WO2021223326A1 - 含有功能性石英包层的光纤预制棒及其制备方法 - Google Patents

含有功能性石英包层的光纤预制棒及其制备方法 Download PDF

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WO2021223326A1
WO2021223326A1 PCT/CN2020/102946 CN2020102946W WO2021223326A1 WO 2021223326 A1 WO2021223326 A1 WO 2021223326A1 CN 2020102946 W CN2020102946 W CN 2020102946W WO 2021223326 A1 WO2021223326 A1 WO 2021223326A1
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tail
quartz
purity
shank
gas
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PCT/CN2020/102946
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English (en)
French (fr)
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陈宏达
王龙飞
李凡
眭立洪
罗詠淋
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江苏永鼎股份有限公司
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Publication of WO2021223326A1 publication Critical patent/WO2021223326A1/zh

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    • C—CHEMISTRY; METALLURGY
    • 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]
    • C—CHEMISTRY; METALLURGY
    • 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
    • C03B37/01205—Manufacture of preforms for drawing fibres or filaments starting from tubes, rods, fibres or filaments
    • C03B37/01211—Manufacture of preforms for drawing fibres or filaments starting from tubes, rods, fibres or filaments by inserting one or more rods or tubes into a tube
    • C—CHEMISTRY; METALLURGY
    • 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]
    • C03B37/01446—Thermal after-treatment of preforms, e.g. dehydrating, consolidating, sintering
    • C—CHEMISTRY; METALLURGY
    • 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]
    • C03B37/01466—Means for changing or stabilising the diameter or form of tubes or rods
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00—Technologies relating to the processing of minerals
    • Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
    • Y02P40/57—Improving the yield, e-g- reduction of reject rates

Definitions

  • the invention belongs to the technical field of optical fibers, and specifically relates to an optical fiber preform containing a functional silica cladding layer and a preparation method thereof.
  • optical fiber preform When manufacturing optical fibers, the purified raw materials must first be made into a glass rod that meets certain requirements, which is called “optical fiber preform.”
  • the core layer has a low refractive index (n1) and the outer layer is a cladding layer with a low refractive index (n2), which should have a refractive index distribution and geometric dimensions that meet the requirements.
  • a typical optical fiber preform has a diameter of about 10-25nm and a length of about 60-120nm.
  • optical fiber preforms In the communication optical fiber preparation process, one of the important contents is the preparation of optical fiber preforms.
  • the manufacturing of optical fiber preforms is divided into core rod manufacturing and cladding manufacturing.
  • a cladding is deposited on the outside of the core rod to prepare an optical fiber preform.
  • the technologies used to prepare optical fiber preforms mainly include in-tube method represented by plasma chemical vapor deposition (PCVD) and improved chemical vapor deposition (MCVD), and axial vapor deposition (VAD) and external vapor deposition.
  • Out-of-tube method represented by deposition method (OVD).
  • the outer cladding layer is manufactured mainly by direct OVD synthesis and quartz sleeve assembly.
  • the exhaust gas treatment equipment will not only extract the reaction waste gas, but also extract a certain reaction product, that is, nano-silica powder.
  • a nano-silica powder cake with relatively low water content and low salt content can be obtained. These particles are directly discharged into the air and will cause dust pollution.
  • the main waste disposal method is landfill, but the landfill method still causes certain harm to the environment, especially the soil, and wastes resources.
  • the tube preform is composed of a pre-prepared mandrel and a tube.
  • the tube is vacuum drawn from the end of the tube tail handle and melted in a drawing furnace or an extension furnace to finally become an optical fiber or an optical fiber preform.
  • the structure diagram of the casing preform is shown in Figure 1.
  • the core rod of the tube preform includes a core layer and an inner cladding.
  • the inner cladding is silica glass with a certain doping and refractive index adjustment.
  • the tube is used as the outer layer of the optical fiber preform.
  • the outer cladding is generally pure silica glass. .
  • the light guide structure of the entire optical fiber preform is mainly realized by the design of the core rod, so the preparation of the core rod is very demanding. However, for some deposition processes, it is difficult to prepare core rods with low attenuation and superior bending resistance, and it is difficult to directly implement the tube rod process.
