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3% 27017 4 Ttof "E75 3,740,242 United States Patent 0 1C6 Patented June 19,, 1973

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3% 27017 4 Ttof June 19, 1973 / - NI. FAULSTICH ETAL 3,740,242 OPTICAL GLASSES Original Filed Aug. 31, 1966 180 / ' >nd If‘x /\x : 1.75 lx'f/nf‘uu . .I.l 1'70 55 50 45 4D 35 Vd INVDVIOPS: 3% 27017 4 ttOF "e75 3,740,242 United States Patent 0 1C6 Patented June 19,, 1973 :1 2 being greater and in a few cases practically equal to the 3,740,242 Slog-content. OPTICAL GLASSES Marga Faulstich, Mainz, and Willy Ritze, Mainz It will be obvious that it is desirable to eliminate thoria Monbach, Germany from glass compositions, since thoria is often a radio Continuation of abandoned application Ser. No. 1,960, active material. Further and similarly, it will he obviously Jan. 12, 1970, which is a continuation of application desirable to remove beryllia from optical glass composi Ser. No. 576,403, Aug. 31, 1966. This application Mar. tions, since beryllia is toxic, and therefore, a physiologi 4, 1971, Ser. No. 121,167 cally undesirable component. Claims priority, application Germany, Sept. 4, 1965, It has been known in the past to produce thoria- and J 28,924 l0 beryllia-free glasses having optical properties in the same Int. Cl. C03c 3/08, 3/10, 3/30 general range as those indicated to be desirable therefor. US. Cl. 106-54 22 Claims These glasses generally have been prepared with a silica content of at most about 15 percent. In the manufacture ABSTRACT OF THE DISCLOSURE of these glasses, it has been found to be necessary to melt Thorium oxide and beryllium oxide-free glasses suitable 15 the compositions in platinum crucibles and to carry out to continuous melting and production having the follow the production of optical glass from these compositions ing comparative values: in batch operations, since continuous or automatic pro duction could not be accomplished without devitri?cation Index of refraction: Abbe value of the product. 20 It is therefore an object of this invention to provide nd71d 1.750 _____________________________ ..._ __ VdVa 37 a novel glass composition. It is another object of this invention to provide a novel and having a composition: glass composition which can be produced continuously Weight percent and/ or automatically. SiOZ _________________________________ ____ 18.0-23.1 25 It is still a further object of this invention to provide B203 ________________________________ __ 7.6-14.8 a novel glass composition which is free from beryllia 31024-1320, ___________________________ -_ 27.0-33s and thoria as essential components thereof. BaO _________________________________ __ 27.1-46.2 Other and additional objects of this invention will be come apparent from a consideration of this entire speci? La203EEO-P153203 ________________________________ __________________________ _.__ 30.7~-62.9 cation, including the claims appended hereto. CdO ___ ____ _.._ 0.8-—16.1 In accord with and ful?lling these objects, one aspect ZrOz ._ 1.0-3.5 of this invention includes providing a glass composition CClO-l-Zl‘Og ___________________________ __ 23-191) having the following proportions of constituents: 35 Wt. percent This application is a continuation of application Ser. SiOz __ 18-25 No. 1,960, ?led ] an. 12, 1970, which is a continuation of B203 _ _____ 7-15 Ser. No. 576,403, ?led Aug. 31, 1966 both of which are SiO2+B2O3 _____________________________ -_ 23-35 abandoned. BaO ____ __.__ __.._ 27-50 This invention relates to a novel class of optical glasses, La2O3 _____ 3-20 and more particularly refers to such glasses which are stable against devitri?cation and are otherwise an im BaO'l‘La203CdO _________________________________ __._.. 0.5-18 provement over glasses provided by the prior art. ZrOZ _ 0.5-5 It is known to produce optical glasses having various CdO-i-ZrOz _____________________________ -5 2-23 indices of refraction and Abbe values. It is further known ‘to produce glasses having as the upper value of their re It is also possible to add up to 6 weight percent, pref fractive indices and Abbe values: erably no more than 5 weight percent, of TiO; and/or Ta2O5 to the glasses, thereby improving the chemical sta nd 1.761 vdVd 41 50 bility and resistance to devitri?cation. The TiOg-content should best amount to from 2 to 4 weight percent on ac~ n, 1.750 v, 37 count of a possibly undesirable yellow coloration. The addition of up to 1 weight percent of A1203 and/ or W03 These known glasses generally contain thorium oxide is also permissible. and/or beryllium oxide and, in fact, are often of the With the use of the glass composition as stated above, following compositions: 55 it has been found that optical glasses are produced which (a) Alkaline earth (preferably CaO)—lanthanum borates, are extremely stable against