CN1318038A - Method of making soot for optical fiber preforms and preforms made therefrom - Google Patents
Method of making soot for optical fiber preforms and preforms made therefrom Download PDFInfo
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
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- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
- C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
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- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
- C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
- C03B37/01413—Reactant delivery systems
- C03B37/0142—Reactant deposition burners
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- C03B2201/00—Type of glass produced
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- C03B2201/30—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi
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- C03B2201/30—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi
- C03B2201/32—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi doped with aluminium
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- C03B2201/30—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi
- C03B2201/34—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi doped with rare earth metals, i.e. with Sc, Y or lanthanides, e.g. for laser-amplifiers
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- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/06—Doped silica-based glasses
- C03B2201/30—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi
- C03B2201/34—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi doped with rare earth metals, i.e. with Sc, Y or lanthanides, e.g. for laser-amplifiers
- C03B2201/36—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi doped with rare earth metals, i.e. with Sc, Y or lanthanides, e.g. for laser-amplifiers doped with rare earth metals and aluminium, e.g. Er-Al co-doped
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/06—Doped silica-based glasses
- C03B2201/30—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi
- C03B2201/40—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi doped with transition metals other than rare earth metals, e.g. Zr, Nb, Ta or Zn
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/06—Doped silica-based glasses
- C03B2201/30—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi
- C03B2201/50—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi doped with alkali metals
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- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/06—Doped silica-based glasses
- C03B2201/30—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi
- C03B2201/54—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi doped with beryllium, magnesium or alkaline earth metals
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- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2207/00—Glass deposition burners
- C03B2207/30—For glass precursor of non-standard type, e.g. solid SiH3F
- C03B2207/32—Non-halide
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2207/00—Glass deposition burners
- C03B2207/30—For glass precursor of non-standard type, e.g. solid SiH3F
- C03B2207/34—Liquid, e.g. mist or aerosol
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2207/00—Glass deposition burners
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Abstract
Description
发明的领域field of invention
本发明涉及用于制造玻璃的煤烟的形成方法,更确切地说,涉及将液体前体和其他反应物送入火焰制成用于制造光导的煤烟的方法,以及由该方法制成的光导。This invention relates to methods of forming soot for use in the manufacture of glass, and more particularly to methods of feeding liquid precursors and other reactants into a flame to form soot for use in the manufacture of light guides, and the resulting The light guide.
虽然本发明可应用于范围广泛的玻璃煤烟用途,但是它尤其非常适于将煤烟沉积到一个目标物上,形成用于制造光导纤维的预制品,下面将在这方面进行具体描述。While the present invention is applicable to a wide variety of glass soot applications, it is particularly well suited for depositing soot onto a target to form a preform for the manufacture of optical fibers, as will be described in more detail below.
发明的背景background of the invention
本行业内已知有多种方法,涉及由气态反应物制备氧化物,尤其是金属氧化物。这种方法需要一种原料溶液或前体、一个产生并输送气态原料液(下面称为气态反应物)和一种氧化剂到转变反应的部位(本行业内的技术人员也称为煤烟反应带或燃烧带)的装置、一个同时对氧化和燃烧催化以制成称为煤烟的细微球状聚集体的装置。这种煤烟可以以任意方式,从在收集室内的捕获直到旋转轴上的沉积,来进行收集。收集的煤烟可以即刻或随后进行热处理,形成高纯度的无孔透明玻璃制品。这种方法通常用具有独特的喷嘴、注射器、燃烧器和/或燃烧器组件所排列的专门设备来进行。Various methods are known in the art involving the preparation of oxides, especially metal oxides, from gaseous reactants. This method requires a raw material solution or precursor, a gaseous raw material liquid (hereinafter referred to as gaseous reactant) and an oxidizing agent to the conversion reaction site (also known as soot reaction zone by those skilled in the art or combustion zone), a device that simultaneously catalyzes oxidation and combustion to produce fine spherical aggregates called soot. This soot can be collected in any manner, from capture in the collection chamber to deposition on the rotating shaft. The collected soot can be immediately or subsequently heat treated to form a high-purity, non-porous, transparent glass product. This method is usually carried out with specialized equipment having unique nozzles, injectors, burners and/or burner assembly arrangements.
许多使这种方法得以发展的起始研究都集中于制备整体氧化硅玻璃。选择合适的原料是该工作的重要方面。因此,那时就确定了能够在低于约100℃的温度下产生200-300毫米汞柱(mmHg)蒸汽压的材料,就可用来制备所述整体氧化硅玻璃。四氯化硅(SiCl4)的高蒸汽压说明它可用作形成煤烟的方便蒸气源,结果推动了这个发现后来就使用了一系列相似的卤化物基原料。与任何其他因素相比,这个因素更多地导致了目前接受的使用SiCl4、GeCl4、POCl3和BCl3作为原料蒸气源。Much of the initial research that led to the development of this method focused on the preparation of monolithic vitreous silica. Choosing the right raw materials is an important aspect of the job. Thus, at that time it was identified that a material capable of producing a vapor pressure of 200-300 millimeters of mercury (mmHg) at a temperature below about 100°C could be used to make the monolithic vitreous silica. The high vapor pressure of silicon tetrachloride (SiCl 4 ) suggested that it could be used as a convenient source of vapors for the formation of soot, a discovery that subsequently led to the use of a series of similar halide-based feedstocks. More than any other factor, this factor has contributed to the currently accepted use of SiCl4 , GeCl4 , POCl3 , and BCl3 as feed vapor sources.
