CN1473782A - 用于碲酸盐玻璃包层的铅铋硅酸盐玻璃 - Google Patents
用于碲酸盐玻璃包层的铅铋硅酸盐玻璃 Download PDFInfo
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- 239000011521 glass Substances 0.000 title claims abstract description 71
- XHGGEBRKUWZHEK-UHFFFAOYSA-L tellurate Chemical compound [O-][Te]([O-])(=O)=O XHGGEBRKUWZHEK-UHFFFAOYSA-L 0.000 title claims abstract description 31
- 239000005368 silicate glass Substances 0.000 title claims abstract description 19
- 238000005253 cladding Methods 0.000 title abstract description 15
- DQUIAMCJEJUUJC-UHFFFAOYSA-N dibismuth;dioxido(oxo)silane Chemical compound [Bi+3].[Bi+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O DQUIAMCJEJUUJC-UHFFFAOYSA-N 0.000 title abstract 3
- 229910001420 alkaline earth metal ion Inorganic materials 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims description 11
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 4
- 229910052728 basic metal Inorganic materials 0.000 claims description 4
- 150000003818 basic metals Chemical group 0.000 claims description 4
- 239000011247 coating layer Substances 0.000 claims description 4
- 229910016036 BaF 2 Inorganic materials 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 2
- 239000013307 optical fiber Substances 0.000 abstract description 11
- 238000002425 crystallisation Methods 0.000 abstract description 6
- 230000008025 crystallization Effects 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 4
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- 229910001632 barium fluoride Inorganic materials 0.000 abstract description 2
- 229910052593 corundum Inorganic materials 0.000 abstract description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract 2
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 abstract 2
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 abstract 2
- 229910052783 alkali metal Inorganic materials 0.000 abstract 1
- 150000001340 alkali metals Chemical group 0.000 abstract 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract 1
- 230000007547 defect Effects 0.000 abstract 1
- FPHIOHCCQGUGKU-UHFFFAOYSA-L difluorolead Chemical compound F[Pb]F FPHIOHCCQGUGKU-UHFFFAOYSA-L 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- 239000011162 core material Substances 0.000 description 24
- 239000000463 material Substances 0.000 description 15
- 239000000835 fiber Substances 0.000 description 8
- 230000003321 amplification Effects 0.000 description 7
- -1 erbium ion Chemical class 0.000 description 7
- 238000003199 nucleic acid amplification method Methods 0.000 description 7
