WO2021087712A1 - Barium titanate single crystal optical fiber clad in alumina-phosphate glass and preparation method therefor - Google Patents

Barium titanate single crystal optical fiber clad in alumina-phosphate glass and preparation method therefor Download PDF

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WO2021087712A1
WO2021087712A1 PCT/CN2019/115527 CN2019115527W WO2021087712A1 WO 2021087712 A1 WO2021087712 A1 WO 2021087712A1 CN 2019115527 W CN2019115527 W CN 2019115527W WO 2021087712 A1 WO2021087712 A1 WO 2021087712A1
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single crystal
cladding
alumina
phosphate glass
fiber
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PCT/CN2019/115527
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French (fr)
Chinese (zh)
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沈荣存
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南京同溧晶体材料研究院有限公司
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Priority to PCT/CN2019/115527 priority Critical patent/WO2021087712A1/en
Publication of WO2021087712A1 publication Critical patent/WO2021087712A1/en

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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/12—Silica-free oxide glass compositions
    • C03C3/16—Silica-free oxide glass compositions containing phosphorus
    • C03C3/17—Silica-free oxide glass compositions containing phosphorus containing aluminium or beryllium
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B1/00—Single-crystal growth directly from the solid state
    • 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
    • G02B6/02—Optical fibres with cladding with or without a coating

Definitions

  • the invention relates to the technical field of optical fibers, in particular to a barium titanate single crystal optical fiber clad with alumina-phosphate glass and a preparation method thereof.
  • the traditional optical fiber is prepared with inorganic glass or organic polymer as the raw material by the method of melting control.
  • the single crystal fiber as the name suggests, not only has the slender structure and light guiding ability of traditional optical fiber, but also has the unique ordered structure of single crystal material and the physical properties of light, electricity, heat and magnetism. It is made of single crystal material. Commonly used single crystal fibers include Nd:YAG, Ti:Al2O3, Cr:Al2O3, LiNbO3, KBr, Mn2SiO4, etc. In recent years, single crystal optical fiber has received extensive attention due to its unique physical properties and its important application potential in laser technology, sensor technology, integrated optoelectronic systems and other fields.
  • the parameters reflecting the quality of single crystal fiber include diameter, length, intensity, etc.
  • Optical parameters include absorption and emission characteristics, absorption and scattering light conduction loss, which are related to the growth conditions and the internal and surface defects of the fiber. It is of great significance to explore and research the physical properties of single crystal fibers based on different materials.
  • Single crystal fibers are currently mainly made of crystalline materials by drawing and growing, which have the dual characteristics of crystals and fibers.
  • Single crystal fiber has the characteristics of high strength and high temperature resistance, and can be used in a wide range of fields such as conduction, sensing, frequency doubling and holographic data storage.
  • Due to the high refractive index of the crystal it is difficult for the single crystal fiber to be made into a core-cladding structure.
  • the existing single crystal fiber usually has an unclad structure.
  • the single crystal fiber without cladding structure has large transmission loss, its characteristics are easily affected by environmental changes, and the integrity of the fiber surface is also vulnerable to damage.
  • magnesium-doped lithium niobate LiNbO3
  • LiNbO3 pure lithium niobate crystal
  • the present invention provides an alumina-phosphate glass clad barium titanate single crystal optical fiber and a preparation method thereof.
  • the present invention provides an alumina-phosphate glass clad barium titanate single crystal optical fiber, comprising an optical fiber core and a clad material covering the fiber core; the clad material is doped alumina and Er 3+ multi-component phosphate glass, the fiber core material is a composite single crystal fiber, and the composite single crystal fiber is Eu 4+ /Lu 3+ : BaTiO 3 .
  • the fiber core material is a single crystal selenium-tellurium compound.
  • the molar ratio of Eu 4+ to Lu 3+ is (8-12):1.
  • the content of alumina is 5-15 parts by weight, and the content of Er 3+ is 0.5-1.5 parts by weight, based on parts by weight.
  • the composition of the multi-component phosphate glass is: P 2 O 5 : 45 ⁇ 65 parts by weight; K 2 O: 10 ⁇ 20 parts by weight; BaO: 5 ⁇ 10 parts by weight; Al 2 O 3 : 10 ⁇ 20 parts by weight.
  • the ratio of the total number of moles of Eu 4+ and Lu 3+ to the number of moles of BaTiO3 is (1-5):100.
  • the present invention also provides a method for preparing the above-mentioned alumina-phosphate glass-clad barium titanate single crystal optical fiber, which is prepared by using the crystal fiber and its cladding synchronous preparation equipment, and includes the following steps:
  • the seed crystal is seeded on the top of the cladding column. Due to the capillary action, the crystal fiber raw material melt in the lower crucible reaches the top of the cladding column through the crystal fiber supply forming tube. First touch the crystal fiber raw material melt in the crystal fiber supply forming tube, and begin to shoulder;
  • the crystal fiber raw materials are BaTiO 3 , Eu 2 O 3 , and Lu 2 O 3 .
  • the cladding material is a multi-component phosphate glass doped with alumina and Er 3+.
  • the alumina-phosphate glass clad barium titanate single crystal fiber provided by the present invention adopts the fiber core and the clad material coated on the fiber core.
  • the preparation process of the fiber core is simple and has excellent absorption characteristics and The up-conversion strength greatly increases the application range of BaTiO3 single crystal fiber; the clad material uses multi-component phosphate glass doped with alumina and Er 3+ , which is low in cost and can meet the requirements of total reflection.
  • the synchronous preparation equipment of the crystal fiber and its cladding layer of the present application has a simple structure and low cost.
  • the equipment can be used to prepare the cladding layer on the surface of the crystal fiber while growing the crystalline fiber, which greatly reduces the production cost and increases the efficiency of device preparation;
  • the cladding layer is a single crystal cladding, which can be the same matrix as the crystalline fiber or a different matrix.
  • the single crystal cladding has more excellent physical and chemical properties.
  • Composite single crystal fiber Eu 4+ /Lu 3+ : BaTiO 3 among them, the molar ratio of Eu 4+ and Lu 3+ is 8:1, and the ratio of the total number of moles of Eu 4+ and Lu 3+ to the number of moles of BaTiO3 is 3:100.
  • the composite single crystal optical fiber and the preparation method thereof include the following steps:
  • the seed crystal is connected to the top of the mold to pull the melt, so that the seed crystal continuously rearranges atoms or molecules at the interface of the melt, and gradually solidifies as the temperature drops to grow a single crystal with the same shape as the edge of the mold.