然而,使用这些和其他卤化物基的原料作为蒸气源有其缺点。主要的缺点是形成盐酸(HCl)作为氧化的副产物。盐酸不仅损害沉积基材和反应设备,而且对环境也有害。为了克服这个缺点并由于其它原因,导致了使用非卤化物的化合物作为制备光导用煤烟的前体或原料。However, the use of these and other halide-based feedstocks as vapor sources has its drawbacks. The main disadvantage is the formation of hydrochloric acid (HCl) as a by-product of oxidation. Hydrochloric acid not only damages deposition substrates and reaction equipment, but is also harmful to the environment. In order to overcome this disadvantage and for other reasons, non-halide compounds have been used as precursors or raw materials for the preparation of photoconductive soot.
虽然使用非卤化物的硅化合物作为制造熔凝氧化硅玻璃的原料避免了盐酸的形成,例如如美国专利No.5,043,002和5,152,819所述,但是仍存在其他的问题,当煤烟用来制备光导时,尤其如此。已经发现:在输送蒸汽状的聚烷基硅氧烷蒸气至燃烧器过程中,在输送气态反应物至燃烧器的输送管线中或在燃烧器内,高分子物质会以凝胶形式沉积下来。这会导致随后固结成为供拉制光导纤维的预制品的煤烟的沉积速率减小。这也常常会使从预制品中产生缺陷,结果由其形成的光导纤维就有缺陷乃至不能使用。采用硅氧烷原料制成氧化硅煤烟时遇到的另一个问题,是含有高分子量和高沸点的颗粒沉积在光导纤维预制品上。这些颗粒的形成会导致“缺陷”或“聚集缺陷”,它会对用氧化硅煤烟制成的光导的光学质量和结构质量产生有害作用。Although the use of non-halide silicon compounds as raw materials for making fused silica glass avoids the formation of hydrochloric acid, for example as described in U.S. Pat. , especially so. It has been found that during the delivery of vaporous polyalkylsiloxane vapors to the burner, in the delivery lines for the gaseous reactants to the burner or within the burner, polymeric substances are deposited in the form of gels. This results in a reduced deposition rate of soot that subsequently consolidates into a preform from which optical fibers are drawn. This also often creates defects from the preform, with the result that the optical fiber formed therefrom is defective or even unusable. Another problem encountered in making silica soot from siloxane feedstocks is the deposition of particles containing high molecular weight and high boiling points on optical fiber preforms. The formation of these particles leads to "defects" or "aggregate defects" which can have a detrimental effect on the optical and structural quality of lightguides made from silica soot.
其他一些原料,其中有些目前可用于,而其中另一些可能用于形成制造光导用的煤烟,现在还没有接受用来代替卤化物基和上述非卤化物原料通过气相沉积进行输送。例如盐和那些称为稀土元素的物质,其蒸气极其不稳定,常常在可以输送之前就在蒸气态分解了。这些成分会形成固体自溶液中析出,而不是自燃烧器作为气被输送。Other materials, some of which are currently available and some of which may be used to form soot for the manufacture of light guides, are not currently accepted for delivery by vapor deposition in place of the halide-based and non-halide materials described above. For example, salts and those substances called rare earth elements, whose vapors are extremely unstable, often break down in the vapor state before they can be transported. These components will come out of solution as solids rather than being delivered as gas from the burner.
虽然常常可能将至少一定百分比的该成分作为蒸气输送到燃烧带,但是技术上很困难。必需具有装有昂贵设备的精巧系统,将这些成分转化成蒸气,并进一步将它们输送到燃烧带,而在通向燃烧器的输送管线中和燃烧器自身内不会留下固体沉积物。另外,如果多种成分以蒸气形式输送,而且对于所要求的玻璃组合物又要求每种成分是一定百分数,那么就很难控制输送以保证提供该百分数的蒸气混合物,因为不同的成分具有不同的蒸汽压。While it is often possible to deliver at least some percentage of this component as a vapor to the combustion zone, it is technically difficult. It is necessary to have elaborate systems with expensive equipment to convert these components into vapors and transport them further to the combustion zone without leaving solid deposits in the delivery lines to the burners and in the burners themselves. In addition, if multiple components are delivered in vapor form, and a certain percentage of each component is required for the desired glass composition, it is difficult to control the delivery to provide that percentage of the vapor mixture because different components have different vapor pressure.
美国专利申请No.08/767,653揭示:将原料以液体形式输送到注射器或燃烧器,使原料雾化形成含有液态原料微滴的气雾,并在燃烧带将雾化的液态原料转化成煤烟,就能够克服这些和其他的缺点。美国专利申请No.08/767,653揭示的注射器、燃烧器和燃烧器组件,靠很细小的喷孔输送细流液体来进行合适的雾化。因为原料是以液态直接送入燃烧器火焰,而不是蒸气状态,所以原料的蒸汽压就不再是输送的限制因素。因此,现在,许多其他的成分就能够作为原料或掺杂物进行输送,以便形成用于制造光导的煤烟。U.S. Patent Application No. 08/767,653 discloses: feeding the raw material in liquid form to an injector or burner, atomizing the raw material to form an aerosol containing liquid raw material droplets, and converting the atomized liquid raw material into soot in the combustion zone , these and other disadvantages can be overcome. US Patent Application No. 08/767,653 discloses injectors, burners and burner assemblies that rely on very fine orifices to deliver a fine stream of liquid for proper atomization. Because the feedstock is fed directly to the burner flame in a liquid state, rather than in a vapor state, the vapor pressure of the feedstock is no longer the limiting factor for delivery. Therefore, many other components can now be delivered as raw materials or dopants to form soot for the manufacture of light guides.