- 230000005540 biological transmission Effects 0.000 description 6
- 230000003287 optical effect Effects 0.000 description 6
- 239000000758 substrate Substances 0.000 description 6
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
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- 229910052761 rare earth metal Inorganic materials 0.000 description 3
- SITVSCPRJNYAGV-UHFFFAOYSA-L tellurite Chemical compound [O-][Te]([O-])=O SITVSCPRJNYAGV-UHFFFAOYSA-L 0.000 description 3
- 229910004261 CaF 2 Inorganic materials 0.000 description 2
- 229910052691 Erbium Inorganic materials 0.000 description 2
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- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001341 alkaline earth metal compounds Chemical class 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 238000004031 devitrification Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 150000002366 halogen compounds Chemical class 0.000 description 1
- 229910003439 heavy metal oxide Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
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- 229910052712 strontium Inorganic materials 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Abstract
一种用于碲酸盐玻璃包层的铅铋硅酸盐玻璃，由35～65mol％ SiO2、20～45mol％(PbO+Bi2O3)、0～10mol％BaF2(PbF2)、5～25mol％(R2O+MO)(R为碱金属，M为碱土金属离子)、0～10mol％Nb2O5(TiO2)和0～5mol％B2O3(Al2O3)组成。本发明的铅铋硅酸盐玻璃可有效克服碲酸盐玻璃析晶性能及其制造成本高等方面的不足，这对于碲酸盐玻璃光纤预制棒的制备以及玻璃光纤的成功拉制，具有重要的理论和实际意义。
Description
技术领域
本发明涉及硅酸盐玻璃，特别是一种适用于碲酸盐玻璃包层的铅铋硅酸盐玻璃。
背景技术
掺铒光纤放大器EDFA(Er3+Doped Fiber Amplifier)是光纤通讯系统中的重要部件，其原理是利用铒离子在1520-1560nm区域(即C波段)的发光实现光传输信号的放大，这种放大方式替代了传统的光/电/光放大方式，实现了信号光的低噪声和高增益放大。当前，随着计算机网络及其它数据传输业务的飞速发展，长距离传输系统对提高波分复用系统WDM(Wavelength Division Multiplexing)传输容量的需求日益增长。目前得到商业化的EDFA基本上都是以石英为基质的，这种石英基质的EDFA只能工作在C波段，为了增加WDM系统的传输容量，必须增加EDFA的放大带宽，使其放大波段由C波段向L波段(1570-1620nm)扩展。尽管许多物理的和机械的方法用于增加石英基质EDFA的放大带宽，但不能从根本上解决石英基质本身发射带宽的限制(参见在先技术Y.Ohishi，A.Mori，M.Yamada，et al.Gaincharacteristics of tellurite-based erbium doped fiber amplifiers for 1.5μm broadbandamplification，Optics Letters，vol.23，No.4：274-276)。除此之外，其它稀土离子如Tm3+、Pr3+掺杂的基质材料由于能够实现光信号在S波段(1470～1510nm)范围的放大也引起了很大的重视。为了实现高增益和宽带放大，寻找一种合适的用于稀土离子掺杂的基质材料，已是目前研究的热点。碲酸盐玻璃在光通讯窗口具有较大的受激发射截面和较宽的发射线宽FWHM(Full Width at Half Maximum)，被认为是增加WDM系统传输容量的较为吸引人的基质材料(参见在先技术U.S.Patent 5251062，公布日期为1993年10月5日，名称为TELLURITE GLASS AND FIBERAMPLIFIER)。目前报道的碲酸盐玻璃光纤放大器的芯和包层都是采用碲酸盐材料(参见在先技术U.S.Patent 6356387，公布日期为2002年3月12日，名称为TELLURITE GLASS，OPTICAL AMPLIFIER，AND LIGHT SOURCE)，这类材料存在以下两个方面的不足：一方面，碲酸盐玻璃析晶性能较差，光纤拉制过程中容易产生析晶现象，这使其很难实现优质光纤的成功拉制；另一方面，碲酸盐玻璃原料价格较贵，大约为2元/克，为了使碲酸盐玻璃光纤得到实际而又广泛的应用，尽可能的减少制造成本也是一种必要。由于光信号的放大在光纤纤芯内进行，而光纤内包层材料又占据了光纤的绝大部分体积(约占90％)，因此寻找一类合适的与碲酸盐玻璃性能匹配的价格较低的玻璃材料就可以大大降低制造成本。
