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United States Patent (19) (11) 4,172,733 Moritsu Et Al

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United States Patent (19) (11) 4,172,733 Moritsu Et Al United States Patent (19) (11) 4,172,733 Moritsu et al. 45) Oct. 30, 1979 54 VTREOUSENAMEL COMPOSITIONS (56) References Cited U.S. PATENT DOCUMENTS 75 Inventors: Yukikazu Moritsu, Nishinomiya; Kooji Yamada, Kashihara; Masatoshi 3,479,216 1/1969 Counts et al......................... 252/.514 Wada, Izumiotsu; Eiji Munemoto, 4,029,605 6/1977 Kosiorek .............................. 252/514 Hirakata, all of Japan Primary Examiner-Lorenzo B. Hayes Attorney, Agent, or Firm-Armstrong, Nikaido, 73 Assignee: Okumo Chemical Industry Co., Ltd, Marmelstein & Kubovcik Osaka, Japan 57 ABSTRACT 21 Appl. No.: 851,638 A vitreous enamel composition comprising 1 part by weight of a vitreous enamel solid component composed Filed: Nov. 15, 1977 of (1)90-99.9 wt.% of glass powder consisting predom (22) inantly of 40 to 80 wt.% of SiO2, 1-25 wt.% of at least (51) at C’............................................... CO9D 5/38 one of B2O3 and CaO, and 1-20 wt.% of R2O in which (52) U.S. C. .................................. 106/1.15; 106/1.21; R is K, Na or Li, and (2) 0.1-10 wt.% of palladium 106/1.28; 106/54; 252/.514 powder, and 1-20 parts by weight of an organic vehicle. 58 Field of Search .................... 106/1.21, 1.24, 1.28, 106/1.15, 54; 252/514; 427/101, 102, 126 6 Claims, No Drawings 4,172,733 1 2 dium powder, and 1-20 parts by weight of an organic VTREOUSENAMEL COMPOSTIONS vehicle admixed with the solid component. According to this invention it is essential that the This invention relates to vitreous enamel composi vitreous enamel composition contain a glass powder tions, and more particularly to vitreous enamel compo consisting predominantly of 40-80 wt.% of SiO2, 1-25 sitions for undercoating the glass and ceramic articles to wt.% of at least one of B2O3 and CaO, and 1-20 wt.% be electrolessly plated. of R2O in which R is as defined above. The glass pow Generally the surface of glass and ceramic articles der of this invention, although free from any lead com can not be coated by electroless plating when subjected ponent, has a relatively low melting point which is directly thereto. It is therefore necessary to deposition 10 usually about 1000' to about 1250 C. and can be fired at the surface of such an article palladium, silver, gold or a relatively low temperature. Moreover the powder can a derivative thereof to sensitize the surface for electro be fired attemperatures in a wider range than lead glass, less plating. The sensitizing substance must be deposited while retaining the form of glass powder, giving a po on the surface with high adhesion and as uniformly as rous layer of fired glass powder on glass or ceramic possible free of local irregularities. Additionally the 15 articles. Since the glass powder is fired on the surface of layer of the sensitizing material should preferably be the ceramic article, the vitreous layer can be formed as rough-surfaced to the greatest possible extent. adhered thereto with high bond strength. The surface of glass and ceramic articles is usually In this invention, the glass powder of the above com sensitized by applying a sensitizing material directly to position is used conjointly with the organic vehicle in 20 an amount of 1 to 20 times the amount by weight of the the surface (to be hereinafter referred to as "direct cata powder, the amount of the vehicle being exceedingly lyzing method”), by applying a silver paste composed greater than was conventionally used in vitreous enamel of a small amount of silver powder and an organic vehi compositions of this type. Consequently, a rough-sur cle in not more than one half the amount (by weight) of faced layer of the glass powder can be formed uni the silver and firing the resulting coating (to be herein 25 formly on the surface of glass and ceramic articles. after referred to as "silver past firing method”), and by The glass powder of this invention is composed pref. applying a vitreous enamel composition composed of erably of 45-75 wt.% of SiO2, 3-15 wt.% of at least lead glass, an organic acid salt of sensitizing material one of B2O3 and CaO and 5-15 wt.% of R2O. The and a small amount of organic vehicle, followed by composition of the glass powder is determined based firing (to be hereinafter referred to as "glass enamel 30 mainly on the melting temperature of the glass powder, firing method"). the temperature range in which the powder can be With the direct catalyzing method, the adhesion be fired, the adhering properties and strength of the fired tween the sensitizing material and the surface of the layer obtained. With less than 40 wt.