HIGH PURITY SILICA MONOLITHS AND PROCESS FOR THE SYNTHESIS THEREOF
    241.
    发明申请
    HIGH PURITY SILICA MONOLITHS AND PROCESS FOR THE SYNTHESIS THEREOF 有权
    高纯度二氧化硅单体及其合成方法

    公开(公告)号:US20110201714A1

    公开(公告)日:2011-08-18

    申请号:US13123350

    申请日:2009-10-01

    Abstract: The present invention relates to a process for the synthesis of a silica monolith according to a process known as a “sol-gel process” that comprises the following steps: hydrolysis of a silicon alkoxide in order to form a hydrolysis precursor followed by a condensation of said hydrolysis precursor in the presence of an organic solvent, in the presence of water and of a basic catalyst in order to form oligomeric clusters containing several silicon atoms; dispersion of said oligomeric clusters in a solution in order to form a sol; polymerization of the sol in order to obtain a gel via a first heat treatment, at a temperature below the boiling point of the constituents of the sol; drying of the gel via a second heat treatment including an exposure of the gel to around 90° C. for at least 24 hours followed by an increase in temperature, under vacuum, between around 90° C. and around 180° C., said temperature increase being between 0.1/min and 5° C./min; conversion of the gel to a xerogel via a third heat treatment, said heat treatment including a hold at a drying temperature between 850 and 1000° C. for at least an hour; dehydration and densification of the xerogel until the silica monolith is obtained via a fourth heat treatment, said fourth heat treatment comprising a hold at a temperature above 1100° C. for at least one hour. The present invention also relates to a silica monolith obtained by the process of the invention, having a concentration of —OH groups of less than 1 ppm. The present invention also discloses the use of the monolith of the invention for producing optical fibres.

    Abstract translation: 本发明涉及根据已知为“溶胶 - 凝胶法”的方法合成二氧化硅整料的方法,该方法包括以下步骤:水解硅烷醇以形成水解前体,然后冷凝 所述水解前体在有机溶剂的存在下,在水和碱性催化剂的存在下,以形成含有几个硅原子的低聚簇; 将所述低聚簇分散在溶液中以形成溶胶; 在低于溶胶成分的沸点的温度下通过第一热处理获得凝胶的溶胶的聚合; 通过第二热处理干燥凝胶,包括将凝胶暴露于约90℃至少24小时,然后在真空下在约90℃至约180℃之间升高温度,所述 温度升高在0.1 / min〜5℃/ min之间; 通过第三次热处理将凝胶转化为干凝胶,所述热处理包括在850至1000℃之间的干燥温度下保持至少1小时; 干凝胶的脱水和致密化直到通过第四次热处理获得二氧化硅整料,所述第四热处理包括在高于1100℃的温度下保持至少1小时。 本发明还涉及通过本发明的方法得到的二氧化硅石墨,其浓度小于1ppm。 本发明还公开了本发明的整料用于生产光纤的用途。

    Method for producing a cylinder from synthetic quartz glass
    242.
    发明申请
    Method for producing a cylinder from synthetic quartz glass 有权
    从合成石英玻璃制造圆筒的方法

    公开(公告)号:US20100307197A1

    公开(公告)日:2010-12-09

    申请号:US12801378

    申请日:2010-06-04

    CPC classification number: C03B19/01 C03B19/1453 C03B37/01446 C03B2201/04

    Abstract: A known method for producing synthetic quartz glass comprises the method steps: (a) forming a cylindrical SiO2 soot body having an inner portion and at least one free cylinder jacket surface surrounding the inner portion; (b) thermally drying the porous soot body; and (c) vitrifying the dried soot body with formation of the cylinder from synthetic quartz glass. Starting therefrom, to indicate a method which permits a particularly flat radial distribution in the inner portion of the cylinder, it is suggested according to the invention that the dried SiO2 soot body that is present after method step b) should be subjected to a homogenizing method prior to vitrification, the homogenizing method comprising the following steps: (I) heating the soot body to a consolidation temperature to form a sealing layer in the area of the at least one cylinder jacket, the sealing layer sealing the inner portion to the outside; (II) cooling the soot body from the consolidation temperature; and (III) annealing the soot body in the range of a homogenization temperature during a period of at least 5 hours so that the radial profile of the hydroxyl group concentration flattens in the inner portion.