然而,许多成分,尤其是那些一般属于盐的成分,并不容易作为有机金属化合物以液态输送到火焰。所要求的纯度常常极其高,而获得所要求这种纯度的化合物的措施在成本上是很高的。However, many components, especially those generally classified as salts, are not readily transported to the flame as organometallic compounds in liquid form. The required purity is often extremely high, and the steps to obtain the compound at the required purity are cost prohibitive.
因此,需要一种制造用于制备光导的煤烟的方法,具体说就是制备光导纤维预制品的方法,该方法能够精确控制被输送各成分的量,同时避免在输送管线中产生凝胶。进一步讲,所需要的是可制成含有所需化学计量的金属氧化物、常规掺杂物和盐的玻璃煤烟,而不需要昂贵和精巧设备的液态输送方法。Accordingly, there is a need for a method of making soot for use in making optical guides, and in particular optical fiber preforms, that precisely controls the amounts of components being delivered while avoiding gel formation in the delivery lines. Further, what is needed is a liquid delivery method that can produce glass soot containing the desired stoichiometric amounts of metal oxides, conventional dopants and salts, without the need for expensive and elaborate equipment.
发明的概述Overview of the invention
本发明涉及输送液体和其他反应物至邻近燃烧器组件的燃烧带以制成用于制备玻璃的煤烟的方法。在液体输送系统中,提供能由热氧化分解转变为玻璃的液体反应物,并直接引入燃烧器的燃烧带,由此形成无定形态的微细无定形煤烟。这种液体输送系统的例子在以下专利申请中有描述:1996年10月17日申请、名称为“由液体反应物的燃烧形成熔凝氧化硅的方法和设备”的美国专利申请No.08/767,653;1997年7月30日申请、名称为“采用氧气燃烧液体反应物形成氧化硅的方法”的美国专利申请No.08/903,501;1998年6月3日申请、名称为“采用加热器燃烧液体反应物形成氧化硅的方法和设备”的美国专利申请No.09/089,869;1997年10月19日申请、名称为“制备金属氧化物煤烟的燃烧器和方法”的美国临时专利申请No.60/068,255和1998年7月31日申请、名称为“制备用于制造玻璃的煤烟的设备和方法”的美国临时专利申请,这些专利申请的说明书都参考结合于此。无定形的煤烟能够以任意的方法收集,但一般是沉积到一个接收器表面,在该表面上或者基本与沉积同时或者在沉积之后,将煤烟固结成熔凝玻璃体。然后,该玻璃体可以直接制成制品,或者可以对熔凝体进一步进行处理,例如拉伸形成光导如制成光导纤维,这在例如名称为“纯化聚烷基硅氧烷和所形成制品的方法”美国专利申请No.08/574/961中进一步有所叙述,其说明书参考结合于此。The present invention relates to a method of delivering liquids and other reactants to a combustion zone adjacent a burner assembly to produce soot for glass production. In the liquid delivery system, the liquid reactant that can be transformed into glass by thermal oxidative decomposition is provided and directly introduced into the combustion zone of the burner, thereby forming fine amorphous soot in an amorphous form. Examples of such liquid delivery systems are described in the following patent application: U.S. Patent Application No. 08/1996, entitled "Method and Apparatus for Forming Fused Silica by Combustion of Liquid Reactants," filed October 17, 1996. 767,653; U.S. Patent Application No. 08/903,501, filed July 30, 1997, entitled "Method of Combusting Liquid Reactants to Form Silicon Oxide Using Oxygen"; U.S. Patent Application No. 09/089,869, "Method and Apparatus for Forming Silicon Oxide from Liquid Reactants"; U.S. Provisional Patent Application No. .60/068,255 and US Provisional Patent Application, filed July 31, 1998, entitled "Apparatus and Method for Making Soot for Glassmaking," the specifications of which patent applications are hereby incorporated by reference. The amorphous soot can be collected by any method, but is generally deposited onto a receiver surface where the soot is consolidated into a fused glass body, either substantially simultaneously with or after deposition. This glass body can then be directly formed into an article, or the fused body can be further processed, such as stretched to form a light guide, such as an optical fiber, as described, for example, in the article entitled "Methods for Purifying Polyalkylsiloxanes and Formed Articles." is further described in U.S. Patent Application No. 08/574/961, the specification of which is incorporated herein by reference.