  • the technical problem to be solved by the present invention is aimed at the core layer of the optical fiber preform that has a complex refractive index profile design (multi-layer different refractive index) and has a certain doping concentration requirement for the dopant in the above-mentioned prior art. Due to the design, it is difficult to perform one-time deposition molding with VAD or OVD equipment.
  • the present invention provides a method for preparing an optical fiber preform containing a functional silica cladding that can avoid multiple deposition operations, and an optical fiber prepared by the method Preform.
  • the present invention provides a method for preparing an optical fiber preform containing a functional silica cladding, which includes the following steps:
  • step (T2) After the step (T1) is assembled with the quartz cladding sleeve and the core rod, fill the gap between the cladding sleeve and the core rod with high-purity quartz powder; preferably, the purity of the high-purity quartz powder is not low At 99.999%;
  • the high-purity quartz column refers to a high-purity quartz column with a special structure, for example, as shown in FIG. 5 with a hole in the middle and one end Quartz columns with longitudinal shallow grooves on the surface;
  • T4 Install the tail cover plate: install the tail cover plate with barometer, air inlet, exhaust port and Teflon sealing ring at the end of the fiber preform tail handle to fix the position of the core rod;
  • the air pressure gauge in step (T4) is installed at the outlet of the air suction port, and a valve is installed at the rear, and the positive pressure and negative pressure can be displayed.
  • the air inlet is equipped with a valve, and the sealing ring has three From the inside to the outside, they are respectively fixed at the end of the mandrel tail handle, the end of the tail high-purity quartz column and the end of the sleeve tail handle, forming two high-purity quartz columns located between the mandrel and the tail of the high-purity quartz column and the tail of the high-purity quartz column.
  • the two annular gaps between the tail shank of the casing are slotted on the outer surface of the other end of the high-purity quartz column at the tail, so that the two annular gaps can communicate with the quartz powder area.
  • the doping treatment of the quartz powder in step (T5) includes: closing the valve of the gas outlet, and injecting a mixed gas composed of doping gas, helium, argon or nitrogen into the gas inlet , Continue to feed the gas, and then put the preform into the heating furnace, and raise the temperature to 1200°C ⁇ 1400°C, so that the dopant gas can fully react with the quartz powder.
  • the doping gas is silicon tetrachloride or silicon tetrafluoride.
  • the melting and shrinking sintering method in step (T5) includes: after the doping gas and the quartz powder are fully reacted, the temperature is lowered to 600-800°C, the exhaust valve is opened, and the inside of the preform is extracted under negative pressure. Then open the inlet valve to supply helium or a mixture of helium and dopant gas into the preform. After the pressure is stable, the temperature is increased to the melting temperature, and the cladding casing is passed through The doped quartz powder and the core rod are melted and sintered into a complete transparent glass rod;
  • the doping gas in step (T5) is silicon tetrachloride or silicon tetrafluoride.
  • step (T5) different doping gases have different effects.
  • Silicon tetrafluoride is introduced to produce a functional cladding with a lower refractive index than that of undoped silica glass; silicon tetrachloride is introduced to produce A functional cladding with a higher refractive index than undoped silica glass.
  • the refractive index profile of a functional cladding optical fiber preform prepared by doping with silicon tetrachloride is shown in Figure 6;
  • the schematic diagram of the rate profile is shown in Figure 7.
  • the second aspect of the present invention also provides an optical fiber preform, which is prepared by the aforementioned method of the present invention.
  • the third aspect of the present invention also provides an optical fiber preform, which includes in order from the central axis from the inside to the outside: a core rod with a tail shank, a high-purity silica column at the tail, and a quartz cladding tube with a tail shank, wherein, The mandrel with the tail shank is assembled inside the quartz cladding sleeve, the gap between the cladding sleeve with the tail shank and the mandrel with the tail shank is filled with high-purity quartz powder, and the tail tube is filled with a high-purity quartz column.