  • Composite single crystal fiber Eu 4+ /Lu 3+ : BaTiO 3 among them, the molar ratio of Eu 4+ and Lu 3+ is 12:1, and the ratio of the total number of moles of Eu 4+ and Lu 3+ to the number of moles of BaTiO3 is 1:100.
  • the composite single crystal optical fiber and the preparation method thereof include the following steps:
  • the seed crystal is connected to the top of the mold to pull the melt, so that the seed crystal continuously rearranges atoms or molecules at the interface of the melt, and gradually solidifies as the temperature drops to grow a single crystal with the same shape as the edge of the mold.
  • Composite single crystal fiber Eu 4+ /Lu 3+ : BaTiO 3 among them, the molar ratio of Eu 4+ and Lu 3+ is 12:1, and the ratio of the total number of moles of Eu 4+ and Lu 3+ to the number of moles of BaTiO3 is 5:100.
  • the composite single crystal optical fiber and the preparation method thereof include the following steps:
  • the seed crystal is connected to the top of the mold to pull the melt, so that the seed crystal continuously rearranges atoms or molecules at the interface of the melt, and gradually solidifies as the temperature drops to grow a single crystal with the same shape as the edge of the mold.
  • the sample is made into a cylindrical optical fiber with a diameter of 1.0mm and a length of 4mm. The two sides are carefully polished and placed in a fiber coupler.
  • the quartz lamp is used as the light source for measurement.
  • the measurement spectrum ranges from 500 to 1000 nm.
  • a 650nm semiconductor laser was used as the pump light source to pump the sample and measure the up-conversion spectrum of each sample.
  • the results show that BaTiO 3 has an up-conversion spectrum, but the intensity is very weak; however, the composite single crystal fiber Eu 4+ /Lu 3+ : BaTiO 3 of Examples 1 to 3 has an up-conversion spectrum that is much stronger than BaTiO 3 .
  • Alumina-phosphate glass-clad barium titanate single crystal fiber includes an optical fiber core and a cladding material covering the fiber core; the cladding material is a multi-component phosphate glass, and the optical fiber is
  • the core material is a composite single crystal fiber, and the composite single crystal fiber is Eu 4+ /Lu 3+ : BaTiO 3 .
  • Composite single crystal fiber Eu 4+ /Lu 3+ : BaTiO 3 among them, the molar ratio of Eu 4+ and Lu 3+ is 12:1, and the ratio of the total number of moles of Eu 4+ and Lu 3+ to the number of moles of BaTiO3 is 3:100.
  • the composite single crystal optical fiber and the preparation method thereof are prepared by the simultaneous preparation equipment of the crystal fiber and its cladding, including the following steps:
  • the seed crystal is seeded on the top of the cladding column. Due to the capillary action, the crystal fiber raw material melt in the lower crucible reaches the top of the cladding column through the crystal fiber supply forming tube. First touch the crystal fiber raw material melt in the crystal fiber supply forming tube, and begin to shoulder;
  • Alumina-phosphate glass-clad barium titanate single crystal fiber includes an optical fiber core and a cladding material covering the fiber core; the cladding material is a multi-component phosphate glass, and the optical fiber is
  • the core material is a composite single crystal fiber, and the composite single crystal fiber is Eu 4+ /Lu 3+ : BaTiO 3 .
  • Composite single crystal fiber Eu 4+ /Lu 3+ : BaTiO 3 among them, the molar ratio of Eu 4+ and Lu 3+ is 10:1, and the ratio of the total number of moles of Eu 4+ and Lu 3+ to the number of moles of BaTiO3 is 1:100.
  • the composite single crystal optical fiber and the preparation method thereof are prepared by the simultaneous preparation equipment of the crystal fiber and its cladding, including the following steps:
  • the raw materials of the crystal fiber are BaTiO3, Eu2O3, Lu2O3, and the cladding raw materials are doped alumina and Er 3+ multi-component phosphate glass, the content of alumina is 5 parts by weight, and the content of Er 3+ is 0.5 parts by weight, based on parts by weight;
  • the composition of the multi-component phosphate glass is: P 2 O 5 : 45 parts by weight; K 2 O: 20 parts by weight; BaO: 10 parts by weight; Al 2 O 3 : 20 parts by weight;
  • the seed crystal is seeded on the top of the cladding column. Due to the capillary action, the crystal fiber raw material melt in the lower crucible reaches the top of the cladding column through the crystal fiber supply forming tube. First touch the crystal fiber raw material melt in the crystal fiber supply forming tube, and begin to shoulder;
  • Alumina-phosphate glass-clad barium titanate single crystal fiber includes an optical fiber core and a cladding material covering the fiber core; the cladding material is a multi-component phosphate glass, and the optical fiber is
  • the core material is a composite single crystal fiber, and the composite single crystal fiber is Eu 4+ /Lu 3+ : BaTiO 3 .
  • Composite single crystal fiber Eu 4+ /Lu 3+ : BaTiO 3 among them, the molar ratio of Eu 4+ and Lu 3+ is 10:1, and the ratio of the total number of moles of Eu 4+ and Lu 3+ to the number of moles of BaTiO3 is 5:100.
  • the composite single crystal optical fiber and the preparation method thereof are prepared by the simultaneous preparation equipment of the crystal fiber and its cladding, including the following steps:
  • the raw materials of the crystal fiber are BaTiO3, Eu2O3, Lu2O3, and the cladding raw materials are doped alumina and Er3+ multi-component phosphate glass, the content of alumina is 15 parts by weight, and the content of Er 3+ is 1.5 parts by weight, based on parts by weight;
  • the composition of the multi-component phosphate glass is: P 2 O 5 : 65 Parts by weight; K 2 O: 10 parts by weight; BaO: 5 parts by weight; Al 2 O 3 : 10 parts by weight;
  • the seed crystal is seeded on the top of the cladding column. Due to the capillary action, the crystal fiber raw material melt in the lower crucible reaches the top of the cladding column through the crystal fiber supply forming tube. First touch the crystal fiber raw material melt in the crystal fiber supply forming tube, and begin to shoulder;

Abstract

Provided is a barium titanate single crystal optical fiber clad in alumina-phosphate glass, comprising an optical fiber core and a cladding material covering the exterior of the optical fiber core; the cladding material is multi-component phosphate glass doped with alumina and Er3+, the material of the optical fiber core is a composite single crystal optical fiber, and the composite single crystal optical fiber is Eu4+/Lu3+: BaTiO3. Further provided is a method for preparing the described barium titanate single crystal optical fiber clad in alumina-phosphate glass. The barium titanate single crystal optical fiber clad in alumina-phosphate glass provided in the present invention comprises an optical fiber core and a cladding material covering the exterior of the optical fiber core. The preparation process for the optical fiber core is simple, and the optical fiber core has excellent absorption characteristics and upconversion strength, which greatly improves the range of application of a BaTiO3 single crystal optical fiber. In addition, the cladding material uses multi-component phosphate glass doped with alumina and Er3+, thus costs are low and the requirement of total reflection can be met.

