for a period sufficient to provide substantially complete cure. Temperatures of the order of 75 to 100 C, preferably approximately 80 to 90°C may be used.
  • the strength testing rig used consisted of two rings of different diameters that pressed on each side of the glass surface.
  • the rings were constrained to be coaxial by a suitable jig, which was placed in a standard testing machine (Instron). This test rig was thus a biaxial 4-point bend machine.
  • test slide was coated on the compressive side with transparent adhesive tape so that the pieces could be retained and the origin of fracture confirmed to be within the test ring.
  • Test slides were indented with a Vickers diamond indenter at 1 Kg load so as to make a single flaw that would control the strength of the slide. In all test cases, it was confirmed that the fracture originated at this flaw. The purpose of this procedure was to ensure a reasonably constant base value for the strength of untreated glass, so that the effect of any coating would be immediately apparent. Also, any increase in strength above the base value resulting from any applied coating would represent a toughening effect due to that coating.
  • natural vermiculite is converted to the sodium form by refluxing 400g in 1000 ml water containing 390g sodium chloride for 24 hours. The product is washed with water to remove chloride.
  • the sodium vermiculite is converted to the n-butylamine form by reaction with n-butylamine hydrochloride.
  • the sodium vermiculite is refluxed for 24 hours in a solution consisting of 1000 ml water, 400ml n-butylamine and sufficient (about 400ml) concentrated hydrochloric acid to make the pH 5.2
  • n-butylamine product is repeatedly washed until it swells to several times its original volume. It is then milled in a high-speed blender or stirrer producing high
  • a coating consisting of 60% by weight of polyacrylamide (PAA) , and 40% 5 by weight of a reinforcing filler of exfoliated vermiculite
  • aqueous solution containing 20.75% by weight of P-26 PAA (Cyanamid Corp.) is mixed with 10.7g of 18.47% vermiculite sol and 50g of water.
  • 0.05g of (N,N-diethyl-3-aminopropyl)trimethoxysilane (DEAPTMS) is added as a coupling agent.
  • the DEAPTMS is allowed to hydrolyse and interact with the vermiculite for 24 hours before the mixture is applied to the glass.
  • the mixture is applied to freshly cleaned glass as a 5 film approximately 0.1mm thick by means of a Doctor Blade apparatus.
  • the film is allowed to dry in air at room temperature for 24 hours, then cured at 85°C to render the coating water resistant.
  • the modulus of rupture (MOR) measured for indented uncoated glass slides was 56 ⁇ 2 MPa: the MOR measured for indented slides coated as above was 87 ⁇ 4 MPa, a significant enhancement.
  • Pu/SiC composites were prepared by adding SiC whiskers to freshly mixed PU resin. It was intended to apply composites of 3 different whisker amounts as well as unfilled PU to standard cleaned slides and acid washed slides. SiC whiskers were dispersed ultrasonically in the resin, since simple mixing was ineffective.
  • the quantity of SiC whiskers that could be added to the PU resin was limited to a narrow range by the viscosity requirements of the film spreader.
  • the unreinforced PU coating was applied by brush. The complete coating procedure used was as follows:
  • a glass coating consisting of 94% to 91% by weight of polyurethane, and 6% to 9% by weight of reinforcing filler of silicon carbide whiskers is applied to freshly cleaned container glass.
  • Japan: 0.5 u.m diameter, aspect ratio 10 were added to 91.2g of freshly-mixed two-part liquid polyurethane material
  • 400°C provided with a strength-limiting flaw by indenting at lKg, retiring at 200°C, and coated with the mixture to a thickness of approximately 0.1mm.
  • the test glass specimens were kept at room temperature for 2 hours to allow the coating mixture to set, then heated at 80 C for 2 hours to effect a full thermal curing of the polyurethane.
  • test glass was prepared and coated as above, but using no whiskers in the polyurethane.
  • test glass was prepared as above, but provided with no coating.
  • the area under the stress vs., displacement curves produced for each specimen in the fracture testing rig is a measure of the work of fracture, or toughness of the test specimen.
  • Typical stress vs. displacement curves for uncoated indented glass, indented glass coated with polyurethane only and indented glass coated with polyurethane containing 8.8% by weight silicon carbide whiskers are shown in Figures 1, 2 and 3.
  • the relative areas under the curves are in the ratio 1.0 : 2.1 : 40.0 respectively, so that compared to uncoated glass, the coating of polyurethane alone toughens the glass by a factor of 2.1, while the silicon carbide whisker/polyurethane coating toughens the glass by a factor of 40, a substantial increase.
  • the decay of the stress/displacement curve to zero at a displacement near 1.2mm, for glass coated with silicon carbide whiskers/polyurethane, of which Figure 3 is a typical example, does not represent failure of the test piece, as does the corresponding parts of the curves in Figures 1 and 2.
  • the stress applied by the testing machine was removed because the test piece had deformed (without failure) to such an extent that the testing rig no longer performed its function properly, a further demonstration of the resistance to failure supplied, by this coating. On relief of the stress, the test piece returned to its original form.
  • the largest value of the applied stress observed was used, since no stress at rupture per se could be determined.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
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Abstract