  • the end of the tail handle of the preform is equipped with a tail cover plate with a barometer, an air inlet, a suction port and a Teflon sealing ring to fix the position of the mandrel,
  • the air pressure gauge is installed at the outlet of the suction port, and a valve is installed at the rear, and its positive pressure and negative pressure can be displayed; a valve is installed on the gas inlet; and there are three sealing rings, from the inside to the outside. They are respectively fixed on the end of the mandrel tail handle, the end of the tail high-purity quartz column and the end of the casing tail shank, forming two between the mandrel tail shank and the tail high-purity quartz column and between the tail high-purity quartz column and the casing tail shank. The two annular gaps between the two annular gaps are slotted on the outer surface of the other end of the high-purity quartz column at the tail, so that the two annular gaps can communicate with the quartz powder area.
  • the gap between the cladding sleeve with a tail shank and the core rod with a tail shank is filled with high-purity quartz powder, and the purity of the high-purity quartz powder is not less than 99.999%.
  • the tail pipe is filled with a high-purity quartz column.
  • the high-purity quartz column refers to a high-purity quartz column with a special structure, for example, a hole in the middle shown in FIG. 5 and a surface at one end. Quartz column with longitudinal shallow grooves.
  • the present invention provides a method for preparing an optical fiber preform containing a functional silica cladding.
  • the optical fiber preform containing a functional cladding prepared by the method can meet the optical performance requirements of the optical fiber preform, as shown in Figure 6.
  • the functional cladding area with raised or lowered refractive index appearing in Fig. 7, and the method provided by the present invention can reduce the production cost.
  • the method provided by the present invention can avoid multiple deposition operations, and can simplify the manufacturing difficulty of the preform core rod.
  • the present invention also provides a method to simplify the manufacturing difficulty of some special structure preforms, for example, ultra-low loss G652 optical fiber preforms, G654 optical fiber preforms and G657 optical fiber preforms.
  • some special structure preforms for example, ultra-low loss G652 optical fiber preforms, G654 optical fiber preforms and G657 optical fiber preforms.
  • the method for preparing optical fiber preforms containing functional silica cladding provided by the present invention can solve this problem. problem.
  • Figure 1 is a schematic diagram of the structure of the casing preform
  • Figure 2 is a schematic diagram of the components of the preform before assembly
  • Fig. 3 is a schematic diagram of the preform after the components in Fig. 2 are assembled and filled with quartz powder;
  • Figure 4 is a schematic diagram of the combined structure of the tail cover of the preform
  • Figure 5 is a schematic diagram of grooves on the surface of a high-purity quartz column
  • FIG. 6 is a schematic view of the refractive index profile of a functional cladding optical fiber preform prepared by using silicon tetrachloride doping in Example 1 of the present application;
  • Example 7 is a schematic diagram of the emissivity profile of a functional cladding optical fiber preform prepared by doping with silicon tetrafluoride in Example 1 of the present application.
  • the high-purity quartz powder in the present invention refers to quartz powder with a purity of not less than 99.999%
  • the high-purity quartz column refers to a quartz column made of quartz material that meets or exceeds the GE214 standard. Unless specifically explained, other terms involved in the present invention are interpreted according to the conventional meaning in the art.
  • the quartz cladding sleeve and the pre-designed core rod After pickling the quartz cladding sleeve and the pre-designed core rod, they are assembled in a hundred-level clean space. After the assembly is completed, the gap between the cladding sleeve and the core rod is filled with high-purity quartz powder (purity Not less than 99.999%).
  • Three sealing rings are respectively fixed at the end of the mandrel tail handle, the end of the tail high-purity quartz column and the end of the sleeve tail handle from the inside to the outside, forming two between the mandrel tail handle and the tail high-purity quartz column and the tail high-purity
  • the two annular gaps between the quartz column and the tail shank of the casing are slotted on the outer surface of the other end of the high-purity quartz column at the tail, as shown in Figure 5, so that the two annular gaps can communicate with the quartz powder area.
  • Silicon tetrafluoride is used to generate a functional cladding with a lower refractive index than that of undoped silica glass; silicon tetrachloride is used to generate a functional cladding with a higher refractive index than that of undoped silica glass.
  • Schematic diagrams of the refractive index profile distribution of the prepared optical fiber preform are shown in Figures 6 and 7, respectively.

