TW477777B - A method for the manufacture of a quartz glass body and holder element of quartz glass - Google Patents

Abstract

In a known method for the manufacture of a quartz glass body, SiO2 particles are deposited on the cylinder jacket surface of a cylindrical mandrel rotating about its longitudinal axis, by forming an essentially cylindrical porous blank with a holder element of quartz glass being provided in the area of one of the ends of the blank. To improve, on this basis, the reproducibility of characteristics of the products manufactured from the quartz glass body, it is proposed according to the invention that a holder element with a metastable OH concentration of less than 30 wtppm is used, and that the holder element is subjected to a thermal pretreatment. A suitable holder element for holding a blank of porous quartz glass is characterized in that it consists of quartz glass of a metastable OH concentration of less than 30 wtppm.

Description

477777 Case No. 89122677 Amendment V. Description of the Invention (1) The present invention relates to a method for manufacturing a quartz glass body, which includes depositing Si 02 particles on the surface of a cylinder liner of a cylindrical mandrel rotating around its secondary axis to form an essence The upper cylindrical plain sintered blank is connected with a quartz glass clamping element to be applied in one end region of the blank and the blank is sintered. The invention also relates to a quartz glass clamp seat component, which is connected to one end of the blank to hold a cylindrical blank of plain-fired quartz glass. A method and clamping element for this type is obtained from DE-A 1 1 9 6 49 9 3 5

know. In the method described, a hollow cylindrical plain-fired quartz glass blank is manufactured according to the so-called n OV D method π (outside vapor deposition), and a layer of fine Si 02 particles is deposited on a carrier tube rotating about its longitudinal axis. During the deposition process, a quartz glass tubular mount was concealed into one of the billet ends in production. After removing the carrier tube from the billet, the billet can be held on a vertically-oriented burial holder for further processing steps of the billet, such as dehydration treatment in a chlorineous atmosphere. The self-fired ingot is fused into a transparent quartz glass preform. During the vitrification reaction, the holder first maintains the embryo and then removes the appropriate part of the embryo. From DE 1 9 6 4 9 9 3 5 (A 1), a method for manufacturing quartz glass is known, in which Si 02 particles are produced by flame hydrolysis of the material containing the starting material. A sintered chain is formed on a rotating mandrel ( Soot body). A quartz glass tube is buried in one end of the chain material. The density of the blank in this area is adjusted to at least 60% of the theoretical density of quartz glass.

Because the preform and the holder (or individual tubes) are made of quartz glass, the coexistence of all expansion differences and the vitrification reaction is avoided. However, it has been shown that optical fibers with partially mutated optical properties are obtained from the use of preforms made of known clamps. Brief description of the drawings Figure 1 shows the lack of cross-section performance of the blank material manufacturing of the present invention; and

O: \ 67 \ 67135.ptc Page 5 477777 Case No. 89122677 Revision V. Description of the invention (2) Figure 2 shows the cross-sectional performance of the blank manufacturing of the current technology. Brief description of the drawing symbols 1 indicates a material, 2 indicates a tubular clamp seat; 3 indicates the surface of a chain material, 4 indicates a mandrel; 5 indicates a deposition lamp; 6 indicates the movement of a deposition lamp Direction; 7 for an extra light; 8 for a hatched area; and

1 2 represents a clamp seat. The present invention is based on the work of improving a known method based on the reproduction properties of a product made of a quartz glass body. According to the present invention, a suitable supporting element is designated for the work of flammable quartz glass burial. Regarding this method, its work is to solve this problem according to the initial designated method according to the present invention by using a clamping element having a metastability 0 Η below 30 w t p p m and subjecting the clamping element to a pre-heat treatment. It has been shown that the above-mentioned variation in optical properties is due to the fact that the billet has an axial gradient in its hydroxyl concentration (also referred to hereinafter as a concentration of 0 Η). In a known method, the 0 ° -concentration seat element having a maximum concentration of 0 中 in the blank-and the quartz vitreous body made therefrom-is used for bonding.

This can be traced back to the fact that during the manufacturing process, especially during the high-temperature process steps, the base is diffused from the holder element to the blank and to the quartz glass body. However, unexpectedly, the emission of this base is not necessarily related to the hydroxyl concentration of quartz glass. On the contrary, the base concentration of quartz glass contains chemically fixed