La composition de revêtement de verre décrite contient une quantité efficace d'au moins un composant polymère inorganique ou organique et au moins un composant de renforcement incorporé dans le premier composant, la composition de revêtement de verre étant conçue de sorte que lorsqu'elle est appliquée sur un substrat de verre, elle consolide et durcit l'article.
PCT/AU1989/000196 1988-05-05 1989-05-05 Article de verre WO1989010903A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
AUPI808688 1988-05-05
AUPI8086 1988-05-05

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WO1989010903A1 true WO1989010903A1 (fr) 1989-11-16

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0857700A1 (fr) * 1997-02-10 1998-08-12 Saint-Gobain Vitrage Substrat transparent muni d'au moins une couche mince à base de nitrure ou d'oxynitrure de silicium et son procédé d'obtention

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU2425354A (en) * 1954-01-08 1954-03-11 Monsanto Chemical Company Substantially non-shattering glass articles and method of producing same
US3515579A (en) * 1968-06-21 1970-06-02 Nat Patent Dev Corp Non-fogging transparent material
US3805985A (en) * 1970-10-01 1974-04-23 Mitsui Polychemicals Ltd Resin coated glass article having improved anti-shock durability
US4143181A (en) * 1976-08-03 1979-03-06 Societe Francaise Duco Process for the preparation of a coating for glass or ceramic surfaces
CA1050223A (fr) * 1975-01-03 1979-03-13 Robert Wimmer Methode de fabrication d'elements composites
AU5880280A (en) * 1979-05-31 1980-12-04 Sekisui Kagaku Kogyo Kabushiki Kaisha Plasticized thermoplastic resin for interlayer of laminated safety glass
US4280944A (en) * 1979-05-17 1981-07-28 Mitsui-Nisso Corporation Thermosetting polyurethane resin and coating agent thereof prepared from at least two polyoxyalkylene polyols, blocking agent, chain-elongating agent, cross-linking agent and a mixture of diisocyanates
US4510282A (en) * 1981-01-23 1985-04-09 Skw Trostberg Aktiengesellschaft Aqueous dispersions for coating materials
AU4186085A (en) * 1984-05-02 1985-11-07 Saint-Gobain Vitrage Method and apparatus for spraying a reaction mixture capable of forming a transparent protective layer of high optical quality
US4684694A (en) * 1984-12-06 1987-08-04 Saint-Gobain Vitrage Transparent coating layer with self-repairng and fog-resistant properties which can be utilized on panes

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU2425354A (en) * 1954-01-08 1954-03-11 Monsanto Chemical Company Substantially non-shattering glass articles and method of producing same
US3515579A (en) * 1968-06-21 1970-06-02 Nat Patent Dev Corp Non-fogging transparent material
US3805985A (en) * 1970-10-01 1974-04-23 Mitsui Polychemicals Ltd Resin coated glass article having improved anti-shock durability
CA1050223A (fr) * 1975-01-03 1979-03-13 Robert Wimmer Methode de fabrication d'elements composites
US4143181A (en) * 1976-08-03 1979-03-06 Societe Francaise Duco Process for the preparation of a coating for glass or ceramic surfaces
US4280944A (en) * 1979-05-17 1981-07-28 Mitsui-Nisso Corporation Thermosetting polyurethane resin and coating agent thereof prepared from at least two polyoxyalkylene polyols, blocking agent, chain-elongating agent, cross-linking agent and a mixture of diisocyanates
AU5880280A (en) * 1979-05-31 1980-12-04 Sekisui Kagaku Kogyo Kabushiki Kaisha Plasticized thermoplastic resin for interlayer of laminated safety glass
US4510282A (en) * 1981-01-23 1985-04-09 Skw Trostberg Aktiengesellschaft Aqueous dispersions for coating materials
AU4186085A (en) * 1984-05-02 1985-11-07 Saint-Gobain Vitrage Method and apparatus for spraying a reaction mixture capable of forming a transparent protective layer of high optical quality
US4684694A (en) * 1984-12-06 1987-08-04 Saint-Gobain Vitrage Transparent coating layer with self-repairng and fog-resistant properties which can be utilized on panes

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0857700A1 (fr) * 1997-02-10 1998-08-12 Saint-Gobain Vitrage Substrat transparent muni d'au moins une couche mince à base de nitrure ou d'oxynitrure de silicium et son procédé d'obtention
FR2759362A1 (fr) * 1997-02-10 1998-08-14 Saint Gobain Vitrage Substrat transparent muni d'au moins une couche mince a base de nitrure ou d'oxynitrure de silicium et son procede d'obtention
US6114043A (en) * 1997-02-10 2000-09-05 Saint-Gobain Vitrage Transparent substrate provided with at least one thin layer based on silicone nitride or oxynitride and the process for obtaining it
US6503557B1 (en) 1997-02-10 2003-01-07 Saint-Gobain Vitrage Process for depositing at least one thin layer based on silicon nitride or oxynitride on a transparent substrate

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