Description

一种氧化铝-磷酸盐玻璃包层的钛酸钡单晶光纤及其制备方法Alumina-phosphate glass clad barium titanate single crystal optical fiber and preparation method thereof 技术领域Technical field
本发明涉及光纤技术领域，特别一种氧化铝-磷酸盐玻璃包层的钛酸钡单晶光纤及其制备方法。The invention relates to the technical field of optical fibers, in particular to a barium titanate single crystal optical fiber clad with alumina-phosphate glass and a preparation method thereof.
背景技术Background technique
传统的光纤是以无机玻璃或有机聚合物为原料，通过烙融控制的方法制备的。而单晶光纤，顾名思义，就是既具备传统光纤的细长结构和导光能力，又具备单晶材料特有的有序结构和光、电、热、磁等物理性质，其是由单晶材料制成的光学纤维，常用的单晶光纤有Nd:YAG、Ti:Al2O3、Cr:Al2O3、LiNbO3、KBr、Mn2SiO4等。近年来，单晶光纤由于其独特的物理性能，在激光技术、传感技术、集成光电***等领域具有重要的应用潜力而受到广泛的关注。The traditional optical fiber is prepared with inorganic glass or organic polymer as the raw material by the method of melting control. The single crystal fiber, as the name suggests, not only has the slender structure and light guiding ability of traditional optical fiber, but also has the unique ordered structure of single crystal material and the physical properties of light, electricity, heat and magnetism. It is made of single crystal material. Commonly used single crystal fibers include Nd:YAG, Ti:Al2O3, Cr:Al2O3, LiNbO3, KBr, Mn2SiO4, etc. In recent years, single crystal optical fiber has received extensive attention due to its unique physical properties and its important application potential in laser technology, sensor technology, integrated optoelectronic systems and other fields.
    单晶光纤反映单晶光纤质量的参数有直径、长度、强度等，光学参数有吸收和发射特性，吸收和散射光传导损耗，这些与其生长条件和光纤内在及表面缺陷都有关系。对基于不同材料的单晶光纤的制备技术巧物理性能开展探索和研究具有十分重要的意义。... The parameters reflecting the quality of single crystal fiber include diameter, length, intensity, etc. Optical parameters include absorption and emission characteristics, absorption and scattering light conduction loss, which are related to the growth conditions and the internal and surface defects of the fiber. It is of great significance to explore and research the physical properties of single crystal fibers based on different materials.
    单晶光纤目前主要由晶体材料拉丝生长而成，具有晶体和纤维的双重特性。单晶光纤具有高强度、耐高温等特点，可应用于传导、传感、倍频和全息数据存储等广泛领域。但由于晶体折射率较高，单晶光纤很难做成纤芯-包层结构，现有的单晶光纤通常为无包层结构。无包层结构的单晶光纤传输损耗大，特性易受环境变化影响，光纤表面的完整性也易受到破坏。... Single crystal fibers are currently mainly made of crystalline materials by drawing and growing, which have the dual characteristics of crystals and fibers. Single crystal fiber has the characteristics of high strength and high temperature resistance, and can be used in a wide range of fields such as conduction, sensing, frequency doubling and holographic data storage. However, due to the high refractive index of the crystal, it is difficult for the single crystal fiber to be made into a core-cladding structure. The existing single crystal fiber usually has an unclad structure. The single crystal fiber without cladding structure has large transmission loss, its characteristics are easily affected by environmental changes, and the integrity of the fiber surface is also vulnerable to damage.
    对于单晶光纤的包层结构，也有一些研究设计。主要是利用掺镁铌酸锂（MgO：LiNbO3）折射率比纯铌酸锂晶体（LiNbO3）折射率低的原理，使用MgO或者MgF通过扩散的方式将镁离子由外层向中心扩散，从而降低外层铌酸锂晶体的折射率，形成包层。1995年，西安交大阙文修等人在1995年《西安交通大学学报》29卷第9期中公布了利用此方法制作铌酸锂材料单晶光纤包层。这种方法仅适用于铌酸锂（LiNbO3）晶体生长的单晶光纤，对其它晶体材料并不适用，限制了包层应用的范围。另外，这种方法可控性差，扩散程度不均匀，扩散深度不宜控制，产品性能稳定性较差。... For the cladding structure of single crystal fiber, there are also some research designs. It mainly uses the principle that magnesium-doped lithium niobate (MgO: LiNbO3) has a lower refractive index than pure lithium niobate crystal (LiNbO3), and uses MgO or MgF to diffuse magnesium ions from the outer layer to the center through diffusion, thereby reducing The refractive index of the outer layer of lithium niobate crystal forms the cladding layer. In 1995, Que Wenxiu of Xi'an Jiaotong University and others announced the use of this method to make lithium niobate material single crystal optical fiber cladding in the 1995 "Journal of Xi'an Jiaotong University", Volume 29, Issue 9. This method is only suitable for single crystal fibers grown by lithium niobate (LiNbO3) crystals, and is not suitable for other crystal materials, which limits the scope of cladding applications. In addition, this method has poor controllability, uneven diffusion, unsuitable control of diffusion depth, and poor product performance stability.
技术问题technical problem
为了解决现有技术的缺陷，本发明提供了一种氧化铝-磷酸盐玻璃包层的钛酸钡单晶光纤及其制备方法。In order to solve the defects of the prior art, the present invention provides an alumina-phosphate glass clad barium titanate single crystal optical fiber and a preparation method thereof.
技术解决方案Technical solutions
本发明提供的一种氧化铝-磷酸盐玻璃包层的钛酸钡单晶光纤，包括光纤纤芯以及包覆于光纤纤芯外的包层材料；所述包层材料为掺杂氧化铝和Er 3+的多组分磷酸盐玻璃，所述光纤纤芯材料为复合单晶光纤，所述复合单晶光纤为Eu 4+/Lu 3+: BaTiO 3。 The present invention provides an alumina-phosphate glass clad barium titanate single crystal optical fiber, comprising an optical fiber core and a clad material covering the fiber core; the clad material is doped alumina and Er 3+ multi-component phosphate glass, the fiber core material is a composite single crystal fiber, and the composite single crystal fiber is Eu 4+ /Lu 3+ : BaTiO 3 .
优选地，光纤纤芯材料为单晶态硒碲化合物所述复合单晶光纤中，Eu 4+、Lu 3+的摩尔比为（8-12）：1。 Preferably, the fiber core material is a single crystal selenium-tellurium compound. In the composite single crystal fiber, the molar ratio of Eu 4+ to Lu 3+ is (8-12):1.
