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UNITED STATES PATENT OFFICE 2,577,627 GLASS COMPOSITION and METHOD of MAKNG SAME Alexis G

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UNITED STATES PATENT OFFICE 2,577,627 GLASS COMPOSITION and METHOD of MAKNG SAME Alexis G Patented Dec. 4, 1951 is ..." 2,577,627 UNITED STATES PATENT OFFICE 2,577,627 GLASS COMPOSITION AND METHOD OF MAKNG SAME Alexis G. Pincus, Southbridge, Mass., assignor to American Optical Company, Southbridge, Mass., a voluntary association of Massachusetts No Drawing. Application May 1, 1947, Serial No. 745,239 10. Claims. (CI, 106-4) - - - - - This invention relates to fluoride resistant characteristics have been encountered which glasses and has particular reference to a glass have rendered most of these prior art glasses which is highly resistant to attack by hydro commercially impracticable. There are several fluoric acid, anhydrous hydrogen fluoride and characteristics which are required in glasses of fluorides in general, and to improved composi this nature: tions and methods of making the same. (1) That the glass first has a high resistance One of the principal objects of the .invention to attack by hydrofluoric acid, anhydrous hydro is to provide glasses of the above character, in gen fluoride and fluorides in general; proved compositions therefor and methods of (2) That the compositions be such that they making the same, which can be fabricated in O may be readily fabricated by known commercial large scale commercial production by known means; commercial methods and within the usual tem (3) That they possess characteristics which perature ranges, and which possess characteris will enable refabrication by heat or mechanical tics enabling refabrication while retaining a means without loss of desired transparency and transparent homogenous vitreous nature. 5 homogeneity; . A further object is to provide a glass composi (4) That they possess high resistance to attack tion of the above nature consisting essentially of by water; the metaphosphates of metallic elements of low (5). And that they possess desirable and prac atomic weight so that the resulting glass has a tical characteristics as to thermal expansion co relatively high percentage of P2O5 and method 20 efficient and resistance to breakage from thermal of making the same whereby, during melting, a Shock. minimum loss of P2O5 by volatilization will occur Some more recent glasses possessed most of the and which melt can be cooled and fabricated above desirable characteristics, but it has been without harmful tendency to form crystals, ream found that, when attempts have been made to or other loss of homogeneous, transparent, vitre 25 form, large commercial batches of Such glasses, ous characteristics. Some difficulties as to the fabrication of the Another object is to provide a zinc aluminum glasses occurred even though smaller size melts phosphate type of glass containing a controlled could be successfully fabricated. amount of boric oxide. The present invention, therefore, is directed to A further object of the invention is to provide the obtaining of a glass possessing all of the a glass substantially free from attack by fluoride 30 above enumerated desirable characteristics and vapors, hydrofluoric acid, which glass consists which may be made in large commercial melts essentially of phosphorus pentoxide, an ingredi and by known commercial processes or methods. ent or ingredients selected from the group con In Patent No. 2,381,925 issued August 14, 1945 sisting of aluminum oxide and boric oxide and an to applicant, there are disclosed glasses resistant ingredient or ingredients selected from the group 35 to hydrofluoric acid formed by combination of consisting of one or more df the bivalent oxides: P2O5, Al2O3 and ZnO. BeO and PbO were men beryllium oxide, magnesium oxide and zinc oxide, tioned in said patent as equivalents of ZnO. and with or without the addition of minor in Small additions of alkali oxide or fluoride were gredients such as fluorine, alkali oxides and cal mentioned therein also as assisting the melting cium oxide. 40 and Working of such glasses. In said patent it Other objects and advantages of the invention was mentioned that definite attempts were made | will become apparent from the following de to eliminate as far as possible any trace of sili Scription and it will be apparent that many con dioxide (SiO2) or boric oxide (B2O3) for, as changes may be made in the specific formulas, a result of research at that time and with the compositions and methods described herein with proportions of P2O5 and Al2O3 given, such in out departing from the spirit of the invention gredients proved detrimental to the fluoride re as expressed in the accompanying claims. I, sistance of the resultant glass. therefore, do not wish to be limited to the exact It has been found, however, by research and formulas, compositions and methods given herein experimentation that by increasing the P2O5 con as the preferred examples only have been set 50 tent to the