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C2a, Ca-Réc24 Neys Jan. 20, 1942. C. J. KINZE ET AL Re. 22,011 METHOD OF MAKING ENAMELYNARE Original Filled Nov. lo, l938 2 Sheets-Sheet l A7 C2 M A2 CalAAa a -5, a Y2%244CAA a 72.2/70-s, a 22%2a4CAAa A.S. a t 22, 2a24/AA 4 - M/a TO 65 t A O O 2 30 A SO 60 TO AWA/6A/7 AW 664/75 AFa S2. A 7. // 6.2. so | | P|| ||2. -20% (2A4Aa a -s a s | 2NN A% oaaa/AAA a 742.72 - S. a. to H2214-N SN-2evo24cz as a HZ24-1ES A2 (AAC/A/Aa. A Zapa -s, a NS. 68 AZZ7 4-1 || || 22% eac/a/aa a -My, a | AA || || || N/AS. s. A || Q to FEEETTT O IO 20 so 40 50 66 O (UAFAaa/7 /W 6aa/?s aata S4. a7. CA/a1a/as M A7222222NVENTOrs cazzas coz72025, a. C2a, Ca-réC24 NEYs Reissued Jan. 20, 1942 Re. 22,011 UNITED STATES PATENT OFFICE 22,011 METHoo of MARINGENAMELWARE Charles J. Kinzie and Charles E. Commons, Jr., Niagara Falls, N.Y., assignors to The Titanium Alloy Manufacturing Company, New York, N.Y., a corporation of Maine Original No. 2,249,007, dated July 15, 1941, Serial No. 239,772, November 10, 1938. Application for reissue October 22, 1941, Serial No. 416,134 19 Claims. (C. 91-3) Our invention relates to the production of im degree of acid resistance of enamelware made proved coatings of white enamels and glazes on from frits containing the same, sheet metal, more particularly vitreous enamels Opacifier .-Cerium oxide. This material is on a sheet iron base, - used to a limited extent as a mill addition Opac We have discovered a novel process of enamel ifier. In some enamels percentages of 6% are ing iron, particularly sheet iron, whereby here as effective as 6% tin Oxlde. tofore unknown and advantageous results in wit The reflectance values for each enamel were reous enamel coatings are attained. One fea determined by means of a reflectometer, and ture of our improved enameling methods con are shown in graphical form in the drawings, sists in the discovery that certain zirconium ox O with the percentage mill additions for each opac ides and other opacifiers can be used as mill ad ifer also charted to show the reflectance results dition opacifiers in percentages considerably of each test, he term reflectance is used to higher than heretofore, with unexpected bene conform with modern nomenclature, and in this ficial results in the enamelware produced. case may be taken to indicate the degree of The opacifiers tested in the practice of this opacity or covering power. The visual results invention are as follows: as seen by the eye conform to the reflectance Opacifter A-The zirconium oxide opacifying readings in this series as shown. composition described in the pending applica In the drawings, Figure 1 is a graphical pres tion for patent fled by Charles J. Kinzie Novem entation of the reflectance figures for the enam ber 1, 1938, Serial No. 238,139, which composition 20 els described in Example 1. Figure 2 is a graph consists of over 98% ZrO2 crystals essentially free ical presentation of the reflectance figures for from alkali-metal compounds and is of particle the enamels described in Example 2. Figure 3 size range of 0.40 to 0.90 micron intimately as is a graphical presentation of the reflectance sociated with a dried gelatinous zirconium pre figures for the enamels described in Example 3. clpitate. Figure 4 is a graphical presentation of the re Opacifter B-The zirconium oxide white opac 5. flectance figures for the enamels described in ifying composition described in Example B of Example 4. In the graphs, the letters A, B, C, U. S. Patent No. 2,102,627 of December 21, 1937. D, E, G, H and refer to the opacifiers similar This opacifier contained 88.06% ZrO2. ly identified hereinafter. The letters "S.P.' re Opacifier C.-A high grade tin oxide contain 3) fer to enamels produced in accordance with the ing in excess of 99% SnO and of the grade present invention, while the letters "N. P.' refer usually used in modern tin oxide enamel opaci to enannels produced in accordance with prior fying. art methods. In view of the fact that information available Opacifier D-The zirconium oxide opacifier to the trade is based on enameling tests with described in U. S. Patent No. 1,588,476 of June either tin oxide or zirconium oxide D or zir 15, 1926, to Kinzie, representing the most suc conium oxide B in percentages up to about 5 or cessful commercial zirconium oxide opacifier up 6%, it is not surprising that the effectiveness to quite recent times. of zirconium oxide B in the higher percentages Opacifier E-This consists of a mixture of 75 has not until this time been discovered, and the parts by weight zirconium oxide, Opacifier A, and (0 import of such discovery in developing a new 25 parts by weight of zinc oxide, the latter being enameling technique has not until