O: \ 67 \ 67135.ptc Page 6 477777 _ Case No. 89122677 (Xue Yue—Amendment _ ·. V. Description of the invention (3) degrees and a metastable 0H concentration, but only the latter in terms of 0H-based emissions It is a problem. Therefore, according to the method of the present invention, it is possible to use a quartz glass clamping element with a high 0 H concentration, as long as its metastability is less than 30 wtppm (weight ratio ppm). Due to the fact that the clamping element used is the lowest possible The metastable OH concentration (low) is 30 wtppm, which greatly eliminates the emission of 0% radicals so that the material and the system made it transparent. The substantially uniform axial distribution of hydroxyl groups in the clear quartz glass body is generally known. π is the concentration of radicals that can be removed by the temperature treatment of quartz glass. The solution of metastable 0 Η groups in quartz glass requires a certain activation energy. In any case, the diffusion system of metastable 0 Η groups in the quartz glass component requires The degree of temperature, the duration of temperature treatment, the length of the diffusion path, etc. are determined. The larger the component, the longer the diffusion path (= the maximum distance between a point within the component and the surface of the free component). In the sense of the present invention, the hydroxyl concentration is interpreted as 104 (rc temperature plus «hot It can be removed at a diffusion path of 5 mm at 48 hours. &Quot; Metastable OH concentration Η Λ Use a metastable OH during the metastable glass. Equivalent concentration. Special pieces are required to be made in the metastable 0H component. The higher subpieces are made with lower 0H, but this measure has a specific concentration in the province. The concentration item is stable during the 0H period to ensure the use of 0. Quartz application concentration does not need to be specified. British glass held low 0H before seeing to glass. Hold the base element and preheat the original piece together according to the often quite concentrated concentration of stone quartz

The glass is thought of by the master. Because of the processing, it is better to use the Asian lending plus clear glass 0H clamp base and stop here. Yu Gao stabilized after 0H heat. The concentration element holder can be stabilized at 0H. Due to the special reachable element invention, the concentration can be reduced after the reduction of the concentration is high. The production is advocated by quartz. Quartz can be made of quartz. Use a metastable 0H concentration less than 1 wtppm. Of the clamping element. Consider

477777

Amendment No. 89122677 V. Description of Invention (4). The above meaning ’This is a quartz glass fiber component whose original OH concentration has been reduced to a maximum weight of 丨% by heating to 〇 4 〇 C degrees for 48 hours (diffusion path 5 mm). Therefore, in order to avoid the emission of metastable oxonyl radicals, the obtained warp radicals are distributed substantially uniformly in the axial direction and are used in the transparent quartz glass body made with them. The higher the temperature and the longer the treatment period after a heating, the lower the metastable concentration of the post-treated clamping element. Thermal post-treatment proved successful including heating the clamp element at a temperature of at least 900 ° C. The clamp seat element is advantageously heated at least at a temperature. The heating period within the heating post-treatment range is suitable for 5 hours, and more preferably 20 hours or more. The method according to the invention proves to be particularly advantageous when the cylindrical holder element is used for local burial in an end region of the produced blank. Regarding the clamping element, the above work is solved according to the present invention. Starting from the clamping element of the above-mentioned type, a clamping element containing metastable 0H concentration lower than = quartz glass is used. The quartz glass of a clip element of MPPm has the lowest possible metastability 0H concentration and disperse any or only 0H based on the blank to be clamped or in the quartz glass x to ensure the essence in the blank or the transparent quartz glass body On the upper axis, evenly distributed. On the one hand, low-based quartz glass Γ; on the other hand, after the γ thermal post-treatment, the quartz glass with a relatively high initial metastable OH concentration can be chosen ... 0H concentration. In view of the above-mentioned technical work and its definition of low metastable OH concentration, please refer to the explanation of the method according to the present invention for further advantages and effects. Further consideration of the 0H group in the chain and the quartz glass body The lowest possible axial gradient of the lowest possible emission degree, a clamping seat element is preferably a metastable 011 thick household "= quartz glass ring at lwtppm. Low again

477777 _ 一 $ 0年 U 月 约 Revision _ · V. Description of the invention (5) The lost component according to the present invention should have a characteristic cylindrical area, at least partially buried in the blank held by it according to its purpose. The cylindrical area is buried in the blank to ensure a firm bond. The following will explain the present invention in more detail based on specific examples and drawings. The diagram illustrates the graphical representation in detail: °. Figure 1. Process steps for depositing Si 〇2 particles, made from sintered quartz glass as a blank, according to the present invention, a holder is buried on the front side; and-Figure 2 is the same process as Figure 1 Steps; but with the current state of the technology, it is pointed out that the chain zone is added to the pre-chain to increase the 0H concentration. Specific example Figure 1 is a cross-sectional representation of two made of plain-wound quartz glass blank 1. A tube-shaped holder 2 type holder is buried in the front 3 areas of the blank 1. The outer diameter of the blank 1 is about 80 mm, and the length is about 700 mm. It is deposited on the mandrel 4 rotating around its longitudinal axis by flame hydrolysis of 31 (: 14 and 〇6 (: 14) according to the known OVD method. The Si 02 particle layer is made. The inner surface of the material 1 is coated with germanium dioxide. A pedestal lamp 5 is moved back and forth along the surface of the material 1 to deposit S i 〇2 particles (with Ge 02 particles) to form a layer. Kill During the manufacturing method, the clamp base 2 is buried firmly in a part of the length in the front edge 1 of the blank 1. The clamp base 2 has an outer diameter of 25 mm and a wall thickness of 9 mm. The metastable OH-based diffusion path of the clamp base 2 Therefore, it is 4.5 mm. The particularly stable burial of the clamp base 2 can be adjusted to a higher temperature in the front side 3 by an additional lamp 7, and then adjusted to a higher density, so that the surface of the clamp base 2 is melted with the blank 1. The weight of the blank 1 produced in this way can exceed 2 kg. After removing the mandrel 2, the material can be processed. The material holder 2 is piled up from the buried material 1-partly reprocessed. The fused quartz glass is used to manufacture the holder 2. The OH concentration of quartz glass is about 80 wtppm. The temperature is adjusted to 104 ° C during 48 hours to reduce the OH concentration