本发明的方法与本行业内已知的其他玻璃煤烟的制造方法相比,有许多优点。本发明能够精确改变并控制所形成煤烟的组成,从而可提供具有很好确定的非常准确的指数变化剖面以及其他特性的光导纤维。本发明还为工业提供一种同时可输送很多种类的成分进入火焰制成多组分玻璃煤烟的方法。任意多种的有机金属、稀土元素并且现在盐类能够全部同时输送进入火焰,制成均匀的煤烟。相似地,这些成分能够同时或有选择地在同一煤烟制备程序中进行输送,以便制成满足特定层状需求的预制品。因此,用本发明方法制成的光导纤维预制品就具有各成分含量精确的优点,其中有些成分从没有在单个光导纤维预制品中存在过。The method of the present invention has many advantages over other glass soot manufacturing methods known in the industry. The present invention enables precise variation and control of the composition of the soot formed, thereby providing optical fibers with well-defined and very accurate exponential profile and other characteristics. The present invention also provides the industry with a method for simultaneously delivering many types of components into a flame to produce multicomponent glass soot. Any number of organometallics, rare earth elements, and now salts can all be delivered simultaneously into the flame, creating a uniform soot. Similarly, these components can be delivered simultaneously or selectively in the same soot preparation process to produce preforms meeting specific layer requirements. Therefore, optical fiber preforms made by the method of the present invention have the advantage of precise amounts of components, some of which are never present in a single optical fiber preform.
为了获得这些和其他优点,要将一种非水性液体反应物和一种水溶液进行雾化,形成由许多液滴组成的气雾。该气雾被送入燃烧带,并在燃烧带的火焰内反应,形成细微的玻璃煤烟颗粒。To achieve these and other advantages, a non-aqueous liquid reactant and an aqueous solution are atomized to form an aerosol of liquid droplets. This aerosol is fed into the combustion zone where it reacts within the flames of the combustion zone to form fine glass soot particles.
在本发明的另一方面,非水性液体反应物和水溶液被输送到燃烧器组件。非水性液体反应物和水溶液从燃烧器组件排放进入火焰,它们在火焰中进行反应,形成煤烟。煤烟沉积到目标物上,形成预制品。In another aspect of the invention, a non-aqueous liquid reactant and an aqueous solution are delivered to the combustor assembly. The non-aqueous liquid reactant and aqueous solution are discharged from the burner assembly into the flame where they react to form soot. The soot is deposited onto the target, forming a preform.
在本发明的又一方面,用输送非水性液体反应物和水溶液至燃烧器组件的方法,制成光导纤维预制品。非水性液体反应物和水溶液以气雾的形式从燃烧器组件排放进入火焰,该气雾由许多非水性液体反应物液滴和许多水溶液液滴组成。液滴在火焰内反应,形成煤烟而沉积到目标物上,成为预制品。In yet another aspect of the invention, an optical fiber preform is formed by delivering a non-aqueous liquid reactant and an aqueous solution to a burner assembly. The non-aqueous liquid reactant and aqueous solution are discharged from the burner assembly into the flame in the form of an aerosol consisting of many droplets of the non-aqueous liquid reactant and many droplets of the aqueous solution. The liquid droplets react in the flame to form soot and deposit on the target, becoming a preform.
在本发明的再一方面,将水溶液的输送与常规蒸汽的输送结合起来。水溶液在燃烧器组件中用气体雾化,形成由许多液滴组成的气雾,同时将另一种反应物蒸发输送到燃烧器组件中。该蒸汽状态的反应物和气雾在邻近燃烧器组件的燃烧带内进行反应,形成细微的玻璃煤烟。In yet another aspect of the invention, the delivery of an aqueous solution is combined with the delivery of conventional steam. The aqueous solution is atomized with gas in the burner assembly to form an aerosol of many liquid droplets while vaporizing another reactant into the burner assembly. The reactants in the vapor state react with the gas mist in the combustion zone adjacent to the burner assembly to form fine glass soot.
本发明的另一些特征和优点将在下面的详细说明部分中描述,其中部分可从描述中显而易见,或从本发明的操作实践中认识到。本行业的技术人员将会明白,上面的概述和下面的详细说明两者都是示范性和说明性的,旨在进一步说明在这里要求权利的本发明。Additional features and advantages of the invention will be set forth in the detailed description which follows, and in part may be obvious from the description, or may be learned by practice of the invention. It will be appreciated by those skilled in the art that both the foregoing general description and the following detailed description are exemplary and explanatory and are intended to further explain the invention as claimed herein.
为进一步理解本发明,本说明书内包括一些附图,附图构成本说明书的一部分。这些附图说明了本发明的几个实施方式,与文字描述一同用来说明本发明的原理。For further understanding of the present invention, some accompanying drawings are included in this specification, and the accompanying drawings constitute a part of this specification. The drawings illustrate several embodiments of the invention and together with the description serve to explain the principles of the invention.
附图的简要说明Brief description of the drawings
图1示意说明用于本发明方法中液体输送系统的第一优选实施方式。Figure 1 schematically illustrates a first preferred embodiment of the liquid delivery system used in the method of the present invention.
图2示意说明用于本发明方法中液体输送系统的第二优选实施方式。Figure 2 schematically illustrates a second preferred embodiment of a liquid delivery system for use in the method of the present invention.
图3示意说明用于本发明方法中蒸汽和液体混合输送系统的优选实施方式。Figure 3 schematically illustrates a preferred embodiment of a mixed vapor and liquid delivery system for use in the process of the present invention.