优选地，所述多组分磷酸盐玻璃中，氧化铝的掺量为5-15重量份，Er 3+的掺量为0.5-1.5重量份，以重量份计。 Preferably, in the multi-component phosphate glass, the content of alumina is 5-15 parts by weight, and the content of Er 3+ is 0.5-1.5 parts by weight, based on parts by weight.
优选地，所述多组分磷酸盐玻璃组成为：P 2O 5：45~65重量份；K 2O：10~20重量份；BaO：5~10重量份；Al 2O 3：10~20重量份。 Preferably, the composition of the multi-component phosphate glass is: P 2 O 5 : 45~65 parts by weight; K 2 O: 10~20 parts by weight; BaO: 5~10 parts by weight; Al 2 O 3 : 10~ 20 parts by weight.
优选地，所述Eu 4+、Lu 3+的总摩尔数与BaTiO3摩尔数之比为（1-5）：100。 Preferably, the ratio of the total number of moles of Eu 4+ and Lu 3+ to the number of moles of BaTiO3 is (1-5):100.
本发明还提供了上述氧化铝-磷酸盐玻璃包层的钛酸钡单晶光纤的制备方法，利用晶体纤维及其包层同步制备设备制得，包括以下步骤：The present invention also provides a method for preparing the above-mentioned alumina-phosphate glass-clad barium titanate single crystal optical fiber, which is prepared by using the crystal fiber and its cladding synchronous preparation equipment, and includes the following steps:
（1）在下坩埚内装入晶体光纤原料，在上坩埚内装入包层原料；加热下坩埚和上坩埚；(1) Load the crystal fiber raw material in the lower crucible, and load the cladding material in the upper crucible; heat the lower crucible and the upper crucible;
（2）待晶体光纤原料和包层原料融化后在包层柱顶部种籽晶，由于毛细管作用，下坩埚内的晶体光纤原料熔体通过晶体光纤供料成形管达到包层柱顶，籽晶先接触到晶体光纤供料成形管内的晶体光纤原料熔体，开始放肩；(2) After the crystal fiber raw material and the cladding material are melted, the seed crystal is seeded on the top of the cladding column. Due to the capillary action, the crystal fiber raw material melt in the lower crucible reaches the top of the cladding column through the crystal fiber supply forming tube. First touch the crystal fiber raw material melt in the crystal fiber supply forming tube, and begin to shoulder;
（3）晶体不断生长，由于毛细管作用，上坩埚内的包层原料熔体通过包层供料成形管达到包层柱顶，至晶体接触到包层供料成形管内的包层原料熔体，包层供料成形管内的包层原料熔体附着在光纤晶体外壁生长；从而光纤晶体和包层材料同步生长。(3) Crystals continue to grow. Due to capillary action, the cladding material melt in the upper crucible reaches the top of the cladding column through the cladding supply forming tube until the crystal contacts the cladding material melt in the cladding feeding forming tube. The cladding material melt in the cladding supply forming tube is attached to the outer wall of the fiber crystal to grow; thus, the fiber crystal and the cladding material grow simultaneously.
       优选地，步骤（1）中，所述晶体光纤原料为BaTiO 3、Eu 2O 3、Lu 2O 3。 Preferably, in step (1), the crystal fiber raw materials are BaTiO 3 , Eu 2 O 3 , and Lu 2 O 3 .
优选地，步骤（1）中，所述包层原料为掺杂氧化铝和Er 3+的多组分磷酸盐玻璃。 Preferably, in step (1), the cladding material is a multi-component phosphate glass doped with alumina and Er 3+.
有益效果Beneficial effect
本发明提供的氧化铝-磷酸盐玻璃包层的钛酸钡单晶光纤采用包括光纤纤芯以及包覆于光纤纤芯外的包层材料，光纤纤芯制备工艺简单，具有优异的吸收特性和上转换强度，大大提高了BaTiO3单晶光纤的应用范围；包层材料使用掺杂氧化铝和Er 3+的多组分磷酸盐玻璃，成本低，而且可以能够满足全反射的要求。 The alumina-phosphate glass clad barium titanate single crystal fiber provided by the present invention adopts the fiber core and the clad material coated on the fiber core. The preparation process of the fiber core is simple and has excellent absorption characteristics and The up-conversion strength greatly increases the application range of BaTiO3 single crystal fiber; the clad material uses multi-component phosphate glass doped with alumina and Er 3+ , which is low in cost and can meet the requirements of total reflection.
采用本申请的晶体纤维及其包层同步制备设备结构简单，成本低廉，利用该设备可在生长晶体纤维时同时制备晶体纤维表面的包层，大大降低了生产成本、增加器件制备效率；制备出的包层为单晶包层，可以与晶体纤维同基质，也可以不同基质，单晶包层拥有更加优异的物化性能。The synchronous preparation equipment of the crystal fiber and its cladding layer of the present application has a simple structure and low cost. The equipment can be used to prepare the cladding layer on the surface of the crystal fiber while growing the crystalline fiber, which greatly reduces the production cost and increases the efficiency of device preparation; The cladding layer is a single crystal cladding, which can be the same matrix as the crystalline fiber or a different matrix. The single crystal cladding has more excellent physical and chemical properties.
本发明的最佳实施方式The best mode of the present invention
下面对本发明作出进一步说明。The present invention will be further explained below.
       制备复合单晶光纤Eu 4+/Lu 3+: BaTiO 3。 Preparation of composite single crystal fiber Eu 4+ /Lu 3+ : BaTiO 3 .
实施例1 Example 1
       复合单晶光纤Eu 4+/Lu 3+: BaTiO 3；其中，Eu 4+、Lu 3+的摩尔比为8：1，Eu 4+、Lu 3+的总摩尔数与BaTiO3摩尔数之比为3：100。 Composite single crystal fiber Eu 4+ /Lu 3+ : BaTiO 3 ; among them, the molar ratio of Eu 4+ and Lu 3+ is 8:1, and the ratio of the total number of moles of Eu 4+ and Lu 3+ to the number of moles of BaTiO3 is 3:100.