发明内容
本发明要解决的技术问题在于克服上述现有技术的不足，提供一种适用于碲酸盐玻璃的包层玻璃，即铅铋硅酸盐玻璃。
本发明技术方案的依据是：作为包层的铅铋硅酸盐玻璃和作为芯料的碲酸盐玻璃在折射率、膨胀系数以及软化温度方面满足如下关系：(1)芯料折射率ncore与内包层玻璃折射率nclad之间关系为ncore＞nclad，并使光纤数值孔径NA(NA＝ncore 2-nclad 2)介于0.2与0.45之间；(2)芯料玻璃膨胀系数与内包层玻璃的膨胀系数之间以成丝后不产生内部压应力为准，一般情况下相差±20×10-7/℃，优选情况为内包层玻璃的膨胀系数稍低于芯层玻璃的膨胀系数；(3)芯料和内包层玻璃的软化温度相差±50℃以内，优选情况为内包层玻璃的软化温度稍大于芯料玻璃的软化温度。
本发明的技术解决方案如下：
一种用于碲酸盐玻璃包层的铅铋硅酸盐玻璃，其特征在于它的组成如下：
原料 成份范围(mol％)
SiO2 35～65
(PbO+Bi2O3) 20～45
BaF2 0～10
(R2O+MO) 5～25
Nb2O5 0～10
(B2O3+Al2O3 0～5
其中：R为碱金属，M为碱土金属离子。
根据本发明的目的，该玻璃是以SiO2为玻璃形成体的系统，其组成范围为35～65mol％。重金属氧化物PbO或Bi2O3或两者的组合体，其组成范围为20～45mol％。玻璃成分中还含有组成范围为5～25mol％的R2O+MO或其组合体，在成分中用以调整玻璃的稳定性、物理性质，以实现与芯料玻璃的性能匹配。0～10mol％的BaF2或CaF2或PbF2或其组合体加入到成分中，用来调整玻璃的膨胀系数、软化温度等。另外，成分中还含有0～10mol％的Nb2O5或WO3或TiO2或其组合体，用于调整玻璃的折射率。0～5mol％的B2O3或Al2O3或其组合体用来提高玻璃的抗析晶性能。该玻璃系统具有较好的析晶稳定性和化学稳定性，并且可以实现与芯料碲酸盐玻璃性能的匹配。
为了尽可能减少玻璃原料中的杂质引起的损耗，玻璃制备所需原料均为高纯级(＞99.9％)。玻璃熔制过程如下：首先以常规方法按照一定的配比称取一定的混合料。碱金属和碱土金属以碳酸盐的形式引入，其它组份均以所述形式加入。混合料充分搅拌均匀，然后放入石英或刚玉坩锅内，将坩锅放入800～1200℃的硅碳棒电炉中进行熔制，熔制时间为30～60分钟。然后将制成的玻璃熔融液倒入事先预热的铁模上，待冷却后将玻璃在其转变温度附近退火至室温。
本发明实现的铅铋硅酸盐玻璃可有效克服碲酸盐玻璃析晶性能及其制造成本高等方面的不足，这对于碲酸盐玻璃光纤预制棒的制备以及玻璃光纤的成功拉制，具有重要的理论和实际意义。
附图说明
图1为铅铋硅酸盐玻璃包层材料和碲酸盐玻璃芯料材料粘度曲线的比较。
具体实施方式
本发明铅铋硅酸盐玻璃的10个具体实施例如表1所示。表中示出了相应玻璃的软化温度、折射率、热膨胀系数等性能参数，所述组成均表示为mol％。玻璃成分可以根据这些性能参数进行成分上的修改，以便实现与纤芯玻璃的组合。0～10mol％的BaF2可以被以下不易潮解的任选卤素化合物XY2(X＝Ca，Mg，Pb，Sr；Y＝F，Cl，Br)或它们的组合体替代。对玻璃进行组成上修改的条件是：(1)芯料折射率ncore与内包层玻璃折射率nclad之间关系为：ncore＞nclad，并使光纤数值孔径NA(NA＝ncore 2-nclad 2)介于0.2与0.45之间；(2)芯料玻璃膨胀系数与内包层玻璃的膨胀系数之间以成丝后不产生内部压应力为准，一般情况下相差±20×10-7/℃，优选情况为内包层玻璃的膨胀系数稍低于芯层玻璃的膨胀系数，这样可以保证纤芯和包层的紧密接触，增加光纤的强度；(3)芯料和内包层材料的软化温度相差±50℃以内，优选情况为内包层材料的软化温度稍大于芯料材料的软化温度。
表1组份
1 2 3 4 5 6 7 8 9 10(mol％)SiO2 60 55 50 55 37.5 37.5 37.5 65 35 40PbO 0 0 0 40 37.5 37.5 37.5 0 35 15Bi2O3 35 35 35 0 0 0 0 20 10 12.5Na2O 5 5 5 5 25 10 10 0 5 15K2O 0 0 0 0 0 0 0 5 5 10CaO 0 0 0 0 0 15 0 0 5 0BaO 0 0 0 0 0 0 15 0 5 0BaF2 0 5 10 0 0 0 0 0 0 0Nb2O5 0 0 0 0 0 0 0 10 0 2.5B2O3 0 0 0 0 0 0 0 0 5 2.5Al2O3 0 0 0 0 0 0 0 0 0 2.5膨胀系数
105 121 130 105 161 124 130 135 132 145(10-7/℃)软化温度
482 411 388 464 369 435 426 450 399 413(℃)折射率nd1.972 1.971 1.968 1.868 1.809 1.864 1.818 1.782 1.956 1.911