    Abstract translation: 用于生产合成石英玻璃的已知方法包括以下方法步骤:(a)形成具有内部部分和围绕内部部分的至少一个自由圆筒形护套表面的圆柱形SiO 2烟灰体; (b)热干燥多孔烟炱体; 和(c)通过合成石英玻璃形成圆筒来使干燥的烟灰体玻璃化。 从此开始,为了表示允许气缸内部特别平坦的径向分布的方法,根据本发明,建议在方法步骤b)之后存在的干燥的SiO 2烟炱体应经受均匀化方法 在玻璃化之前,均化方法包括以下步骤:(I)将烟灰体加热至固化温度,以在至少一个气缸套的区域中形成密封层,密封层将内部部分密封到外部; (II)从固结温度冷却烟灰体; 和(III)在均匀化温度范围内在至少5小时的时间内使烟灰体退火,使得羟基浓度的径向分布在内部变平。

    Production process of synthetic quartz glass
    243.
    发明授权
    Production process of synthetic quartz glass 有权
    人造石英玻璃的生产工艺

    公开(公告)号:US07841211B2

    公开(公告)日:2010-11-30

    申请号:US10535935

    申请日:2003-11-28

    Abstract: First of all, there is provided a production process of a synthetic quartz glass which has less impurity, has a high-temperature viscosity characteristic equal to or more than that of a natural quartz glass, and hardly deforms even in a high-temperature environment, and especially a production process of a highly heat resistant synthetic quartz glass which is free from the generation of bubbles and is dense. Secondly, there is provided a highly heat resistant synthetic quartz glass body which is easily obtained by the production process of the present invention, and especially a transparent or black quartz glass body which is free from the generation of bubbles, is dense, has high infrared absorption rate and emission rate, and has an extremely high effect for preventing diffusion of alkali metal. The process is a process of producing a highly heat resistant quartz glass body having an absorption coefficient at 245 nm of 0.05 cm−1 or more, and the silica porous body was subjected to a reduction treatment, followed by baking, thereby forming a dense glass body.

    Abstract translation: 首先,提供了杂质少,具有等于或高于天然石英玻璃的高温粘度特性的合成石英玻璃的制造方法,即使在高温环境下也几乎不变形, 特别是高度耐热的合成石英玻璃的生产过程,其不产生气泡并且致密。 其次,提供了通过本发明的制造方法容易获得的高耐热性合成石英玻璃体,特别是不产生气泡的透明或黑色石英玻璃体,具有高红外 吸收率和排放率,对防止碱金属的扩散具有极高的效果。 该方法是制造吸收系数在245nm为0.05cm -1以上的高耐热性石英玻璃体的工序,对二氧化硅多孔体进行还原处理,然后进行烧成,由此形成致密的玻璃 身体。

    Optical fiber manufacture
    244.
    发明申请
    Optical fiber manufacture 有权
    光纤制造

    公开(公告)号:US20100287993A1

    公开(公告)日:2010-11-18

    申请号:US12799561

    申请日:2010-04-27

    Abstract: The specification describes methods for the manufacture of very large optical fiber preforms wherein the core material is produced by MCVD. Previous limitations on preform size inherent in having the MCVD starting tube as part of the preform process are eliminated by removing the MCVD starting tube material from the collapsed MCVD rod by etching or mechanical grinding. Doped overcladding tubes are used to provide the outer segments of the refractive index profile thus making most effective use of the MCVD produced glass and allowing the production of significantly larger MCVD preforms than previously possible.

    Abstract translation: 该说明书描述了用于制造非常大的光纤预制件的方法,其中芯材料通过MCVD制造。 通过蚀刻或机械研磨,通过从收缩的MCVD棒中除去MCVD起始管材料,从而消除了将MCVD起始管作为预制件工艺的一部分而固有的预制件尺寸的限制。 掺杂的外包管用于提供折射率分布的外部部分,从而最有效地利用MCVD生产的玻璃,并允许生产比之前可能的显着更大的MCVD预成型件。

    Method for Producing a Hollow Cylinder of Synthetic Quartz Glass, and Thickwalled Hollow Cylinder Obtained According to the Method
    245.
    发明申请
    Method for Producing a Hollow Cylinder of Synthetic Quartz Glass, and Thickwalled Hollow Cylinder Obtained According to the Method 有权
    合成石英玻璃中空圆柱体的制造方法和根据该方法获得的厚壁空心圆筒

    公开(公告)号:US20100081554A1

    公开(公告)日:2010-04-01

    申请号:US12448294

    申请日:2007-12-13

    Abstract: A known method for producing a hollow cylinder of synthetic quartz glass comprises the steps of: (a) providing an inner tube of synthetic quartz glass having an inner bore defined by an inner wall, (b) cladding the inner tube (3′) with an SiO2 soot layer (4′), and (c) sintering the SiO2 soot layer with formation of the hollow cylinder. Starting therefrom, to indicate a method in which on the one hand the sintering process is completed before the hollow cylinder is further processed together with the core rod, and in which on the other hand a complicated machining of the inner bore of the hollow cylinder of quartz glass is not required, the invention suggests that during sintering the surface temperature of the inner wall of the inner tube should be kept below the softening temperature.