    上述复合单晶光纤及其制备方法，包括以下步骤：... The composite single crystal optical fiber and the preparation method thereof include the following steps:
    （1）在坩埚中部放置中部设有毛细管的晶体生长模具，将原料BaTiO 3、Eu 2O 3、Lu 2O 3置于坩埚中，加热坩埚使原料熔化形成熔体； (1) Place a crystal growth mold with a capillary in the middle of the crucible, place the raw materials BaTiO 3 , Eu 2 O 3 , and Lu 2 O 3 in the crucible, and heat the crucible to melt the raw materials to form a melt;
    （2）在模具顶部接籽晶提拉熔体，使籽晶在熔体的交界面上不断进行原子或分子重排，随降温逐渐凝固而生长出与模具边缘形状相同的单晶。... (2) The seed crystal is connected to the top of the mold to pull the melt, so that the seed crystal continuously rearranges atoms or molecules at the interface of the melt, and gradually solidifies as the temperature drops to grow a single crystal with the same shape as the edge of the mold.
实施例2Example 2
       复合单晶光纤Eu 4+/Lu 3+: BaTiO 3；其中，Eu 4+、Lu 3+的摩尔比为12：1，Eu 4+、Lu 3+的总摩尔数与BaTiO3摩尔数之比为1：100。 Composite single crystal fiber Eu 4+ /Lu 3+ : BaTiO 3 ; among them, the molar ratio of Eu 4+ and Lu 3+ is 12:1, and the ratio of the total number of moles of Eu 4+ and Lu 3+ to the number of moles of BaTiO3 is 1:100.
       上述复合单晶光纤及其制备方法，包括以下步骤：... The composite single crystal optical fiber and the preparation method thereof include the following steps:
    （1）在坩埚中部放置中部设有毛细管的晶体生长模具，将原料BaTiO 3、Eu 2O 3、Lu 2O 3置于坩埚中，加热坩埚使原料熔化形成熔体； (1) Place a crystal growth mold with a capillary in the middle of the crucible, place the raw materials BaTiO 3 , Eu 2 O 3 , and Lu 2 O 3 in the crucible, and heat the crucible to melt the raw materials to form a melt;
    （2）在模具顶部接籽晶提拉熔体，使籽晶在熔体的交界面上不断进行原子或分子重排，随降温逐渐凝固而生长出与模具边缘形状相同的单晶。... (2) The seed crystal is connected to the top of the mold to pull the melt, so that the seed crystal continuously rearranges atoms or molecules at the interface of the melt, and gradually solidifies as the temperature drops to grow a single crystal with the same shape as the edge of the mold.
实施例3Example 3
       复合单晶光纤Eu 4+/Lu 3+: BaTiO 3；其中，Eu 4+、Lu 3+的摩尔比为12：1，Eu 4+、Lu 3+的总摩尔   数与BaTiO3摩尔数之比为5：100。 Composite single crystal fiber Eu 4+ /Lu 3+ : BaTiO 3 ; among them, the molar ratio of Eu 4+ and Lu 3+ is 12:1, and the ratio of the total number of moles of Eu 4+ and Lu 3+ to the number of moles of BaTiO3 is 5:100.
    上述复合单晶光纤及其制备方法，包括以下步骤：... The composite single crystal optical fiber and the preparation method thereof include the following steps:
    （1）在坩埚中部放置中部设有毛细管的晶体生长模具，将原料BaTiO 3、Eu 2O 3、Lu 2O 3置于坩埚中，加热坩埚使原料熔化形成熔体； (1) Place a crystal growth mold with a capillary in the middle of the crucible, place the raw materials BaTiO 3 , Eu 2 O 3 , and Lu 2 O 3 in the crucible, and heat the crucible to melt the raw materials to form a melt;
    （2）在模具顶部接籽晶提拉熔体，使籽晶在熔体的交界面上不断进行原子或分子重排，随降温逐渐凝固而生长出与模具边缘形状相同的单晶。... (2) The seed crystal is connected to the top of the mold to pull the melt, so that the seed crystal continuously rearranges atoms or molecules at the interface of the melt, and gradually solidifies as the temperature drops to grow a single crystal with the same shape as the edge of the mold.
    测试BaTiO 3、实施例1至3的复合单晶光纤Eu 4+/Lu 3+: BaTiO 3的吸收特性。 Test BaTiO 3, Examples 1 to the composite crystal of the optical fiber Eu 3 4+ / Lu 3+ embodiment: BaTiO 3 absorption characteristics.
    将样品制成直径1.0mm，长4mm的圆柱形光纤，两面经过仔细抛光后放到光纤耦合器中，以石英灯光源作为光源进行测量，测量光谱范围500-1000nm。结果显示，BaTiO 3、实施例1至3的复合单晶光纤Eu 4+/Lu 3+: BaTiO 3在650nm附近均具有明显的吸收峰，而且，实施例1的复合单晶光纤Eu 4+/Lu 3+: BaTiO 3在650nm附近的吸收峰最大，实施例2和3的复合单晶光纤Eu 4+/Lu 3+: BaTiO 3在650nm附近的吸收峰少小；证明：复合单晶光纤Eu 4+/Lu 3+: BaTiO 3具有比BaTiO 3更优异的吸收特性。 The sample is made into a cylindrical optical fiber with a diameter of 1.0mm and a length of 4mm. The two sides are carefully polished and placed in a fiber coupler. The quartz lamp is used as the light source for measurement. The measurement spectrum ranges from 500 to 1000 nm. The results show, BaTiO 3, to the composite in Example 1 Single Crystal Fiber Eu 3 embodiment 4+ / Lu 3+: BaTiO 3 have obvious absorption peak around 650nm, moreover, the single crystal in Example 1 embodiment the composite fiber Eu 4+ / Lu 3+ : BaTiO 3 has the largest absorption peak near 650nm, the composite single crystal fiber Eu 4+ /Lu 3+ : BaTiO 3 of Examples 2 and 3 has a small absorption peak near 650nm; it proves: composite single crystal fiber Eu 4+ /Lu 3+ : BaTiO 3 has better absorption characteristics than BaTiO 3.
       测试BaTiO 3、实施例1至3的复合单晶光纤Eu 4+/Lu 3+: BaTiO 3的上转换效率。 Conversion efficiency of BaTiO 3: Test BaTiO 3, 4+ / Lu 3+ Example 1 to a single crystal fiber composite of Eu 3.
       用650nm的半导体激光器作为泵浦光源，对样品泵浦，并测量个样品的上转换光谱。结果显示：BaTiO 3有上转换光谱，但强度非常弱；然而，但是实施例1至3的复合单晶光纤Eu 4+/Lu 3+: BaTiO 3上转换光谱强度比BaTiO 3明显增强很多。 A 650nm semiconductor laser was used as the pump light source to pump the sample and measure the up-conversion spectrum of each sample. The results show that BaTiO 3 has an up-conversion spectrum, but the intensity is very weak; however, the composite single crystal fiber Eu 4+ /Lu 3+ : BaTiO 3 of Examples 1 to 3 has an up-conversion spectrum that is much stronger than BaTiO 3 .
