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United States Patent Office Patented June 26, 1962 1 2 1.91 to About 1.93

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United States Patent Office Patented June 26, 1962 1 2 1.91 to About 1.93 3,041,191 United States Patent Office Patented June 26, 1962 1 2 1.91 to about 1.93. The optimum brilliance is taken in 3,04,191 LARGE DAMETER HIGH REFRACTIVE conjunction with optimum visibility to the observer whose O NDEX GLASS BEADS eye is not too far removed from the axis of the directed Vincent L. Dya d'Adrian, Shrewsbury, Mo., assignor light, such as in the case of an automobile driver who to Flex-O-Lite Manufacturing Corporation, St. Louis, views a reflective highway marking paint. These beads Mo., a corporation of Missouri therefore provide a good range of reflection to the viewer. No Drawing. Filled Mar, 15, 1961, Ser. No. 95,815 Further, the glass beads of this invention find particular 10 Claims. (C. 106-147) utility in applications upon highway paint or outdoor signs for illumination since they withstand attack of sulfur This invention relates to improvements in glass beads 0 containing fumes. Lead oxide containing beads are sub and in particular is concerned with glass beads of special ject to conversion to lead sulfide and a formation of an composition capable of being made of relatively large opaque coating when contacted with such sulfur contain diameter and of high refractive index. The instant ap ing industrial gases which are quite often encountered in plication is a continuation-in-part of my co-pending ap industrial regions. This undesirable attribute of the lead plication, Serial No. 656,772, filed May 3, 1957, now 5 oxide beads has been obviated by the instant invention E. No. 2,980,547, for High Refractive Index Glass through the provision of a large diameter high refractive CaCS. index bead which is not subject to attack by sulphur con The glass beads of this invention find particular utility taining gases. as reflective beads used in highway marking paints, signs, To provide the glass bead composition using the barium and the like, which are adapted to be illuminated at night, 20 oxide, titanium dioxide, boron oxide, and alumina com and for illuminating other surfaces through reflective ponents, conventional chemical components may be em brilliance of a light directed upon the surface. A particu ployed. Thus, barium carbonate, titanium dioxide, boric lar feature of this invention is the provision of a glass acid, and alumina may be used as a source for the raw bead composition that makes possible the manufacture of materials. Barium peroxide may also be employed for its i. beads of increased diameter over those previously 25 capacity as an oxidizing agent and to insure a water white lace. color and as a source of barium oxide to provide a high The glass beads of this invention have a refractive in refractive index component. The above components are dex of about 1.82 up to 2.0, and lie preferably in the readily available in the industry and are easily produced range of about 1.90 to about 1.95 for the desirable re in the usual glass making and bead producing techniques flective brilliance properties. Essentially, the glass bead 30 to provide the improved large diameter glass beads of this composition of this invention for the manufacture of in invention. creased diameter glass beads uses about 49-65% by Accordingly, it is a primary object of this invention to Weight of barium oxide, about 20-40% by weight of ti provide a crystal glass bead having a relatively large tanium dioxide, 6-14% by weight of boron oxide, and diameter up to about one-eighth inch in size and having about 1-11% by weight of alumina. This glass is made 35 reflective characteristics of great brilliance. from charges consisting essentially of about 50-65% bar It is a further object of this invention to provide a trans ium carbonate, 15-33% titanium dioxide, 9-20% boric parent glass bead having a refractive index of about 1.82 acid, up to about 2.5 barium peroxide, and about 0.8- to about 1.95 and upwards and consisting essentially of 9% alumina. barium oxide, titanium dioxide, boron oxide, and alumi The alumina component is an added component in ad 40 ia. dition to the first three mentioned componets which have Still another object of this invention is to provide a glass been disclosed in my prior co-pending application. The bead composition of relatively high diameter up to about alumina is used essentially as a high refractive index com one-eighth inch which has a high refractive index of at ponent which helps prevent devitrification and makes least about 1.82. possible the manufacture of larger beads to provide a 45 Still another object of this invention is to provide a crystal clear or so-called water white glass bead composi improved glass bead composition and high refractive in tion. Such larger beads of previous compositions, in the dex consisting