优选实施方式的详细说明Detailed Description of the Preferred Embodiment
许多煤烟收集和煤烟沉积技术都被用来制造玻璃制品。虽然本发明能够用于许多这样的技术中,但是,它尤其适于那些用来在目标物上沉积煤烟以制成用于制造光导尤其是光导纤维的玻璃预制品的技术。然而,本行业技术人员将会明白,本发明的方法也能够用于制造平面波导。A number of soot collection and soot deposition techniques are used to create glass products. While the present invention can be used in many such techniques, it is particularly suitable for those techniques for depositing soot on a target to form a glass preform for making light guides, especially optical fibers. However, it will be apparent to those skilled in the art that the method of the present invention can also be used to fabricate planar waveguides.
在制造光导纤维的过程中,煤烟一般是均匀地沉积到目标物上或其内。将收集的煤烟固结成高纯的玻璃预制品,之后,经受进一步的加工步骤例如拉伸,形成能够传输并导向光的细纤维。因此,本发明将在该方面展开描述。然而,光导纤维行业的技术人员将会明白,也有其他系统和与这里所述系统有些改变的系统,可以采用本发明来实现上述和这里所要求权利的功能。下面将详细说明本发明的优选实施方式,附图中示意说明了这些实施方式的例子。During the manufacture of optical fibers, soot is generally deposited uniformly on or into the target. The collected soot is consolidated into a high-purity glass preform, which is then subjected to further processing steps such as stretching to form thin fibers that transmit and guide light. Accordingly, the invention will be described in this regard. However, those skilled in the fiber optic industry will appreciate that there are other systems, and systems with some variation from those described herein, that can employ the present invention to perform the functions described above and claimed herein. Preferred embodiments of the invention will now be described in detail, examples of which are schematically illustrated in the accompanying drawings.
图1中示意说明将液体送入燃烧带形成用于制造玻璃的多组分煤烟的系统的第一优选实施方式。输送液体的系统10包括装有水溶液14的水溶液容器12、装有非水性液体反应物18的非水性液体反应物容器16和也可采用的装有掺杂物22的掺杂物容器20。另外,输送液体的系统10包括雾化燃烧器组件26,例如一个雾化燃烧器组件和相关的输送机构,(下面总称为“燃烧器组件”)。对于这种燃烧器组件,1996年10月17日申请、名称为“由液体反应物的燃烧形成熔凝氧化硅的方法和设备”的美国专利申请No.08/767,653;1997年7月30日申请、名称为“采用氧气燃烧液体反应物形成氧化硅的方法”的美国专利申请No.08/903,501;1998年6月3日申请、名称为“采用加热器燃烧液体反应物形成氧化硅的方法和设备”的美国专利申请No.09/089,869;1997年10月19日申请、名称为“制备金属氧化物煤烟的燃烧器和方法”的美国临时专利申请No.60/068,255和1998年7月31日申请、名称为“制备用于制造玻璃的煤烟的设备和方法”的美国临时专利申请中都有所描述,其说明书参考结合于此。A first preferred embodiment of a system for feeding liquid into a combustion zone to form multicomponent soot for glassmaking is schematically illustrated in FIG. 1 .
在操作中,将水溶液14、非水性液体反应物18和掺杂物22根据所要求的化学计量进行混合,并储存在它们各自的容器12、16和20内。水溶液14优选装有水溶性盐例如碱金属硝酸盐、碱金属碳酸盐、碱金属硫酸盐、碱金属乙酸盐、碱土金属硝酸盐、碱土金属碳酸盐、碱土金属硫酸盐或碱土金属乙酸盐。更具体地说,水溶液14含有一种或多种水溶性盐例如硝酸钡、乙酸钡、氯化钡、硝酸锶、乙酸锶、氯化锶、硝酸锑、乙酸锑、硝酸铅、碳酸铅、硫酸铅、乙酸铅、硝酸镧、碳酸镧、硫酸镧、乙酸镧、硝酸钴、乙酸钴、氯化钴、硝酸钕、氯化钕、硝酸钾、氯化钾、硝酸镨(praeseodymium)、硝酸铯、氯化铯、硫酸铯、氢氧化铯、氯化钙、硝酸铝、硝酸钠、氯化钠、氯化铒和硫酸铒,但是也可以含有能够混入并以水溶液形式输送的其他盐和/或其他成分。In operation, the
非水性液体反应物18优选是液态的有机金属化合物例如八甲基环四硅氧烷,但也可以是硅醇盐、金属醇盐或用合适的有机溶剂例如乙二醇单甲醚使之可溶的其他含硅基材。掺杂物22,如果使用的话,可以是酮盐、醇盐、乙酸盐、β-二酮盐、或溶解于合适有机溶剂例如乙二醇单甲醚的镨、钬和铥的氟-β-二酮盐。优选的掺杂物22一般是性能对光导纤维有利的铒、锗和其他稀土元素。The non-aqueous
如果需要,水溶液14、非水性液体反应物18和掺杂物22以所要求的数量通过液体输送管线24输送到燃烧器组件26。液体14、18和22以雾化液滴30的形式从燃烧器组件26排放进入火焰28中。液滴30在雾化过程中均匀地混合,并在火焰28中反应,制成煤烟流32。煤烟流32优选指向目标物例如旋转轴34,此时燃烧器组件26沿着旋转轴34的长度来回移动,使煤烟沉积到旋转轴34上,就形成含有所要求量的包含于水溶液14、非水性液体反应物18和掺杂物22内元素的氧化物的均匀煤烟体36。
将液体输入燃烧带形成用于制造玻璃的多组分煤烟的系统的第二优选实施方式,如图2所示。象第一优选实施方式一样,液体输送系统包括储存水溶液44的水溶液容器42、储存非水性液体反应物48的非水性液体反应物容器46、和可能采用的储存掺杂物52的掺杂物容器50。然而,与本发明的第一优选实施方式不同的是,输送液体的系统40包括第一燃烧器组件56,它与非水性液体反应物容器46和掺杂物容器50选择性地连通,还包括第二燃烧器组件66,与水溶液容器42连通。如下所述,本行业技术人员将会明白,水溶液44和非水性液体反应物48可以包含一种或多种上面本发明第一优选实施方式所述的化合物。A second preferred embodiment of a system for feeding liquid into a combustion zone to form multicomponent soot for glassmaking is shown in FIG. 2 . Like the first preferred embodiment, the liquid delivery system includes an aqueous solution container 42 for storing an aqueous solution 44, a non-aqueous liquid reactant container 46 for storing a non-aqueous liquid reactant 48, and an optional adulterant container for storing an adulterant 52 50. However, unlike the first preferred embodiment of the present invention, the liquid delivery system 40 includes a first burner assembly 56 in selective communication with the non-aqueous liquid reactant container 46 and the dopant container 50, and also includes The second burner assembly 66 communicates with the aqueous solution container 42 . As will be described below, those skilled in the art will appreciate that the aqueous solution 44 and the non-aqueous liquid reactant 48 may contain one or more of the compounds described above for the first preferred embodiment of the present invention.