 To
       制备氧化铝-磷酸盐玻璃包层的钛酸钡单晶光纤。... Preparation of alumina-phosphate glass-clad barium titanate single crystal fiber.
实施例4 Example 4
       氧化铝-磷酸盐玻璃包层的钛酸钡单晶光纤，包括光纤纤芯以及包覆于光纤纤芯外的包层材料；所述包层材料为多组分磷酸盐玻璃，所述光纤纤芯材料为复合单晶光纤，所述复合单晶光纤为Eu 4+/Lu 3+: BaTiO 3。 Alumina-phosphate glass-clad barium titanate single crystal fiber includes an optical fiber core and a cladding material covering the fiber core; the cladding material is a multi-component phosphate glass, and the optical fiber is The core material is a composite single crystal fiber, and the composite single crystal fiber is Eu 4+ /Lu 3+ : BaTiO 3 .
       复合单晶光纤Eu 4+/Lu 3+: BaTiO 3；其中，Eu 4+、Lu 3+的摩尔比为12：1，Eu 4+、Lu 3+的总摩尔数与BaTiO3摩尔数之比为3：100。 Composite single crystal fiber Eu 4+ /Lu 3+ : BaTiO 3 ; among them, the molar ratio of Eu 4+ and Lu 3+ is 12:1, and the ratio of the total number of moles of Eu 4+ and Lu 3+ to the number of moles of BaTiO3 is 3:100.
    上述复合单晶光纤及其制备方法，利用晶体纤维及其包层同步制备设备制得，包括以下步骤：... The composite single crystal optical fiber and the preparation method thereof are prepared by the simultaneous preparation equipment of the crystal fiber and its cladding, including the following steps:
（1）在下坩埚内装入晶体光纤原料，在上坩埚内装入包层原料；加热下坩埚和上坩埚；所述晶体光纤原料为BaTiO3、Eu2O3、Lu2O3，所述包层原料为掺杂氧化铝和Er 3+的多组分磷酸盐玻璃，氧化铝的掺量为10重量份，Er 3+的掺量为1重量份，以重量份计；多组分磷酸盐玻璃组成为：P 2O 5：55重量份；K 2O：15重量份；BaO：7.5重量份；Al 2O 3：15重量份； (1) Fill the lower crucible with the raw material of the crystal fiber, and load the raw material for the cladding in the upper crucible; heat the lower crucible and the upper crucible; the raw materials of the crystal fiber are BaTiO3, Eu2O3, Lu2O3, and the cladding raw materials are doped alumina and Er 3+ multi-component phosphate glass, the content of alumina is 10 parts by weight, and the content of Er 3+ is 1 part by weight, based on parts by weight; the composition of the multi-component phosphate glass is: P 2 O 5 : 55 parts by weight; K 2 O: 15 parts by weight; BaO: 7.5 parts by weight; Al 2 O 3 : 15 parts by weight;
（2）待晶体光纤原料和包层原料融化后在包层柱顶部种籽晶，由于毛细管作用，下坩埚内的晶体光纤原料熔体通过晶体光纤供料成形管达到包层柱顶，籽晶先接触到晶体光纤供料成形管内的晶体光纤原料熔体，开始放肩；(2) After the crystal fiber raw material and the cladding material are melted, the seed crystal is seeded on the top of the cladding column. Due to the capillary action, the crystal fiber raw material melt in the lower crucible reaches the top of the cladding column through the crystal fiber supply forming tube. First touch the crystal fiber raw material melt in the crystal fiber supply forming tube, and begin to shoulder;
（3）晶体不断生长，由于毛细管作用，上坩埚内的包层原料熔体通过包层供料成形管达到包层柱顶，至晶体接触到包层供料成形管内的包层原料熔体，包层供料成形管内的包层原料熔体附着在光纤晶体外壁生长；从而光纤晶体和包层材料同步生长。(3) Crystals continue to grow. Due to capillary action, the cladding material melt in the upper crucible reaches the top of the cladding column through the cladding supply forming tube until the crystal contacts the cladding material melt in the cladding feeding forming tube. The cladding material melt in the cladding supply forming tube is attached to the outer wall of the fiber crystal to grow; thus the fiber crystal and the cladding material grow simultaneously.
实施例5Example 5
       氧化铝-磷酸盐玻璃包层的钛酸钡单晶光纤，包括光纤纤芯以及包覆于光纤纤芯外的包层材料；所述包层材料为多组分磷酸盐玻璃，所述光纤纤芯材料为复合单晶光纤，所述复合单晶光纤为Eu 4+/Lu 3+: BaTiO 3。 Alumina-phosphate glass-clad barium titanate single crystal fiber includes an optical fiber core and a cladding material covering the fiber core; the cladding material is a multi-component phosphate glass, and the optical fiber is The core material is a composite single crystal fiber, and the composite single crystal fiber is Eu 4+ /Lu 3+ : BaTiO 3 .
       复合单晶光纤Eu 4+/Lu 3+: BaTiO 3；其中，Eu 4+、Lu 3+的摩尔比为10：1，Eu 4+、Lu 3+的总摩尔数与BaTiO3摩尔数之比为1：100。 Composite single crystal fiber Eu 4+ /Lu 3+ : BaTiO 3 ; among them, the molar ratio of Eu 4+ and Lu 3+ is 10:1, and the ratio of the total number of moles of Eu 4+ and Lu 3+ to the number of moles of BaTiO3 is 1:100.