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Abstract

一种含功能性包层光纤预制棒及其制备方法，该方法所制备含功能性包层光纤预制棒能够满足预制棒对光学性能的要求，降低生产成本，此外，该方法能够降低简化预制棒芯棒的制造难度，简化了部分特殊结构预制棒的制造难度。

Description

含有功能性石英包层的光纤预制棒及其制备方法 技术领域
本发明属于光纤技术领域，具体涉及一种含有功能性石英包层的光纤预制棒及其制备方法。
背景技术
制造光纤时，必须先将经过提纯的原料制成一根满足一定要求的玻璃棒，称之为“光纤预制棒”，光纤预制棒是拉制光纤的原始棒体材料，其内层为高折射率(n1)的芯层，外层为低折射率(n2)的包层，应具有符合要求的折射率分布与几何尺寸。典型的光纤预制棒直径约为10～25nm，长度约为60～120nm。
在通信光纤制备过程中，重要内容之一是光纤预制棒的制备，光纤预制棒的制造分为芯棒制造与外包层制造，即先制造芯棒(包括芯层和光学包层)，再在芯棒外面沉积包层而制得光纤预制棒。目前，用于制备光纤预制棒的技术主要有以等离子体化学气相沉积法(PCVD)和改进的化学气相沉积法(MCVD)为代表的管内法和以轴向气相沉积法(VAD)和外气相沉积法((OVD)为代表的管外法。外包层制造以直接OVD合成和石英套管组装为主。
在利用管外法沉积制备光纤预制棒时，由于需要抽取沉积腔中的反应废气，需要利用尾气处理设备向沉积腔体提供一定负压。在该抽取过程中，尾气处理设备不但会抽走反应废气，同时也会抽取出一定的反应生成物，即纳米二氧化硅粉末。在使用布袋除尘型的干式尾气 处理设备时，能够得到相对含水量、含盐量都较低的纳米二氧化硅粉饼，这些颗粒直接排放到空气中会造成粉尘污染。目前废料主要处理方式是填埋，但填埋方式，仍然会对环境特别是土壤造成一定的危害，且浪费资源。
使用套管法制备光纤预制棒，可以使光纤预制棒的制造工艺实现从一步法到二步法的转变，以提高生产效率。套管预制棒由预先制备好的芯棒和套管组成，通过从套管尾柄末端进行真空抽取，并于拉丝炉或延伸炉中进行融缩操作，最终成为光纤或光纤预制棒。套管预制棒的结构示意图如图1所示。
套管预制棒的芯棒包含芯层和内包层，其中内包层为进行一定掺杂调整折射率后的石英玻璃，而套管则作为光纤预制棒的外包层，该外包层一般为纯石英玻璃。整根光纤预制棒的导光结构主要依靠芯棒的设计来实现，所以对于芯棒的制备要求很高。但是，对于一些沉积工艺来说，制备低衰减、超强抗弯曲的芯棒是存在困难的，很难直接通过套管棒工艺实现。
发明内容
本发明要解决的技术问题是针对上述现有技术中存在的对于有复杂折射率剖面设计的(多层不同折射率)，且对掺杂剂有一定掺杂浓度要求的光纤预制棒芯层的设计，难以通过VAD或者OVD设备进行一次沉积成型的问题，本发明提供一种可避免进行多次沉积的操作 的含有功能性石英包层的光纤预制棒的制备方法，以及由该方法制备的光纤预制棒。
本发明解决其技术问题所采用的技术方案是：首先本发明提供了一种含有功能性石英包层的光纤预制棒的制备方法，包括以下步骤：
(T1)、将石英包层套管和芯棒酸洗后，进行组装，其中，所述芯棒是带有尾柄的芯棒，所述石英包层套管是带有尾柄的石英包层套管；
(T2)将步骤(T1)石英包层套管和芯棒组装完成后，在包层套管和芯棒的间隙填入高纯石英粉末；优选地，所述高纯石英粉末的纯度不低于99.999％；