在操作中,水溶液44有选择地输送到第二燃烧器组件66,而非水性液体反应物48和掺杂物52(如果需要的话),有选择地输送到第一燃烧器组件56。第一燃烧器组件56将雾化液滴60排放进入火焰58内,在火焰中液滴60燃烧,形成煤烟流62,它含有由所选择的包含于非水性液体反应物48和掺杂物52内的成分氧化而生成的氧化物的均匀混合物。第二燃烧器组件66可以与第一燃烧器组件56同时或分别启动,将雾化的液滴70排放进入火焰68内,形成均匀的煤烟流72,它含有由包含于水溶液44内的成分氧化而形成的氧化物。煤烟流62和72优选指向目标物例如旋转轴74,当第一燃烧器组件56和第二燃烧器组件66沿着旋转轴74的长度来回移动时,煤烟流62和72的煤烟以均匀层沉积到旋转轴74上。根据输送速率,所形成的煤烟体76含有来自于煤烟流62和72的所有氧化物。In operation, the aqueous solution 44 is selectively delivered to the second burner assembly 66 and the non-aqueous liquid reactant 48 and dopant 52 (if desired) are selectively delivered to the first burner assembly 56 . The first burner assembly 56 discharges the atomized liquid droplets 60 into the flame 58 where the liquid droplets 60 burn to form a soot stream 62 containing the selected non-aqueous liquid reactants 48 and dopants A homogeneous mixture of oxides produced by the oxidation of the components in 52. The second burner assembly 66 can be activated simultaneously with the first burner assembly 56 or separately to discharge the atomized liquid droplets 70 into the flame 68 to form a uniform soot stream 72 containing the components contained in the aqueous solution 44. oxides formed by oxidation. The soot streams 62 and 72 are preferably directed toward a target such as the axis of rotation 74, and as the first burner assembly 56 and the second burner assembly 66 move back and forth along the length of the axis of rotation 74, the soot from the soot streams 62 and 72 are A uniform layer is deposited onto the rotating shaft 74 . The resulting soot body 76 contains all of the oxides from the soot streams 62 and 72, depending on the delivery rate.
本发明这个实施方式所用的多燃烧器组件通常有利于产生比本发明第一实施方式大的煤烟沉积速率。另外,燃烧器组件56和66的空间排列使煤烟能够以非连续层的方式沉积,这可提供一种受控的和成本上有效的方法,制备具有被良好确定的指数变化剖面和其他特性的光导。The multiple burner assembly used with this embodiment of the invention generally facilitates a greater soot deposition rate than the first embodiment of the invention. Additionally, the spatial arrangement of the burner assemblies 56 and 66 enables the soot to be deposited in discrete layers, which can provide a controlled and cost-effective method of producing light guide.