% of SiO2 present, article is very low, rendering the electroless coating the fired vitreous layer is liable to corrosion by the adhered to the article only with very low strength. 35 plating bath, with the result that the subsequent plating According to the silver paste firing method, the electro process gives metal coatings of reduced bond strength. less plating is limited only to copper plating which With more than 80 wt.% of SiO2 present, too high a requires the use of large quantities of expensive silver, firing temperature (melting temperature) will be re hence commercially very disadvantageous. The vitre quired, adversely affecting the glass or ceramic article ous enamel firing method has the following drawbacks. 40 perse and producing a tendency to reduce the catalytic Since the glass component used is lead glass which is properties of the palladium powder. Further if the low melting, there is an extreme limitation on the range amount of at least one of B2O3 and CaO is less than 1 wt. of adjustable temperatures for forming on the surface of %, difficulty is likely to arise in melting the glass pow ceramic articles a fired layer in which the lead glass der. Conversely if it is more than 25 wt.%, the resulting retains its particulate form. Frequently, therefore, the 45 vitreous layer will have a reduced chemical stability glass particles per se are fused, giving a smooth-sur and become susceptible to corrosion by the plating bath. faced vitreous layer instead of forming a porous rough Further if R2O is present in an amount of less than 1 wt. surface. Moreover the glass tends to cover the sensitiz %, difficulty is likely to take place in melting the glass ing material, rendering the material less exposed, with powder. With use of more than 20 wt.% of R2O, a the result that the electroless coating, if formed, will 50 reduced chemical stability and increased susceptibility have reduced adhesion thereto. to corrosion by the plating bath will result. An object of this invention is to provide a vitreous Insofar as the above components are used within the enamel composition capable of giving coatings on ranges defined above, at least one or two of BaO, MgO, which platings can be formed with outstanding adhe NaF, ZnO, TiO2, ZrO2, SnO2, Al2O3, BiO3 and Fe2O3 SO. 55 can be used in an amount of up to 20 wt.% in this Another object of this invention is to provide a vitre invention. Among these components, BaO and MgO act ous enamel composition which permits electroless de to promote vitrification, while NaF serves to adjust the position of nickel, cobalt and other metals as well as melting temperature of the glass powder. ZnO, TiO2, copper. ZrO2, Al2O3, Fe2O3, etc., are effective in giving an These and other objects of this invention will become 60 improved chemical stability to the glass powder. apparent from the following description. The glass powder can be produced according to the The vitreous enamel composition of this invention is usual method. For example, a vitreous mixture of the characterized in that the composition comprises: 1 part above composition is melted in the usual manner at by weight of a vitreous enamel solid component com 1300-1600 C. for 1-6 hours and the molten mass is posed of (1) 90-99.9 wt.% of glass powder consisting 65 quenched in water and thereafter mechanically treated predominantly of 40–80 wt.% of SiO2, 1-25 wt.% of at in a ball mill or the like. The resulting slurry is dried to least one of B2O3 and CaO, and 1-20 wt.% of R2O in obtain a cake, which is then pulverized by suitable which R is K, Na or Li, and (2) 0.1-10 wt.% of palla means such as oscillating screen. The glass powder of 4,172,733 3 4. this invention is usually 0.5 to 20, more particularly 0.5 85 wt.% of isopropyl alcohol is well suited to the prep to 10u in particle size. aration of the present composition adapted for coating. According to this invention, a palladium powder is Paste-like thermoplastic compositions amenable to admixed with the glass powder to obtain a vitreous screen printing can be prepared with use of wax-like enamel solid component. Useful palladium powders are 5 vehicles composed of 40-60 wt.% of stearyl or cetyl finely divided metal palladium and inorganic com alcohol and 60-40 wt.% of thermoplastic resin, such as pounds thereof, such as palladium oxide, palladium a wax-like mixture of 40 wt.% of stearyl alcohol, 5 wt. hydroxide, palladium black, etc. Palladium oxide is % of polyethylene glycol (trademark: "PEG-1540,' prepared by the usual manner, for example palladium product of Sanyo Chemical Industries Co., Japan), 2 wt. chloride is heated with sodium nitrate at a temperature 10 % of cellulose resin (“EC-N-22'), 3 wt.% of acrylic of about 600 C.
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