devitri?cation and are suit silica-free or with a silica content equal to or less than able for continuous and/ or automatic production. The 15 weight percent, the lanthanum oxide content being production may be of parisons and/or gobs, and further, the composition of this invention can be fused in rela greater than 20 weight percent, plus additions of biva 60 tively large quantity into shaped objects of high optical lent oxides such as ZnO, PbO and CdO 50 weight per quality. It has been found that the glass of this invention cent, plus stabilizing oxides such as Al2O3, ZrOg, TiO'g, has a viscosity of at least about 1200 poises in its plastic Ta2O‘5 and W0, in small quantities. condition during working of the parisons or gobs directly (b) Alkaline earth borates (preferably BaO)-lanthanum from the melt. silicoborates, the lanthanum oxide content amounting 65 According to another aspect of this invention, it has to between 20 and 30 percent when the Bat) content been found practical to replace up to about 8 weight per is less than 50 percent. A stabilization of these glasses cent of the barium oxide, preferably up to about 5 weight against devitri?cation would be achieved either with percent of the barium oxide, with calcium oxide, 3 to 15 percent Th02 or with 2 to 15 percent BeO. strontium oxide, zinc oxide and/or up to about 2 weight 70 The above-listed compositions contain B202 and Si02 percent magnesia. Thus, it may be practical to substitute as glass formers, the percentages of boric acid by weight a more inexpensive constituent or mixture of con 3,740,242 stituents for what has heretofore been considered to be thus producing a charge for a 7-liter melt having the fol an essential components. lowing proportions: Further, where the Abbe values are desirably less than Oxides: Weight percent 42, it is necessary to provide at least about 5 percent of SiOZ _________________________-_________ 18.0 lead oxide in the composition. Lead oxide can be present 9.0 in proportions of up to about 18 percent, if desired. 5 B203 _______________-..__________________ Understanding of this invention will be facilitated by BaO _________________.______._______.._.___ 38.1 reference to the accompanying drawing which is a PbO ___________________________________ graphical representation of the physical properties of various glasses made according to this invention. In this 10 La2O3 _______________________________..__ 17.8 drawing, the arrows indicate the area in which devitrili ZI‘OZ __..._______._____.._-__...____..._______.___ 3 3 cation glasses can be made. The X’s indicate various co . - Ti02 ___________________________________ 1.9 positions within the scope of the invention which are 1.5 similarly devitri?cation-resistant. T3205 .__.____.____.....__._._...__.______..________ W03 ____________________________________ 0.3 The following examples are given by way of illustration 0.3 of this invention only, and should not be construed as 15 AS203 __.__.._....__.__.____....__._.___._....._____.._.__..._ being in any way limiting upon the scope thereof. All lIn a similar manner, the compositions set forth in the parts and percentages are by weight, unless speci?ed to following Table I have been formulated as optical glasses the contrary. having the indices of refraction and Abbe values also in In the production of glass according to each of these dicated in Table I. TABLE I Example N0______ 10 11 12 Oxide: “98526M1“85904910 examples, the following procedure was used: As is illustrated by the examples, the glass of the in Iron-free raw materials of the greatest possible purity vention is thorium oxide and beryllium oxide-free optical are used for all optical glasses. The cationic oxide con glass which can be fabricated by continuous or automatic tents of each raw material are determined analytically production without devitri?cation, consisting essentially before use. The weighed-out batch is mixed in a com 40 of the following composition: mercial-type mixer for 5 minutes. The well-mixed batch Weight percent is set in a platinum crucible for about 6 hours at 1270° SiO2 _____-_____________________________ l8—23.1 C., and then clari?ed at 1300° C. for 2.5 hours. The melt B203 --__________.--.___...._.__-__---_..._-_-_ 7.6—14.8 is homogenized by introducing an agitator into the melt siO2+B203 .._.___.___...._._..__._____._..._____._.__... 27—33.8 and stirring it for about 75 minutes from 1280° c. to 45 BaO ______-____________________________ 27.1-46.2 1605° C. at 120 rpm. The melt can be cast at 1060° C. La2O3 .._...____._____._._________.....____._____...... 3.6-19.2 into block glass in a preheated pot mold, or fed as gobs or BaO-l-La2O3 ..___________________________ 10-315 parisons to a corresponding blow table or parison mold CdO ________.._______.________________..__.
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