图3示意说明用于实施本发明方法的蒸汽和液体混合输送系统80的优选实施方式。该蒸汽和液体混合输送系统80包括储存水溶液84的水溶液容器82,和将水溶液84输送到第一燃烧器组件94的液体输送管线90。另外,蒸汽和液体混合输送系统80还包括通过蒸气输送管线92输送蒸汽反应物88到第二燃烧器组件96的蒸汽输送系统86。蒸汽输送系统86可以是本行业已知的任何蒸汽输送系统,例如但不局限于美国专利No.5,043,002和No.3,698,936所揭示的蒸汽输送系统,其说明书在参考结合于此。蒸汽反应物88优选是卤化物基的原料,例如但不局限于SiCl4,或非氯化物基的原料,例如但不局限于八甲基环四硅氧烷。水溶液84优选含有水溶性盐例如碱金属硝酸盐,碱金属碳酸盐、碱金属硫酸盐、碱金属乙酸盐、碱土金属硝酸盐、碱土金属碳酸盐、碱土金属硫酸盐、或碱土金属乙酸盐。更具体地说,水溶液84含有一种或多种水溶性盐例如硝酸钡、乙酸钡、氯化钡、硝酸锶、乙酸锶、氯化锶、硝酸锑、乙酸锑、硝酸铅、碳酸铅、硫酸铅、乙酸铅、硝酸镧、碳酸镧、硫酸镧、乙酸镧、硝酸钴、乙酸钴、氯化钴、硝酸钕、氯化钕、硝酸钾、氯化钾、硝酸镨、硝酸铯、氯化铯、硫酸铯、氢氧化铯、氯化钙、硝酸铝、硝酸钠、氯化钠、氯化铒和硫酸铒,但是也可以含有能够混入并以水溶液形式输送的其他盐和/或其他成分。Figure 3 schematically illustrates a preferred embodiment of a mixed vapor and
操作中,水溶液84有选择地输送到燃烧器组件94,蒸发的反应物88输送到第二燃烧器组件96。在第一燃烧器组件94处,水溶液84用气体例如空气雾化,但优选使用氧气或与氧气一同使用惰性气体例如氮气,形成由许多粒径通常约为10-200微米的液滴组成的气雾。多数液滴的粒径一般约为20微米。雾化的液滴98排放进入靠近第一燃烧器组件94形成的第一火焰,在其中雾化液滴98进行燃烧,形成第一煤烟流102,它含有由所选择的包含于水溶液84内的成分氧化形成的氧化物的均匀混合物。蒸汽反应物88通过蒸汽输送管线92和第二燃烧器组件96作为蒸汽104被输送,蒸汽104被排放进入靠近第二燃烧器组件96形成的第二火焰106内。蒸汽104在第二火焰106内燃烧,形成煤烟流108,它含有由所选择的包含于蒸汽反应物88内的成分氧化形成的氧化物的均匀混合物。第一和第二煤烟流102、108分别指向目标物,例如旋转轴110;当第一燃烧器组件94和第二燃烧器组件96沿着旋转轴110的长度来回移动时,煤烟流102和108内的煤烟以均匀层沉积到旋转轴110上。根据输送速率,所形成的煤烟体112含有分别来自于第一和第二煤烟流102和108的所有氧化物。In operation,
虽然图3中未示出,但还可以附加一个燃烧器组件和相关的输送机构到图3所示的系统中,用以输送通常用于制造光导纤维的煤烟的附加掺杂物。本发明的这个实施方式结合了蒸汽沉积的较高煤烟沉积率和以水溶液形式输送的盐所提供的独特的光学性能。本行业技术人员将会明白,蒸气反应物88和水溶液84可以送入同一个火焰,制成均匀的煤烟流,能够以本行业内通常所知的任意方式收集,而且随后可进一步加工成光导、尤其是光导纤维的预制品。Although not shown in FIG. 3, a burner assembly and associated delivery mechanism may be added to the system shown in FIG. 3 to deliver additional inclusions of soot commonly used in the manufacture of optical fibers. This embodiment of the invention combines the higher soot deposition rates of vapor deposition with the unique optical properties provided by salts delivered in aqueous solution. Those skilled in the art will understand that the
虽然在附图中未示出,但本行业技术人员将会明白,图1、2和3所示的系统并不局限于图中所示的燃烧器组件和相关输送机构的数目。每种系统都可添装一些燃烧器组件和相关的输送机构来实施本发明的方法。总的来说,燃烧器组件的数目越多,煤烟沉积速率就越大。此外,也可以将本发明与本行业内通常所的其他蒸汽输送系统结合使用,以便在光导纤维的煤烟制造过程中,提供更大的灵活性。Although not shown in the drawings, those skilled in the art will appreciate that the systems shown in Figures 1, 2 and 3 are not limited to the number of burner assemblies and associated delivery mechanisms shown in the figures. Each system can be supplemented with burner assemblies and associated delivery mechanisms to implement the method of the present invention. In general, the greater the number of burner assemblies, the greater the soot deposition rate. Additionally, the present invention can be used in conjunction with other vapor delivery systems commonly known in the industry to provide greater flexibility in the optical fiber soot manufacturing process.
本行业技术人员将会明白,在不脱离本发明的精神和范围情形下,可以对本发明制造光导纤维预制品的煤烟的方法进行各种改变和变化。因此,如果它们是在所附权利要求及其等效内容的范围内,那么本发明就覆盖这些改变和变化。另外,所附权利要求内的所有装置或步骤和起同样作用的装置或步骤的相应结构、材料、操作以及要旨,是包括与本文所具体要求的其他要旨结合以实现其功能的任意结构、材料或操作的。Those skilled in the art will recognize that various changes and modifications can be made in the method of the present invention for making soot from an optical fiber preform without departing from the spirit and scope of the invention. Thus, it is intended that the present invention covers such changes and modifications as come within the scope of the appended claims and their equivalents. In addition, all the means or steps in the appended claims and the corresponding structures, materials, operations and gist of the devices or steps having the same effect include any structure, material, and combination with other gist specifically required herein to realize their functions. or operational.