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-j number 89122677 V. Description of the invention (6) to 4.8 wtppm. This means that the metastable OH concentration of clamp seat 2 is about 75 wtppm before adjustment. With proper use of the holder, and according to the above definition (temperature = 104 (t), processing period = 48 hours, diffusion path < 5 mm), holder 2 no longer contains all measurable metastable OH concentrations. After the Dianji program, the billet was cleaned, dried in a 900 ° C chlorine atmosphere, and sintered at a temperature of about 1350 ° C. The mandrel thus obtained is covered with a "sleeve" to make a so-called single fiber preform. The fibers drawn from the pre-mold can exhibit uniform optical properties over the entire length of the fiber. Especially at the wavelength of 1 3 5 5 nm (in the 〇H absorption band) The optical agricultural reduction is less than 0.7 dB / km. Comparative Specific Example 1 In the comparative specific example, the blank 1 was manufactured as described in Specific Example 1, but the misplacement 12 (see Figure 2) was not adjusted before application. Temperature. The OH concentration of the holder 12 is about 55 wtppm. The preform made by the holder 12 is also pulled out of the single fiber. The optical attenuation is not uniform. At a wavelength of 1385 nm, the attenuation rate is 0 · 6 dB / km and 7 Between dB / km, the maximum attenuation value appeared in the preform area that was originally close to the clamp base 12. After using the clamp base 1 2 〇 Ο concentration measurement results 〇Η concentration was only 5.6 wtppm. The result is about 5 〇wtppm The "metastable" π is released from the holder 12 during the manufacturing process, dissolves in the reference material 1 and then puts the above-mentioned high attenuation value at 1385 nm in the pre-field. Figure 2 shows the inner hatched area 8 A simplified diagram of increasing the concentration range of 0%, as in the method according to the current state of technology, which typically occurs after the billet is sintered. The distribution of the 0Η group in the reaction mixture 1 with increasing concentration was released from the holder 12 during the deposition process. The released 0Η group diffused into the plain calcined quartz glass around the holder 12, and then the preform and A fiber with an axial gradient of 0 ° is generated in the fiber drawn from it. It is particularly important for the processing steps to be performed at higher temperatures such as about 900 ° C and

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Claims (1)

477777 Amendment No. 89122677 (January date ft ▼ Please range: 1. A method for manufacturing a quartz glass body, including the accumulation of S i 0 2 particles on the surface of a cylindrical mandrel cylinder sleeve rotating about its longitudinal axis, An essentially cylindrical plain sintered billet and a quartz glass clamp seat element are applied to one end of the billet to connect and fuse the billet; it is characterized by using a metastable 0H concentration of less than 30 wtppm, and its clamp The base element undergoes heat pretreatment. 2. The method according to item 1 of the scope of the patent application, which uses a meta-stable OH concentration of less than 1 wtppm. 3. The method according to item 1 or 2 of the scope of patent application, The heating pretreatment includes heating the clamp base element at a temperature of at least 900 ° C. 4. The method according to item 3 of the patent application scope, wherein the clamp base element is heated at a temperature of at least 1000 ° C. The heating pretreatment package includes heating the clamping element 5. The method according to item 1 of the patent application scope includes heating the clamping element for at least 5 hours. 6. The method according to item 5 of the patent application scope requires at least 20 hours. 7 According to Shen The method according to item 1 of the patent application, wherein a cylindrical clamping seat element is partially buried in an end region of the blank to be made. 8. A quartz glass is connected with one end of the material to hold the circle of plain-fired quartz glass. The clamping element of the cylindrical blank is characterized in that the clamping element is made of a quartz glass with a metastable OH concentration of less than 30 wtppm. 9. According to the clamping element of the eighth aspect of the patent application, the metastable OH concentration is low At 1 wtppm 〇 10. According to the patent application scope item 8 or 9 of the clamping seat element, wherein it features a cylindrical area at least partially buried therein to hold the blank. O: \ 67 \ 67135.ptc Page 13