(T3)在尾管内填入高纯石英柱；优选地，所述的高纯石英柱是指具有特殊结构的高纯石英柱，例如，如附图5中所示的中间带孔，一端有表面开纵向浅槽的石英柱；
(T4)安装尾部盖板：在光纤预制棒尾柄末端安装带有气压表、进气口、抽气口和特氟龙密封圈的尾部盖板，用以固定芯棒位置；
(T5)将光纤预制棒挂至融缩设备上，对石英粉末进行掺杂处理，然后融缩烧结得到透明玻璃棒。
其中，上述方法中，步骤(T4)所述气压表安装于抽气口出口位置，后部安装阀门，其正压与负压均可显示，所述进气口上安装有阀门，所述密封圈有三个，从内到外分别固定在芯棒尾柄末端、尾部高纯石英柱末端和套管尾柄末端，形成两个位于芯棒尾柄与尾部高纯石英柱之间和尾部高纯石英柱与套管尾柄之间的两个环形间隙，通过在 尾部高纯石英柱另一端外表面开槽，使得两个环形间隙均能与石英粉末区域联通。
进一步的，上述方法中，步骤(T5)所述对石英粉末进行掺杂处理包括：关闭出气口的阀门，向进气口通入由掺杂气体、氦气、氩气或氮气组成的混合气体，持续通入气体，然后将预制棒放入加热炉中，升温至1200℃～1400℃，使掺杂气体与石英粉末进行充分反应。优选地，其中所述掺杂气体为四氯化硅或四氟化硅。
更进步一步的，上述方法中，步骤(T5)所述融缩烧结方法包括：掺杂气体与石英粉末进行充分反应后，降温至600～800℃，打开抽气阀门，负压抽取预制棒内部的混合气体，然后打开进气端阀门，向预制棒内部供入氦气或氦气与掺杂气体的混合气，待压力表示数稳定后，升温至融缩温度，将包层套管、经过掺杂的石英粉末和芯棒融缩烧结为完整的透明玻璃棒；
优选地，其中步骤(T5)所述掺杂气体为四氯化硅或四氟化硅。
其中步骤(T5)，不同的掺杂气体的效果不同，通入四氟化硅是为了生成比无掺杂的石英玻璃折射率更低的功能性包层；通入四氯化硅是为了生成比无掺杂石英玻璃折射率更高的功能性包层。例如，使用四氯化硅掺杂制备成的功能性包层光纤预制棒折射率剖面分布示意如图6所示；使用四氟化硅掺杂制备成的含功能性包层光纤预制棒的射率剖面示意图如图7所示。
本发明第二方面还提供了一种光纤预制棒，其由本发明前述方法制备得到。
本发明第三方面还提供了一种光纤预制棒，其由从中心轴由内向外依次包括：带尾柄的芯棒、尾部高纯石英柱和带尾柄的石英包层套管，其中，带尾柄的芯棒组装在石英包层套管内部，带尾柄的包层套管和带尾柄的芯棒的间隙内填有高纯石英粉末，尾管内填有高纯石英柱。
进一步，优选地，所述预制棒的尾柄末端安装带有气压表、进气口、抽气口和特氟龙密封圈的尾部盖板，用以固定芯棒位置，
更进一步的，所述气压表安装于抽气口出口位置，后部安装阀门，其正压与负压均可显示；所述进气口上安装有阀门；所述密封圈有三个，从内到外分别固定在芯棒尾柄末端、尾部高纯石英柱末端和套管尾柄末端，形成两个位于芯棒尾柄与尾部高纯石英柱之间和尾部高纯石英柱与套管尾柄之间的两个环形间隙，通过在尾部高纯石英柱另一端外表面开槽，使得两个环形间隙均能与石英粉末区域联通。
更进一步的，所述光纤预制棒，其带尾柄的包层套管和带尾柄的芯棒的间隙内填有高纯石英粉末，所述高纯石英粉末的纯度不低于99.999％。所述的尾管内填有高纯石英柱，优选地，所述的高纯石英柱是指具有特殊结构的高纯石英柱，例如，如附图5中所示的中间带孔，一端有表面开纵向浅槽的石英柱。
本发明的有益效果是：
第一、本发明提供了一种含功能性石英包层的光纤预制棒的制备方法，所述方法制备的含功能性包层光纤预制棒能够满足光纤预制棒对光学性能的要求，如图6和图7中出现的折射率抬高或者降低的功 能性包层区域，并且，本发明提供的方法能够降低生产成本。