       上述复合单晶光纤及其制备方法，利用晶体纤维及其包层同步制备设备制得，包括以下步骤：... The composite single crystal optical fiber and the preparation method thereof are prepared by the simultaneous preparation equipment of the crystal fiber and its cladding, including the following steps:
（1）在下坩埚内装入晶体光纤原料，在上坩埚内装入包层原料；加热下坩埚和上坩埚；所述晶体光纤原料为BaTiO3、Eu2O3、Lu2O3，所述包层原料为掺杂氧化铝和Er 3+的多组分磷酸盐玻璃，氧化铝的掺量为5重量份，Er 3+的掺量为0.5重量份，以重量份计；多组分磷酸盐玻璃组成为：P 2O 5：45重量份；K 2O： 20重量份；BaO：10重量份；Al 2O 3：20重量份； (1) Fill the lower crucible with the raw material of the crystal fiber, and load the raw material for the cladding in the upper crucible; heat the lower crucible and the upper crucible; the raw materials of the crystal fiber are BaTiO3, Eu2O3, Lu2O3, and the cladding raw materials are doped alumina and Er 3+ multi-component phosphate glass, the content of alumina is 5 parts by weight, and the content of Er 3+ is 0.5 parts by weight, based on parts by weight; the composition of the multi-component phosphate glass is: P 2 O 5 : 45 parts by weight; K 2 O: 20 parts by weight; BaO: 10 parts by weight; Al 2 O 3 : 20 parts by weight;
（2）待晶体光纤原料和包层原料融化后在包层柱顶部种籽晶，由于毛细管作用，下坩埚内的晶体光纤原料熔体通过晶体光纤供料成形管达到包层柱顶，籽晶先接触到晶体光纤供料成形管内的晶体光纤原料熔体，开始放肩；(2) After the crystal fiber raw material and the cladding material are melted, the seed crystal is seeded on the top of the cladding column. Due to the capillary action, the crystal fiber raw material melt in the lower crucible reaches the top of the cladding column through the crystal fiber supply forming tube. First touch the crystal fiber raw material melt in the crystal fiber supply forming tube, and begin to shoulder;
（3）晶体不断生长，由于毛细管作用，上坩埚内的包层原料熔体通过包层供料成形管达到包层柱顶，至晶体接触到包层供料成形管内的包层原料熔体，包层供料成形管内的包层原料熔体附着在光纤晶体外壁生长；从而光纤晶体和包层材料同步生长。(3) Crystals continue to grow. Due to capillary action, the cladding material melt in the upper crucible reaches the top of the cladding column through the cladding supply forming tube until the crystal contacts the cladding material melt in the cladding feeding forming tube. The cladding material melt in the cladding supply forming tube is attached to the outer wall of the fiber crystal to grow; thus the fiber crystal and the cladding material grow simultaneously.
实施例6Example 6
       氧化铝-磷酸盐玻璃包层的钛酸钡单晶光纤，包括光纤纤芯以及包覆于光纤纤芯外的包层材料；所述包层材料为多组分磷酸盐玻璃，所述光纤纤芯材料为复合单晶光纤，所述复合单晶光纤为Eu 4+/Lu 3+: BaTiO 3。 Alumina-phosphate glass-clad barium titanate single crystal fiber includes an optical fiber core and a cladding material covering the fiber core; the cladding material is a multi-component phosphate glass, and the optical fiber is The core material is a composite single crystal fiber, and the composite single crystal fiber is Eu 4+ /Lu 3+ : BaTiO 3 .
       复合单晶光纤Eu 4+/Lu 3+: BaTiO 3；其中，Eu 4+、Lu 3+的摩尔比为10：1，Eu 4+、Lu 3+的总摩尔   数与BaTiO3摩尔数之比为5：100。 Composite single crystal fiber Eu 4+ /Lu 3+ : BaTiO 3 ; among them, the molar ratio of Eu 4+ and Lu 3+ is 10:1, and the ratio of the total number of moles of Eu 4+ and Lu 3+ to the number of moles of BaTiO3 is 5:100.
    上述复合单晶光纤及其制备方法，利用晶体纤维及其包层同步制备设备制得，包括以下步骤：... The composite single crystal optical fiber and the preparation method thereof are prepared by the simultaneous preparation equipment of the crystal fiber and its cladding, including the following steps:
（1）在下坩埚内装入晶体光纤原料，在上坩埚内装入包层原料；加热下坩埚和上坩埚；所述晶体光纤原料为BaTiO3、Eu2O3、Lu2O3，所述包层原料为掺杂氧化铝和Er3+的多组分磷酸盐玻璃，氧化铝的掺量为15重量份，Er 3+的掺量为1.5重量份，以重量份计；多组分磷酸盐玻璃组成为：P 2O 5：65重量份；K 2O：10重量份；BaO：5重量份；Al 2O 3：10重量份； (1) Fill the lower crucible with the raw material of the crystal fiber, and load the raw material for the cladding in the upper crucible; heat the lower crucible and the upper crucible; the raw materials of the crystal fiber are BaTiO3, Eu2O3, Lu2O3, and the cladding raw materials are doped alumina and Er3+ multi-component phosphate glass, the content of alumina is 15 parts by weight, and the content of Er 3+ is 1.5 parts by weight, based on parts by weight; the composition of the multi-component phosphate glass is: P 2 O 5 : 65 Parts by weight; K 2 O: 10 parts by weight; BaO: 5 parts by weight; Al 2 O 3 : 10 parts by weight;
（2）待晶体光纤原料和包层原料融化后在包层柱顶部种籽晶，由于毛细管作用，下坩埚内的晶体光纤原料熔体通过晶体光纤供料成形管达到包层柱顶，籽晶先接触到晶体光纤供料成形管内的晶体光纤原料熔体，开始放肩；(2) After the crystal fiber raw material and the cladding material are melted, the seed crystal is seeded on the top of the cladding column. Due to the capillary action, the crystal fiber raw material melt in the lower crucible reaches the top of the cladding column through the crystal fiber supply forming tube. First touch the crystal fiber raw material melt in the crystal fiber supply forming tube, and begin to shoulder;
（3）晶体不断生长，由于毛细管作用，上坩埚内的包层原料熔体通过包层供料成形管达到包层柱顶，至晶体接触到包层供料成形管内的包层原料熔体，包层供料成形管内的包层原料熔体附着在光纤晶体外壁生长；从而光纤晶体和包层材料同步生长。(3) Crystals continue to grow. Due to capillary action, the cladding material melt in the upper crucible reaches the top of the cladding column through the cladding supply forming tube until the crystal contacts the cladding material melt in the cladding feeding forming tube. The cladding material melt in the cladding supply forming tube is attached to the outer wall of the fiber crystal to grow; thus the fiber crystal and the cladding material grow simultaneously.

Claims (8)

  1. 一种氧化铝-磷酸盐玻璃包层的钛酸钡单晶光纤，其特征在于：包括光纤纤芯以及包覆于光纤纤芯外的包层材料；所述包层材料为掺杂氧化铝和Er 3+的多组分磷酸盐玻璃，所述光纤纤芯材料为复合单晶光纤，所述复合单晶光纤为Eu 4+/Lu 3+: BaTiO 3。 An alumina-phosphate glass-clad barium titanate single crystal optical fiber, which is characterized in that it comprises an optical fiber core and a cladding material covering the fiber core; the cladding material is doped alumina and Er 3+ multi-component phosphate glass, the fiber core material is a composite single crystal fiber, and the composite single crystal fiber is Eu 4+ /Lu 3+ : BaTiO 3 .
  2. 根据权利要求1所述的一种氧化铝-磷酸盐玻璃包层的钛酸钡单晶光纤，其特征在于：所述复合单晶光纤中，Eu 4+、Lu 3+的摩尔比为（8-12）：1。 The alumina-phosphate glass clad barium titanate single crystal fiber according to claim 1, characterized in that: in the composite single crystal fiber, the molar ratio of Eu 4+ to Lu 3+ is (8 -12): 1.