this time been essentially free from load and sulfur and sul disclosed. fates. In modern enameling, the practice is to add Opacifier G-A type of zirconium oxide opaci not in excess of about 3% of the opacifier at fying material with an appreciable silica content the mill along with clay, water, etc. to a so and containing 1 to 2% of water rather firmly called superopaque frit, mill the charge to about fixed by the zirconium or zirconium and silica, 6 to 12 grams residue on a 200 mesh sieve from This HaO is released at enamel firing tempera a 100 cc. slip, and apply the slip in two coats tures, and produces a HaO gas bubble opacity in at a total rate of from 55 to 65 grans per square addition to that produced by the zirconia com SO foot. In one coat practice, the mill addition plex. opacifier is increased to from 4 to 6%, milled to Opacifier H.--Titanium dioxide of the grade the same fineness, and is applied at the rate of generally used as a paint pigment. This mate about 45 to 50 grams per square foot in one coat. rial is the most powerful of the paint pigments 55 Reflectance results ranging from 68 to about 72 in pigmenting effects. In enamel manufacture are possible at these rates of application in mod it is often used in the frit batch, due to the fact ern practice. that it is a flux in silicate melts, and has the With the foregoing background, we decided effect of lowering the melting point of the melt that enameling results could be improved by tak and in many cases has a specific effect on the 60 ing advantage of the fact that zirconium oxides, 2 22,011 such as those identified above as Opacifiers A and with mill additions of from 2 to 4 percent tin B, are capable of continuing to increase opacity oxide or zirconium oxide type B. when used as an addition at the mill in amounts Ename formula-Rauty batch (parts by weight) of over 5% and so produce enamelware with the desired reflectance with low enamel application Feldspar ------------------------------- 49.0 rates. Accordingly, we made millings with 10 to Quartz powder-------...-a, -...------------ 5.60 5% and 20% of zirconium oxide B, along with Borax --------------------------------- 28.2 7% clay, A% magnesium carbonate and Water, Sodium nitrate-------------------------- 5.00 to the fineness as in regular commercial use. Sodium carbonate----------------------- 4.87 Upon applying the enamel slip to ground-coated O Cryolite -------------------------------- 20 sheet iron and firing the same, however, we Sodium antinonate --------------------- 16.00 found that the surface was not passable, the Fluorspar ------------------------------ 5.00 enamel had not smoothed out, doubtless due to inc oxide------------------------------ 2.40 the effect of the refractory ZrO2 adjacent to the Calcium carbonate---------------------- 1.8 frit particles in rendering the same more refrac Titanium oxide------------------------- 4.00 tory, with the result that these enamels did not Sodium silico fuoride--...--------------. 4.00 smooth out to the lustrous finish obtained with The raw materials are we mixed and charged an enamel of the same degree of fineness but to the earne frit netting inace at a ten having a lower opacifier addition. perature of about 250 F., ind melted down to After a considerable amount of tests and ex the point where the raw materials combine to perimentation, we found that if the frit in the form a uniform eit which is poured into Water charge carrying the high zirconium oxide B to quench and for the frit, which is the dred. opacifier addition was reduced by milling to a Such frit is of the following calculated compo particle size considerably finer than normally sition: used, or to a point where over 95% by weight of Percent all the frit particles were at or below 44 microns Na2O--KaO ------. - - - - - - - - - - -- a- or a as ran a- - -- 1- 19.19 in size, such an enannel slip could be sprayed onto CaFa ---------------------------------- 4.68 metalware in exceedingly thin coatings and fired . Na3AFe ------------------------------- 12 to highly iustrous surfaces having high re ZnO ---------------------------------- 2.25 fiectance with a white color and a degree of re 30 Sb2O5 --------------------------------- 12.56 sistance to mechanical abuse far in excess of BO ---------------------------------- 9.4 any enamel produced by modern methods. We SiO2 --------------------------------- 3.16 also were surprised to find by calculations that TiO2 ---------------------------------- 3.74 the high mill addition opacified enamel in thin AlO -------------------------------- 8.62 coats was more economical, and that in compar ing the raw material costs of our improved meth CaO - ....
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