第二、现有技术对于有复杂折射率剖面设计的(多层不同折射率)，且对掺杂剂有一定掺杂浓度要求的光纤预制棒芯层的设计，难以通过VAD或者OVD设备进行一次沉积成型，本发明提供的方法可避免进行多次沉积的操作，能够简化预制棒芯棒的制造难度。
第三、本发明还提供简化了部分特殊结构预制棒的制造难度的方法，例如，超低损耗的G652光纤预制棒、G654光纤预制棒和G657光纤预制棒，为了实现其光学特性，需要设置某些低折射率区域或者高折射率区域，在普通VAD或者OVD工艺中难以提高掺杂浓度或难以实现掺杂，而本发明提供的含有功能性石英包层的光纤预制棒的制备方法能够解决该问题。
附图说明
下面结合附图和实施例对本申请的技术方案进一步说明。
图1是套管预制棒结构示意图；
图2是预制棒组装前的部件示意图；
图3是图2中各部件组装完成并填充石英粉末后的预制棒示意图；
图4是预制棒尾部盖板组合结构示意图；
图5是高纯石英柱表面开槽示意图；
图6是本申请实施例1使用四氯化硅掺杂制备成的含功能性包层光纤预制棒的折射率剖面示意图；
图7是本申请实施例1使用四氟化硅掺杂制备成的含功能性包层光纤预制棒的射率剖面示意图。
具体实施方式
需要说明的是，在不冲突的情况下，本申请中的实施例及实施例中的特征可以相互组合。本发明所述高纯石英粉末是指纯度不低于99.999％的石英粉末，所述高纯石英柱是指由满足或者高于GE214标准的石英材质制成的石英柱。本发明所涉及其他术语除非特别解释，均按照本领域常规含义解释。
实施例1含功能性包层的光纤预制棒的制备
将石英包层套管和预先设计好的芯棒进行酸洗后，在百级洁净空间内进行组装，组装完成后，在包层套管和芯棒的间隙内填入高纯石英粉末(纯度不低于99.999％)。
预制棒组装完成后，在其尾柄末端安装上带有气压表(正压与负压均可显示，安装于抽气口出口位置，后部安装阀门)、进气口(需安装阀门)、抽气口和特氟龙密封圈的尾部盖板，用以固定芯棒位置。盖板内部通以冷却水进行冷却，盖板结构如图4所示
三个密封圈从内到外分别固定在芯棒尾柄末端、尾部高纯石英柱末端和套管尾柄末端，形成两个位于芯棒尾柄与尾部高纯石英柱之间和尾部高纯石英柱与套管尾柄之间的两个环形间隙，通过在尾部高纯石英柱的另一端外表面开槽，如图5，使得两个环形间隙均能与石英粉末区域联通。
在安装完尾部盖板后，将预制棒挂设至融缩设备上，关闭出气口的阀门，向进气口通入掺杂气体(可使用四氯化硅或四氟化硅)、氦 气、其他惰性气体(氩气、氮气等)按一定比例混合的混合气体。持续通入气体，并观察抽气口处气压表的正压示数，达到工艺需求的压力后关闭进气口。随后将预制棒缓慢下降放入加热炉中，缓慢升温至1200℃至1400℃(该温度视需掺杂的掺杂源、需要的掺杂浓度等工艺要求确定)，维持温度一定时间以保证掺杂剂进行充分反应。随后逐步降温至800℃，打开抽气阀门，以一定负压抽取预制棒内部的混合气体，当达到一定工艺压力后，打开进气端阀门，向预制棒内部供入氦气(或氦气与掺杂气体的混合气)，待压力表示数稳定后，逐步升温至融缩温度，将包层套管、经过掺杂的石英粉末和芯棒融缩烧结为完整的透明玻璃棒。
该过程中，不同的掺杂气体的效果不同。通入四氟化硅是为了生成比无掺杂的石英玻璃折射率更低的功能性包层；通入四氯化硅是为了生成比无掺杂石英玻璃折射率更高的功能性包层。制备所得的光纤预制棒折射率剖面分布示意图分别如图6和7所示。
以上述依据本申请的理想实施例为启示，通过上述的说明内容，相关工作人员完全可以在不偏离本项申请技术思想的范围内，进行多样的变更以及修改。本项申请的技术性范围并不局限于说明书上的内容，必须要根据权利要求范围来确定其技术性范围。