Claims (22)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US10651398P | 1998-10-30 | 1998-10-30 | |
| US60/106,513 | 1998-10-30 |
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| CN1318038A true CN1318038A (en) | 2001-10-17 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN99810253A Pending CN1318038A (en) | 1998-10-30 | 1999-10-18 | Method of making soot for optical fiber preforms and preforms made therefrom |
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| Country | Link |
|---|---|
| EP (1) | EP1135345A1 (en) |
| JP (1) | JP2002528379A (en) |
| KR (1) | KR20010089372A (en) |
| CN (1) | CN1318038A (en) |
| AU (1) | AU1316700A (en) |
| BR (1) | BR9914871A (en) |
| CA (1) | CA2344806A1 (en) |
| ID (1) | ID28395A (en) |
| WO (1) | WO2000026151A1 (en) |
| ZA (1) | ZA200100713B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102781857A (en) * | 2010-03-02 | 2012-11-14 | 贺利氏石英英国有限公司 | Manufacture of synthetic silica glass |
| CN106053705A (en) * | 2016-07-22 | 2016-10-26 | 黄石科森色谱科技有限公司 | Production method of reversed-phase chromatographic plate |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6849334B2 (en) * | 2001-08-17 | 2005-02-01 | Neophotonics Corporation | Optical materials and optical devices |
| US7575784B1 (en) | 2000-10-17 | 2009-08-18 | Nanogram Corporation | Coating formation by reactive deposition |
| EP1333935A4 (en) | 2000-10-17 | 2008-04-02 | Nanogram Corp | Coating formation by reactive deposition |
| US7491431B2 (en) | 2004-12-20 | 2009-02-17 | Nanogram Corporation | Dense coating formation by reactive deposition |
| US20060130530A1 (en) * | 2004-12-21 | 2006-06-22 | Anderson James G | Method of doping silica glass with an alkali metal, and optical fiber precursor formed therefrom |
| US8069690B2 (en) | 2005-12-16 | 2011-12-06 | Ofs Fitel, Llc | Apparatus and method for fabricating glass bodies using an aerosol delivery system |
| JP5656469B2 (en) * | 2010-06-23 | 2015-01-21 | 株式会社フジクラ | Glass base material manufacturing apparatus and manufacturing method |
| EP3950610A1 (en) * | 2020-08-06 | 2022-02-09 | Heraeus Quarzglas GmbH & Co. KG | Alternative fluorinating agent ii: fluid and soot accumulation |
Family Cites Families (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3883336A (en) * | 1974-01-11 | 1975-05-13 | Corning Glass Works | Method of producing glass in a flame |
| CA1166527A (en) * | 1979-09-26 | 1984-05-01 | Shiro Takahashi | Method and apparatus for producing multi-component glass fiber preform |
| JPS56155035A (en) * | 1980-04-25 | 1981-12-01 | Nippon Telegr & Teleph Corp <Ntt> | Light transmitting fiber and its preparation |
| JPS57183089A (en) * | 1981-05-06 | 1982-11-11 | Nec Corp | Manufacture of quartz glass rod |
| US5110335A (en) * | 1990-06-25 | 1992-05-05 | At&T Bell Laboratories | Method of glass soot deposition using ultrasonic nozzle |
| US5212757A (en) * | 1991-10-03 | 1993-05-18 | At&T Bell Laboratories | Fatigue resistant optical fiber |
| US6312656B1 (en) * | 1995-12-19 | 2001-11-06 | Corning Incorporated | Method for forming silica by combustion of liquid reactants using oxygen |
| EP0868401B1 (en) * | 1995-12-19 | 2004-08-04 | Corning Incorporated | Method and apparatus for forming fused silica by combustion of liquid reactants |
| US5979185A (en) * | 1997-07-16 | 1999-11-09 | Corning Incorporated | Method and apparatus for forming silica by combustion of liquid reactants using a heater |
-
1999
- 1999-10-18 BR BR9914871-4A patent/BR9914871A/en not_active Application Discontinuation
- 1999-10-18 CN CN99810253A patent/CN1318038A/en active Pending
- 1999-10-18 KR KR1020017005329A patent/KR20010089372A/en not_active Abandoned
- 1999-10-18 AU AU13167/00A patent/AU1316700A/en not_active Abandoned
- 1999-10-18 WO PCT/US1999/024304 patent/WO2000026151A1/en not_active Ceased
- 1999-10-18 ID IDW00200101010A patent/ID28395A/en unknown
- 1999-10-18 CA CA002344806A patent/CA2344806A1/en not_active Abandoned
- 1999-10-18 JP JP2000579542A patent/JP2002528379A/en not_active Withdrawn
- 1999-10-18 EP EP99956587A patent/EP1135345A1/en not_active Withdrawn
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102781857A (en) * | 2010-03-02 | 2012-11-14 | 贺利氏石英英国有限公司 | Manufacture of synthetic silica glass |
| CN102781857B (en) * | 2010-03-02 | 2016-09-07 | 贺利氏石英英国有限公司 | The preparation of the silica glass of synthesis |
| CN106053705A (en) * | 2016-07-22 | 2016-10-26 | 黄石科森色谱科技有限公司 | Production method of reversed-phase chromatographic plate |
Also Published As
| Publication number | Publication date |
|---|---|
| CA2344806A1 (en) | 2000-05-11 |
| EP1135345A1 (en) | 2001-09-26 |
| BR9914871A (en) | 2001-07-03 |
| WO2000026151A1 (en) | 2000-05-11 |
| AU1316700A (en) | 2000-05-22 |
| JP2002528379A (en) | 2002-09-03 |
| ZA200100713B (en) | 2001-07-17 |
| KR20010089372A (en) | 2001-10-06 |
| ID28395A (en) | 2001-05-17 |
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