Method and burner for forming silica-containing soot

Glass manufacturing – Processes – With shaping of particulate material and subsequent fusing...

Reexamination Certificate

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C065S414000, C065S416000, C065S421000, C065S531000, C065SDIG008

Reexamination Certificate

active

06260385

ABSTRACT:

FIELD OF THE INVENTION
The present invention relates to the formation of silica-containing soot and articles made from silica-containing soot and, more particularly, to a method and a burner for forming silica-containing soot and articles from liquid silicon-containing compounds.
BACKGROUND OF THE INVENTION
Various processes are known to produce metal oxide soot through the use of burners. The soot can be the end-product itself, or it can be collected on a target to form a porous pre-sintered body which can be subsequently consolidated into a dense body. Alternatively, the soot collected on the target can be simultaneously heat treated to form a dense body. The majority of processes in practice today feed reactants to the burner in vaporous form, which require sophisticated vaporizing and delivering systems. The complexity of the equipment and process control increases substantially when the end products are multicomponent systems, which require separate feed for individual reactants.
Silicon, germanium, zirconium, and titanium metal halides are often used as vaporous reactants in forming metal oxide glasses. For example, hydrolysis of SiCl
4
has been the industry preference for producing high purity silica over the years. The conversion of SiCl
4
into SiO
2
, through pyrolysis and hydrolysis, however, has the disadvantage of producing chlorine or a very strong acid by-product, hydrochloric acid (HCl). Hydrochloric acid is not only detrimental to many deposition substrates and reaction equipment, but also harmful to the environment. Emission abatement systems have proven to be very expensive due to loss and maintenance of equipment caused by the corrosiveness of HCl. As an alternative, high purity quartz or silica has also been produced by thermal decomposition and oxidation of silanes. However, this requires taking safety measures to prevent the violent reaction that results from the introduction of air into a closed container of silanes. Silanes react with carbon dioxide, nitrous oxide, oxygen, or water to produce high purity materials that are potentially useful in producing, among other things, semiconductor devices. However, silanes are much too expensive and reactive to be considered for commercial production of fused silica except possibly for small scale applications requiring extremely high purity.
U.S. Pat. No. 5,043,002 to Dobbins et al., which is relied upon and incorporated by reference, proposed alternative silica precursor materials. This patent disclosed bubbling a carrier gas through a silicon-containing reactant compound, preferably a halide-free compound such as polymethylsiloxanes, in particular, polymethylcyclosiloxanes such as hexamethylcyclotrisiloxane, octamethylcyclotetrasiloxane (“OMCTS”), and decamethylcyclopentasiloxane. A mixture of the reactant compound vapor and nitrogen is transported to the burner at the reaction site, where the reactant is combined with a gaseous fuel/oxygen mixture and combusted. U.S. Pat. No. 5,152,819 to Blackwell et al., the disclosure of which is relied upon and incorporated by reference, describes additional halide-free silicon compounds, in particular, organosilicon-nitrogen compounds having a basic Si—N—Si structure, siloxasilazones having a basic Si—N—Si—O—Si structure, and mixtures thereof, which may be used to produce high purity silica glass without the concomitant generation of corrosive, polluting by-products.
Although the use of halide-free silicon compounds as feedstocks for silica glass production avoids the formation of HCl, some problems remain, particularly when the glass is intended for the formation of high purity bulk fused silica and high quality optical products such as optical waveguides. For example, as disclosed in copending U.S. patent application Ser. No. 08/574,961 entitled “Method for Purifying Polyalkylsiloxanes and the Resulting Products,” which is relied upon and incorporated by reference, the presence of high boiling point impurities in, for example, a polyalkylsiloxane feedstock, can result in the formation of gel deposits in the vaporization and delivery systems carrying the vaporous reactants to the burner or within the burner itself. Such polymerizing and gelling of the siloxane feedstock inhibits the controllability and consistency of the silica manufacturing process. This problem is more prevalent when an oxidizing carrier gas such as oxygen is included in the reactant vapor stream, because oxidizers appear to catalyze polymerization of the siloxane feedstock. Such polymerizing and gelling reduces the deposition laydown rate of the bulk silica soot or soot preform that may be either simultaneously consolidated to form optical members or subsequently consolidated to a blank from which an optical waveguide is fabricated.
An additional problem encountered when silica soot or silica preforms are formed using siloxane feedstocks is that particulates of the high molecular weight, high boiling point impurities may be deposited in the bulk silica soot or collection site, resulting in “defect” or “clustered defect.” Defects or clustered defects are imperfections that adversely affect the optical and structural quality of the optical waveguides formed using the silica soot.
Application Ser. No. 08/767,653, the content of which is relied upon and incorporated by reference, discloses that the clustered defects can be reduced by delivering a liquid siloxane feedstock to a conversion site, atomizing the feedstock at the conversion site, and converting the atomized feedstock at the conversion site into silica. One way to atomize the feedstock at the conversion site involves pneumatically or “airblast” atomizing the liquid siloxane feedstock by delivering the liquid feedstock to the conversion site with an inert gas.
Direct liquid feed to the burner offers many additional advantages such as simplified equipment construction, ease in system operation, reduced production cost, and importantly, capability of producing multicomponent oxide materials with compositions difficult to achieve with the vapor feed burner system.
The challenges for the liquid feed burner design are increasing effectiveness of liquid atomization and reducing turbulence of the flame. For processes such as high purity fused silica lay-down and optical waveguide soot preform formation, the requirements for high deposition rate and uniformity imposes even more strict demand for flame control.
Although atomizing the liquid siloxane feedstock proximate the conversion site using an airblast atomizer reduces clustered defects, such airblast atomization systems presents several further challenges. For example, increasing the atomizing gas velocity desirably produces smaller liquid droplets, which are more readily vaporized and burned in the burner flame. Smaller droplets are desirable because larger droplets cause wart-like defects (“warts”) on the surface of the deposition site. In addition, smaller droplets can be more easily focused with the surrounding gases to produce a more concentrated deposition stream. On the other hand, increasing atomizing gas velocity adds turbulence to the burner flame, which reduces the soot capture rate and can cause other physical defects in the final silica-containing articles made from the soot.
U.S. Pat. No. 5,110,335 to Miller et al. discloses a liquid feed burner using ultrasonic atomizing nozzle. Although liquid atomization by ultrasound can be effective, incorporating an ultrasonic nozzle makes the burner costly and its construction complex. The high temperature environment of certain applications such as the glass manufacturing process may drastically reduce the life of the ultrasound nozzle. In addition, compact burner design is difficult to achieve.
Accordingly, it would be desirable to provide a burner and a method incorporating a liquid delivery system that produces a focused, silica-containing soot deposition stream containing small droplets without the need for high gas velocity. Such a burner and method would desirably provide low burner flame turbulence.
SUMMARY OF THE INVENTION
According

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