    Abstract translation: 用于生产合成石英玻璃的中空圆筒的已知方法包括以下步骤:(a)提供合成石英玻璃的内管,其具有由内壁限定的内孔,(b)用内壁(3')包覆内管 SiO 2烟灰层(4'),和(c)在形成中空圆筒的情况下烧结SiO 2烟灰层。 从此开始,指示一方面在中空圆筒与芯棒一起进一步加工之前烧结过程完成的方法,另一方面,中空圆柱体的内孔的复杂加工 石英玻璃不需要,本发明提出在烧结过程中,内管内壁的表面温度应保持在软化温度以下。

    Optical fiber preform with overclad tubes
    246.
    发明授权
    Optical fiber preform with overclad tubes 有权
    具有外包管的光纤预制件

    公开(公告)号:US07641969B2

    公开(公告)日:2010-01-05

    申请号:US11088076

    申请日:2005-03-23

    CPC classification number: C03B37/01211 C03B2201/03 C03B2201/04 Y10T428/2913

    Abstract: An optical fiber preform is assembled by inserting core rod segments axially end to end inside of a first glass overclad tube having a first, relatively low concentration of a given impurity that contributes to signal attenuation in an optical fiber to be drawn from the preform. The first overclad tube with the contained core rod segments are inserted in a second glass tube having a second concentration of the given impurity which is higher than the first concentration. The wall thickness of the first overclad tube is preferably less than that of the second overclad tube, thus reducing the amount of high purity glass needed to form the first overclad tube and attendant manufacturing costs. The core rod segments may include salvageable remnants from a single long core rod produced, for example, by vapor axial deposition (VAD).

    Abstract translation: 通过将芯棒片段轴向端对端插入第一玻璃外包层管内装配光纤预制件,第一玻璃外包管具有第一相对低浓度的给定杂质,这有助于从预成型件中拉出的光纤中的信号衰减。 将具有所述芯棒段的第一外包管插入具有高于第一浓度的给定杂质的第二浓度的第二玻璃管中。 第一外包层管的壁厚优选小于第二外包层管的壁厚,从而减少形成第一外包层管所需的高纯度玻璃的量和伴随的制造成本。 芯棒段可以包括来自例如通过气相轴向沉积(VAD)产生的单个长芯棒的可补救残余物。

    Single Mode Optical Fiber and Manufacturing Method Therefor
    247.
    发明申请
    Single Mode Optical Fiber and Manufacturing Method Therefor 审中-公开
    单模光纤及其制造方法

    公开(公告)号:US20090084141A1

    公开(公告)日:2009-04-02

    申请号:US12327993

    申请日:2008-12-04

    Abstract: An optical fiber is formed by performing vapor phase deposition of SiO2 on the outside of a glass rod comprising a core section and a first cladding section and drawing a glass preform which formed by a second cladding section. Also, a single mode optical fiber is manufactured so that the ratio of the diameter D of the first cladding section and the diameter d of the core section is in a range of 4.0 to 4.8, and OH concentration is 0.1 ppm or less. Also, an optical fiber is manufactured so that a value of D/d>4.8, and the OH concentration is 0. 1 ppm or less. It is thereby possible to maintain an initial loss in the 1380 nm wavelength range even if hydrogen diffusion occurs.

    Abstract translation: 通过在包括芯部和第一包层部分的玻璃棒的外部进行SiO 2的气相沉积并且拉制由第二包层部形成的玻璃预制件来形成光纤。 此外,制造单模光纤,使得第一包层部分的直径D和芯部分的直径d的比率在4.0至4.8的范围内,并且OH浓度为0.1ppm或更小。 此外,制造光纤,使得D / d> 4.8的值和OH浓度为0.1ppm以下。 因此即使发生氢扩散,也可以保持1380nm波长范围的初始损耗。

    Reduction of optical fiber cane/preform deformation in consolidation
    248.
    发明申请
    Reduction of optical fiber cane/preform deformation in consolidation 有权
    缩小光纤手杖/预制棒的变形

    公开(公告)号:US20080271495A1

    公开(公告)日:2008-11-06

    申请号:US12072013

    申请日:2008-02-22

    Abstract: According to an embodiment of the invention a method of manufacturing optical fiber cane comprises the steps of: (i) providing a core rod manufactured of relatively low viscosity glass; (ii) depositing SiO2 based soot around the core rod to form a soot preform, the soot being of relatively high viscosity material such that the softening point of the low viscosity glass is at least 200° C. lower than the viscosity of the high viscosity outer core region; and (iii) consolidating the soot of the soot preform by exposure to hot zone at temperatures of 1000° C.-1600° C. The soot is consolidated by heating the outer portion of the soot preform at a relatively fast heating rate, the heating rate being sufficient to densify the soot, so as to render the densified material with enough rigidity to confine the heated core rod and to prevent the heated core rod from puddling.