Claims (10)

  1. 一种含有功能性石英包层的光纤预制棒的制备方法，其特征在于，包括以下步骤：
    (T1)、将石英包层套管和芯棒酸洗后，进行组装，其中，所述芯棒是带有尾柄的芯棒，所述石英包层套管是带有尾柄的石英包层套管；
    (T2)将步骤(T1)石英包层套管和芯棒组装完成后，在包层套管和芯棒的间隙填入高纯石英粉末；
    (T3)在尾管内填入高纯石英柱；
    (T4)安装尾部盖板：在光纤预制棒尾柄末端安装带有气压表、进气口、抽气口和特氟龙密封圈的尾部盖板，用以固定芯棒位置；
    (T5)将光纤预制棒挂至融缩设备上，对石英粉末进行掺杂处理，然后融缩烧结得到透明玻璃棒。
  2. 根据权利要求1所述方法，其特征在于，步骤(T4)所述气压表安装于抽气口出口位置，后部安装阀门，其正压与负压均可显示，所述进气口上安装有阀门，所述密封圈有三个，从内到外分别固定在芯棒尾柄末端、尾部高纯石英柱末端和套管尾柄末端，形成两个位于芯棒尾柄与尾部高纯石英柱之间和尾部高纯石英柱与套管尾柄之间的两个环形间隙，通过在尾部高纯石英柱另一端外表面开槽，使得两个环形间隙均能与石英粉末区域联通。
  3. 根据权利要求1所述方法，其特征在于，步骤(T5)所述对石英粉末进行掺杂处理包括：关闭出气口的阀门，向进气口通入由掺杂气体、氦气、氩气或氮气组成的混合气体，持续通入气体，然后将 预制棒放入加热炉中，升温至1200℃～1400℃，使掺杂气体与石英粉末进行充分反应。
  4. 根据权利要求1所述方法，其特征在于，步骤(T5)所述融缩烧结方法包括：掺杂气体与石英粉末进行充分反应后，降温至600～800℃，打开抽气阀门，负压抽取预制棒内部的混合气体，然后打开进气端阀门，向预制棒内部供入氦气或氦气与掺杂气体的混合气，待压力表示数稳定后，升温至融缩温度，将包层套管、经过掺杂的石英粉末和芯棒融缩烧结为完整的透明玻璃棒。
  5. 根据权利要求3～4任一项所述方法，其特征在于，所述掺杂气体为四氯化硅或四氟化硅。
  6. 根据权利要求1所述方法，其特征在于，所述高纯石英粉末的纯度不低于99.999％。
  7. 一种光纤预制棒，其特征在于，由权利要求1～6任一项所述方法制备得到。
  8. 一种光纤预制棒，其特征在于，由从中心轴由内向外依次包括：带尾柄的芯棒、尾部高纯石英柱和带尾柄的石英包层套管，其中，带尾柄的芯棒组装在石英包层套管内部，带尾柄的包层套管和带尾柄的芯棒的间隙内填有高纯石英粉末，尾管内填有高纯石英柱。
  9. 根据权利要求8所述的光纤预制棒，其特征在于，所述预制棒的尾柄末端安装带有气压表、进气口、抽气口和特氟龙密封圈的尾部盖板，用以固定芯棒位置，
    所述气压表安装于抽气口出口位置，后部安装阀门，其正压与负 压均可显示；所述进气口上安装有阀门；所述密封圈有三个，从内到外分别固定在芯棒尾柄末端、尾部高纯石英柱末端和套管尾柄末端，形成两个位于芯棒尾柄与尾部高纯石英柱之间和尾部高纯石英柱与套管尾柄之间的两个环形间隙，通过在尾部高纯石英柱另一端外表面开槽，使得两个环形间隙均能与石英粉末区域联通。
  10. 根据权利要求8～9任一项所述方法，其特征在于，带尾柄的包层套管和带尾柄的芯棒的间隙内填有高纯石英粉末，所述高纯石英粉末的纯度不低于99.999％。
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