  3. 根据权利要求1所述的一种氧化铝-磷酸盐玻璃包层的钛酸钡单晶光纤，其特征在于：所述Eu 4+、Lu 3+的总摩尔数与BaTiO3摩尔数之比为（1-5）：100。 The alumina-phosphate glass-clad barium titanate single crystal fiber according to claim 1, wherein the ratio of the total number of moles of Eu 4+ and Lu 3+ to the number of moles of BaTiO3 is ( 1-5): 100.
  4. 根据权利要求1所述的一种氧化铝-磷酸盐玻璃包层的钛酸钡单晶光纤，其特征在于：所述多组分磷酸盐玻璃中，氧化铝的掺量为5-15重量份，Er 3+的掺量为0.5-1.5重量份，以重量份计。 The alumina-phosphate glass clad barium titanate single crystal fiber according to claim 1, wherein the content of alumina in the multi-component phosphate glass is 5-15 parts by weight , The content of Er 3+ is 0.5-1.5 parts by weight, based on parts by weight.
  5. 根据权利要求1所述的一种氧化铝-磷酸盐玻璃包层的钛酸钡单晶光纤，其特征在于：所述多组分磷酸盐玻璃组成为：P 2O 5：45~65重量份；K 2O：10~20重量份；BaO：5~10重量份；Al 2O 3：10~20重量份。 The alumina-phosphate glass clad barium titanate single crystal optical fiber according to claim 1, wherein the multi-component phosphate glass is composed of: P 2 O 5 : 45-65 parts by weight ; K 2 O: 10-20 parts by weight; BaO: 5-10 parts by weight; Al 2 O 3 : 10-20 parts by weight.
  6. 权利要求1所述的氧化铝-磷酸盐玻璃包层的钛酸钡单晶光纤的制备方法，其特征在于：利用晶体纤维及其包层同步制备设备制得，包括以下步骤：The method for preparing an alumina-phosphate glass-clad barium titanate single crystal optical fiber according to claim 1, characterized in that it is prepared by using a crystal fiber and its cladding synchronous preparation equipment, and comprises the following steps:
    在下坩埚内装入晶体光纤原料，在上坩埚内装入包层原料；加热下坩埚和上坩埚；Fill the lower crucible with crystal fiber raw materials, and load the upper crucible with cladding raw materials; heat the lower crucible and the upper crucible;
    待晶体光纤原料和包层原料融化后在包层柱顶部种籽晶，由于毛细管作用，下坩埚内的晶体光纤原料熔体通过晶体光纤供料成形管达到包层柱顶，籽晶先接触到晶体光纤供料成形管内的晶体光纤原料熔体，开始放肩；After the crystal fiber raw material and the cladding material are melted, the seed crystal is seeded on the top of the cladding column. Due to the capillary action, the crystal fiber raw material melt in the lower crucible reaches the top of the cladding column through the crystal fiber supply forming tube, and the seed crystal first touches The crystal fiber raw material melt in the crystal fiber feed forming tube begins to shoulder;
    晶体不断生长，由于毛细管作用，上坩埚内的包层原料熔体通过包层供料成形管达到包层柱顶，至晶体接触到包层供料成形管内的包层原料熔体，包层供料成形管内的包层原料熔体附着在光纤晶体外壁生长；从而光纤晶体和包层材料同步生长。Crystals continue to grow. Due to capillary action, the cladding material melt in the upper crucible reaches the top of the cladding column through the cladding supply forming tube, until the crystal contacts the cladding material melt in the cladding supply forming tube, and the cladding is supplied The cladding material melt in the material forming tube adheres to the outer wall of the fiber crystal to grow; thus, the fiber crystal and the cladding material grow simultaneously.
  7. 根据权利要求6所述的氧化铝-磷酸盐玻璃包层的钛酸钡单晶光纤的制备方法，其特征在于：步骤（1）中，所述晶体光纤原料为BaTiO 3、Eu 2O 3、Lu 2O 3。 The method for preparing alumina-phosphate glass-clad barium titanate single crystal fiber according to claim 6, characterized in that: in step (1), the raw material of the crystal fiber is BaTiO 3 , Eu 2 O 3 , Lu 2 O 3 .
  8. 根据权利要求6所述的氧化铝-磷酸盐玻璃包层的钛酸钡单晶光纤的制备方法，其特征在于：步骤（1）中，所述包层原料为掺杂氧化铝和Er 3+的多组分磷酸盐玻璃。 The method for preparing an alumina-phosphate glass-clad barium titanate single crystal fiber according to claim 6, characterized in that: in step (1), the cladding material is doped alumina and Er 3+ Of multi-component phosphate glass.
PCT/CN2019/115527 2019-11-05 2019-11-05 Barium titanate single crystal optical fiber clad in alumina-phosphate glass and preparation method therefor WO2021087712A1 (en)

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CA876763A (en) * 1971-07-27 Snitzer Elias Phosphate base laser glass
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US20140119692A1 (en) * 2012-11-01 2014-05-01 National Sun Yat-Sen University Optical fiber and method for manufacturing same
CN109186803A (en) * 2018-08-31 2019-01-11 南京同溧晶体材料研究院有限公司 A kind of high temperature resistant doped fiber temperature sensor
CN109238503A (en) * 2018-08-31 2019-01-18 南京同溧晶体材料研究院有限公司 A kind of high temperature resistant cladded-fiber temperature sensor
CN109269666A (en) * 2018-08-31 2019-01-25 南京同溧晶体材料研究院有限公司 A kind of cladded-fiber temperature sensor
CN109861066A (en) * 2019-01-31 2019-06-07 华南理工大学 A kind of 1.6 μm of powerful single-frequency lasers of high light beam quality

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA876763A (en) * 1971-07-27 Snitzer Elias Phosphate base laser glass
CN102033249A (en) * 2009-09-29 2011-04-27 中国科学院西安光学精密机械研究所 Compositions and preparation method of extra-large mode area metaphosphate optical fiber
US20140119692A1 (en) * 2012-11-01 2014-05-01 National Sun Yat-Sen University Optical fiber and method for manufacturing same
CN109186803A (en) * 2018-08-31 2019-01-11 南京同溧晶体材料研究院有限公司 A kind of high temperature resistant doped fiber temperature sensor
CN109238503A (en) * 2018-08-31 2019-01-18 南京同溧晶体材料研究院有限公司 A kind of high temperature resistant cladded-fiber temperature sensor
CN109269666A (en) * 2018-08-31 2019-01-25 南京同溧晶体材料研究院有限公司 A kind of cladded-fiber temperature sensor
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