    Abstract translation: 根据本发明的实施例,制造光纤手杖的方法包括以下步骤:(i)提供由相对低粘度玻璃制成的芯棒; (ii)在芯棒周围沉积基于SiO 2的烟炱以形成烟炱预制件,该烟炱是相对高粘度的材料,使得低粘度玻璃的软化点至少为200℃。 低于高粘度外芯区域的粘度; 并且(iii)通过在1000℃-1600℃的温度下暴露于热区来固化烟灰预制件的烟灰。通过以相对较快的加热速率加热烟灰预制件的外部部分来固化煤烟,加热 速率足以致密化烟灰,以使致密材料具有足够的刚性以限制加热的芯棒并防止加热的芯棒搅拌。

    Manufacturing method of optical fiber preform, manufacturing method of optical fiber, and optical fiber
    249.
    发明授权
    Manufacturing method of optical fiber preform, manufacturing method of optical fiber, and optical fiber 有权
    光纤预制棒的制造方法,光纤的制造方法以及光纤

    公开(公告)号:US07376316B2

    公开(公告)日:2008-05-20

    申请号:US10567912

    申请日:2004-08-03

    Abstract: Methods of manufacturing an optical fiber preform and an optical fiber, and an optical fiber formed by this method of manufacturing an optical fiber are provided, the optical fiber preform having a desired refractive index profile and being capable of suppressing an increase in loss due to the absorption by OH groups. A pipe is formed by an inside vapor phase deposition method such that glass layer to be formed into a core and a glass layer to be formed into a part of a cladding pipe are deposited in a starting pipe, the glass layers each containing at least one of fluorine, germanium, phosphorous, and chlorine, the starting pipe being made of a silica glass having an outside diameter in the range of 20 to 150 mm and a wall thickness in the range of 2 to 8 mm. The pipe thus formed is collapsed to form a glass rod in which the concentration of hydroxyl groups is 10 weight ppm or less in a region from the surface of the glass rod to a depth of 1 mm therefrom.

    Abstract translation: 提供了制造光纤预制棒和光纤的方法以及通过该光纤制造方法形成的光纤,所述光纤预制棒具有所需的折射率分布并且能够抑制由于 OH基吸收。 通过内部气相沉积方法形成管,使得要形成芯的玻璃层和待形成为包层管的一部分的玻璃层沉积在起始管中,每个玻璃层包含至少一个 的氟,锗,磷和氯,起始管由外径在20〜150mm,壁厚在2〜8mm的范围内的石英玻璃制成。 由此形成的管道在从玻璃棒的表面到其深度为1mm的区域中折叠形成玻璃棒,其中羟基的浓度为10重量ppm以下。

    Method For Producing An Optical Component
    250.
    发明申请
    Method For Producing An Optical Component 审中-公开
    制造光学元件的方法

    公开(公告)号:US20070209400A1

    公开(公告)日:2007-09-13

    申请号:US10593508

    申请日:2005-03-16

    CPC classification number: C03B37/01211 C03B37/0126 C03B2201/04

    Abstract: According to a previously known method for producing an optical component from synthetic quartz glass, a coaxial arrangement comprising an outer jacket tube, an inner jacket tube that is provided with an internal bore, and a core rod whose bottom face rests on a thrust bearing within the internal bore, is fed into a heating zone in a vertical orientation, is softened therein zone by zone, and is elongated so as to obtain the quartz glass component. In order to create a simple and inexpensive method that is based on said method and makes it possible to reproducibly manufacture a high-quality optical component, the thrust bearing is embodied as a constriction of the internal bore of the inner jacket tube.

    Abstract translation: 根据用于从合成石英玻璃制造光学部件的以前已知的方法,一种同轴装置,包括外护套管,设置有内孔的内护套和底面搁置在推力轴承内的芯棒 将内孔以垂直取向供给到加热区域中,逐渐被软化,并且被拉长以获得石英玻璃部件。 为了创建基于所述方法的简单且便宜的方法,并且使得可以可重复地制造高质量的光学部件,推力轴承被实施为内护套管的内孔的收缩。

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