essentially of about 49-65% by Weight of general range of as high as one-eighth inch in diameter, barium oxide, about 20-40% by weight of titanium di are normally slower cooling when used in conventional oxide, about 6-14% by weight of boron oxide, and about manufacturing processes and greater devitrification norm 50 1-11% by weight of alumina. ally occurs. Further objects of this invention will appear in the The conventional high index glass beads used in the in detailed description which follows and will be further ap dustry today are slightly colored and therefore do not have daytime compatibility, since the color of the bead unde parent to those skilled in the art. - sirably changes or masks the color of the surface on which 55 In the production of the high refractive index glass the beads are secured, thereby giving an off-color effect. beads of this invention, it has been an objective to use As a further consequence of the glass bead composition components having a high refractive index which will of this invention, there has been provided a bead which produce a glass bead of clear transparent characteristics. is resistant to sulphur fumes and industrial gases con in the manufacture of such glass beads, there have been taining sulphur such as hydrogen sulfide, sulfur dioxide, 60 used in the novel glass composition, barium carbonate, and the like, which are injurious to glass beads which boric acid, barium peroxide, titanium dioxide, and alu have been previously employed in this field. mina. In some cases the barium peroxide may be elimi Reflective glass beads having a high degree of brilli nated. ance have been described in the Gebhard et al. Patent No. The barium carbonate yields barium oxide in the glass 2,326,634 for use upon roadside signs for night illumina 65 bead composition and is desirably employed as a high tion and upon highway marking paints to provide a bright melting point flux. Additionally, the barium oxide has 1y illuminated surface when the headlight of an automobile a desirably high refractive index of 1.98, which makes shines upon it. However, contrary to the teachings in the it of value in the composition. Gebhard et al. patent, and as a result of this invention, it The boric acid is desirably employed as a low melting has been found that optimum brilliance for reflective glass 70 point flux. The boron oxide has a refractive index of beads is provided at the refractive index range of about 1.464 so that its effect upon the refractive index of the s 3,041,191 3. 4. glass bead composition must be compensated for by the directed light as is the case for an automobile driver. higher refractive index components. Without some reflective angularity, beads which other The titanium dioxide is preferably employed in the wise give very good reflective brilliance, are not visibly rutile form. This form of titanium dioxide has a very reflective when viewed slightly away from the same line high refractive index of 2.7, although it may range from as the path of directed light beam from the illuminating 2.61 to 2.9 in some cases. Thus, the titanium dioxide source to the beads. Thus, when the observer moves is desirably employed as a high refractive indeX com outside the ray of light being presented to the illuminated ponent. surface, no substantial amount of lighted surface can be The bariumperoxide is employed as a desirable oxidiz seen. It has been found in this invention that glass ing agent. The resultant barium oxide in the glass bead 10 beads prepared according to the formulations listed be composition has the same effect as the barium carbonate, low, and having a refractive index in the range of about and the refractive index of 1.98, as mentioned above, is 1.82 up to about 2.0, give a very high degree of brilliance desirable, and, further, the barium oxide finally em coupled with good visibility under the normal conditions ployed as a component in the glass serves as the RO com encountered by an automobile driver whose own head ponent which is a necessary ingredient in glass composi 5 lights light up a highway marking painted strip. Glass tions. - beads of somewhat higher refractive index give a very high The barium peroxide may also desirably be used in degree of brilliance, but relatively poor angular visibility, the formulation to insure crystal clarity and water white such that they are not practicably suitable in highway ness in coloration. In effect, it is used as a safety factor marking paints or on the surfaces of road signs. if off color is to be avoided. As an example in pre 20 The manufacture of the glass is accomplished by melt paring the melt, or in other processes of the formulation ing the glass charge or batch in a conventional glass fur of the glass beads, to avoid the danger of using a reducing nace having a generally closed top with openings for flame which might present an off color, the barium escape of gases.
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