upper limits set forth in said patent forth by way of illustration. - and by decreasing the Al2O3 content it now be Fluoride resisting glasses are not new in the comes practical to introduce B2O3 either as a art. Several different attempts have been made substitute for the Al2O3 or for use in combina to provide glasses possessing this characteristic tion therewith, and thereby obtain compositions but, in most instances, one or more undesirable 55 at this high P2O5 level which have better work 2,577,627 3 4. ing characteristics as to large batch fabrication P2O5 content of melt No. 2. The glasses of the and making possible the obtaining of maximum above melts were Subjected to a hydrofluoric acid durability against fluorides. test Such as Will be described in more detail here It has not only been found that, B2O3 may now inafter, and melt No. 2 was attacked at an ap be added without detriment to the glass but that preciably higher rate than melt No. 1 (0.15 as naterial amounts may be added with decidedly compared with 0.10). advantageous resultS. It has also been found In the forming of a glass melt such as given in that, with the proportions of Al2O3 or B2O3 set Example B above, the desired composition may forth herein, the functions of Zno may be exert be derived from a batch consisting of: cised by the use of MgO, BeO and CaO either O Parts by weight separately or jointly, although it is still preferred Aluminum metaphosphate ---------------- 40 to use ZnO as the major bivalent oxide constitu Zinc metaphosphate---------------------- 14 ent. Magnesium metaphosphate --------------- 23 The present invention relates to glass compos Boric acid crystals----------------------- 9 sitions as follows, in which are stated the range 5 and parts by Weight by which the various in Sodium nitrate--------------------------- 2 gredients may be varied and also certain specific Phosphoric anhydride -------------------- 8 examples of actual formulas Within this range It will be noted, that, as far as possible, meta Which have produced desirable results: phosphates are used as the raw materials be 20 cause it has been found that this yields a dry, Parts by Weight Specific easily weighed, and easily mixed batch with a Range of Examples Ingredient Parts by minimum tendency to volatilize the P2O5 during weight melting. The Said batch can be melted in any A. B C ordinary ceramic refractory, through preferably 25 one of the high aluminum type, at a temperature Phosphorus Pentoxide (POs) 72-85 77 77 75 AiLiminuin Oxide (Al2O3).----- 5- 9 8 8 7 of about 2500 F. The melting should be rapid Boric Oxide (BO3).--------. 1-8 5 5 5 and the furnace should not be held at this maxi Bivalent Oxides (RO).------ 1-12 | 10 mum temperature any longer than absolutely OO necessary for complete melting. Boron ortho such as: 30 phosphate is available as a source of B2O3 and Zinc Oxide (ZnO) --------- 5 2 P2O5, and its use makes possible omission of Magnesium Oxide (MgO) 5 3. Beryllium. Oxide (BeO). O O phosphoric anhydride from the batch. Calcium. Oxide. (CaO). O 3.8 The melt can then be dropped to about 2000 Optional Ingredients F. for further homogenization and for working. 35 The best working range has been found to lie Fluorine---------------------- 0- 5 ----------- O 3, 2 Alkali Oxides----------------- 0- Na30 or between 1900 and 2200 E. The Said melt has Li2O O. 0.5 Satisfactory working characteristics and the re Sultant glass can be lamp-Worked Without de 00. 99.5 vitrification of the parent gaSS or Surface grey It will be noted by reference to the above that ing during prolonged heating in a gas fiane. the P2O5 content is relatively high and, according That is, the glass will retain its initial inherent to the present teachings, the higher the amount transparency throughout the melting, Working of P2O5 present, the more resistant the resultant and after Working. The glass also lends itself glass Will be to hydrofluoric acid attack. Well to the usual mechanical methods of shap In forming the glass batches for producing s ing. Such as griniding With loose abrasives, polish such glasses, it is desirable to so select the pro ing with rouge, cutting, edging and drilling. portions of the ingredients that the positive ele Glasses of this nature may also be annealed nients are present in approximately the meta within the usual ranges and cooled slowly from phosphate ratios. In order to maintain a high approximately 1100'. F. by conventional anneal F2O5 content, it has been found best to use, as ing methods. the metallic oxide constituents, elements of low It has been found that the glasses disclosed atomic weight Such as beryllium, aluminum, herein are resistant to a chemical test as follows: boron and magnesium. During the melting it is A weighed test piece is immersed in 48% hy. desirable to melt at a minimum temperature and drofluoric acid at room temperature (usually 26 for the shortest possible time to minimize loss 5 to 27° C., approximately 78° F.) for one hour of P2O5 by volatilization.
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