以上所述的用作芯料的碲酸盐玻璃基本由50～75mol％的TeO2、15～25mol％的ZnO和0～15mol％的La2O3组成。稀土离子如Er3+、Tm3+、Pr3+、Nd3+等在碲酸盐玻璃中的掺杂浓度为0～2mol％，以高纯氧化物的形式引入。另外，根据实验要求可加入0～3mol％的Yb2O3到玻璃成分中用来增加泵浦光的吸收效率。实验测得摩尔组成为70TeO2+25ZnO+5La2O3的玻璃的热膨胀系数、软化温度以及折射率分别为151×10-7/℃、392℃和2.038。根据碲酸盐玻璃的性能参数，得到两组实用铅铋硅酸盐玻璃配方，其膨胀系数、软化温度以及折射率分别为150×10-7/℃、413℃及1.911和132×10-7/℃、399℃及1.956。此外，碲酸盐玻璃的这些性能参数可以在一定范围内变化，作为包层材料的铅铋硅酸盐玻璃也可以通过玻璃成分的优化，实现与碲酸盐玻璃性能的匹配。为了调整碲酸盐玻璃的化学稳定性和物理性能，玻璃中可加入0～10mol％的碱金属或碱土金属化合物或它们的组合体，这些化合物包括Li2O，Na2O，K2O，LiF，NaF，KF，MgO，CaO，SrO，BaO，MgF2，CaF2，SrF2，BaF2。0～15mol％的GeO2或Nb2O5或WO3或PbO或PbF2或Al2O3或它们的组合体等加入成分中用来增加玻璃的声子能量、提高玻璃的析晶性能、降低玻璃的折射率等。
图1所示为芯料碲酸盐玻璃和内包层铅铋硅酸盐玻璃粘度曲线的比较。所用碲酸盐玻璃和铅铋硅酸盐玻璃的成分分别为摩尔组成的70TeO2+25ZnO+5La2O3+0.1Er2O3和40SiO2+12.5PbO+22.5Bi2O3+10Na2O+5K2O+5BaO+5Nb2O5。可以看出这两种成分在105～107Poise的粘度区域内能够很好的匹配，这一区域是碲酸盐玻璃光纤形成的区域。另外，由表1的数据，铅硅酸盐玻璃的热膨胀系数、软化温度以及折射率等通过成分的调整可以在一定的范围内变化，说明本发明提供的铅硅酸盐玻璃可以满足一系列碲酸盐玻璃的包层材料。
Claims (1)
1、一种用于碲酸盐玻璃包层的铅铋硅酸盐玻璃，其特征在于它的组成如下：
原料 成份范围(mol％)
SiO2 35～65
PbO+Bi2O3 20～45
BaF2+PbF2 0～10
R2O+MO 5～25
Nb2O5+TiO2 0～10
B2O3+Al2O3 0～5
其中：R为碱金属，M为碱土金属离子。
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1298650C (zh) * | 2005-03-18 | 2007-02-07 | 中国科学院上海光学精密机械研究所 | 纳米铋团簇掺杂二氧化硅基光学玻璃及其制备方法 |
| CN101609181B (zh) * | 2009-07-17 | 2011-02-09 | 暨南大学 | 一种低损耗碲酸盐玻璃平面光波导的制作方法 |
| CN102775063A (zh) * | 2012-08-22 | 2012-11-14 | 中国科学院上海硅酸盐研究所 | 含铅氟氧化物闪烁玻璃及其制备方法 |
| CN103771717A (zh) * | 2014-01-23 | 2014-05-07 | 中国科学院上海光学精密机械研究所 | 碲酸盐玻璃复合光纤的制备方法 |
| CN109143459A (zh) * | 2018-09-04 | 2019-01-04 | 同济大学 | 一种稀土离子掺杂的低温石榴石晶棒的包层方法 |
| CN109574509A (zh) * | 2018-12-20 | 2019-04-05 | 山东海富光子科技股份有限公司 | 2至5微米波段内的低损耗高强度全玻璃光纤及制备方法 |
| CN109970347A (zh) * | 2019-04-29 | 2019-07-05 | 齐鲁工业大学 | 一种提高锂离子电池性能的TeO2-V2O5-CuO微晶玻璃负极材料 |
| CN112374749A (zh) * | 2020-11-20 | 2021-02-19 | 长春理工大学 | 一种铋硼铝可调谐的激光玻璃及其制备方法 |
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| CN1298650C (zh) * | 2005-03-18 | 2007-02-07 | 中国科学院上海光学精密机械研究所 | 纳米铋团簇掺杂二氧化硅基光学玻璃及其制备方法 |
| CN101609181B (zh) * | 2009-07-17 | 2011-02-09 | 暨南大学 | 一种低损耗碲酸盐玻璃平面光波导的制作方法 |
| CN102775063A (zh) * | 2012-08-22 | 2012-11-14 | 中国科学院上海硅酸盐研究所 | 含铅氟氧化物闪烁玻璃及其制备方法 |
| CN103771717A (zh) * | 2014-01-23 | 2014-05-07 | 中国科学院上海光学精密机械研究所 | 碲酸盐玻璃复合光纤的制备方法 |
| CN103771717B (zh) * | 2014-01-23 | 2016-02-10 | 中国科学院上海光学精密机械研究所 | 碲酸盐玻璃复合光纤的制备方法 |
| CN109143459A (zh) * | 2018-09-04 | 2019-01-04 | 同济大学 | 一种稀土离子掺杂的低温石榴石晶棒的包层方法 |
| CN109574509A (zh) * | 2018-12-20 | 2019-04-05 | 山东海富光子科技股份有限公司 | 2至5微米波段内的低损耗高强度全玻璃光纤及制备方法 |
| CN109574509B (zh) * | 2018-12-20 | 2021-08-10 | 山东海富光子科技股份有限公司 | 2至5微米波段内的低损耗高强度全玻璃光纤及制备方法 |
| CN109970347A (zh) * | 2019-04-29 | 2019-07-05 | 齐鲁工业大学 | 一种提高锂离子电池性能的TeO2-V2O5-CuO微晶玻璃负极材料 |
| CN112374749A (zh) * | 2020-11-20 | 2021-02-19 | 长春理工大学 | 一种铋硼铝可调谐的激光玻璃及其制备方法 |
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