CN114634311A - Method for improving near-infrared fluorescence intensity of bismuth-doped quartz glass - Google Patents
Method for improving near-infrared fluorescence intensity of bismuth-doped quartz glass Download PDFInfo
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 77
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- 238000010438 heat treatment Methods 0.000 claims abstract description 22
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- 239000000110 cooling liquid Substances 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000001307 helium Substances 0.000 claims abstract description 5
- 229910052734 helium Inorganic materials 0.000 claims abstract description 5
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 4
- 235000011089 carbon dioxide Nutrition 0.000 claims abstract description 4
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 4
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- 238000010791 quenching Methods 0.000 claims description 27
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- 238000001035 drying Methods 0.000 claims description 3
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- 239000001257 hydrogen Substances 0.000 claims 1
- 229910052739 hydrogen Inorganic materials 0.000 claims 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 239000011521 glass Substances 0.000 abstract description 17
- 239000000835 fiber Substances 0.000 abstract description 7
- 230000003287 optical effect Effects 0.000 abstract description 6
- 229910052797 bismuth Inorganic materials 0.000 abstract description 5
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- 230000002708 enhancing effect Effects 0.000 abstract description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 14
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- 238000002844 melting Methods 0.000 description 2
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- 230000001737 promoting effect Effects 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
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- 229910001451 bismuth ion Inorganic materials 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
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Abstract
一种提高铋掺杂石英玻璃的近红外荧光强度的方法，包括以下步骤：将铋掺杂石英玻璃经高温热处理加热至1600‑1700℃的熔融状态，并保温1‑10min；将熔融物迅速放入不同的冷却液体中，并完全浸泡，进行急冷淬火；然后取出，将淬火后的玻璃抛光，得到荧光增强的铋掺杂石英玻璃。所述高温热源包括石墨炉和氢氧焰。所述冷却液体包括去离子水，干冰、液氮以及液氦等。该方法有利于提高掺Bi石英玻璃中铋相关活性中心的浓度，从而增强铋掺杂石英玻璃载近红外波段的荧光强度。这作为掺Bi光纤激光器及光放大器的增益介质具有广泛的应用。
A method for improving the near-infrared fluorescence intensity of bismuth-doped quartz glass, comprising the following steps: heating the bismuth-doped quartz glass to a molten state of 1600-1700° C. through high-temperature heat treatment, and keeping the temperature for 1-10 minutes; into different cooling liquids, immersed completely, and quenched and quenched; then taken out, and polished the quenched glass to obtain fluorescence-enhanced bismuth-doped quartz glass. The high temperature heat source includes a graphite furnace and a hydrogen-oxygen flame. The cooling liquid includes deionized water, dry ice, liquid nitrogen, and liquid helium. The method is beneficial to increase the concentration of bismuth-related active centers in the Bi-doped quartz glass, thereby enhancing the fluorescence intensity of the bismuth-doped quartz glass in the near-infrared band. This has a wide range of applications as a gain medium for Bi-doped fiber lasers and optical amplifiers.
Description
技术领域technical field
本发明属于石英玻璃技术领域，具体的涉及一种通过急冷淬火增加铋相关活性中心的浓度，提高铋掺杂石英玻璃的近红外荧光强度的方法。The invention belongs to the technical field of quartz glass, and in particular relates to a method for increasing the concentration of bismuth-related active centers and increasing the near-infrared fluorescence intensity of bismuth-doped quartz glass by quenching and quenching.
背景技术Background technique
稀土掺杂(主要是Yb3+，Nd3+，Pr3+，Er3+和Tm3+等)的石英光纤在近红外区域是非常有效的活性介质，被广泛应用于光纤放大器等领域。但是在整个光通信波段仍存在光谱空隙。掺Bi玻璃近红外荧光可以覆盖1000-1700nm，其荧光半高宽超过了300nm，在实现高效率宽带光纤放大器方面有潜在的优势。自2005年俄罗斯科学家首次在掺Bi光纤中实现了激光和放大输出以来，掺Bi石英光纤受到科研人员高度关注。采用掺Bi光纤实现1100-1700nm波段的超宽带放大将极大拓展光通信的带宽，从而提高光通信容量。Rare earth doped silica fibers (mainly Yb 3+ , Nd 3+ , Pr 3+ , Er 3+ and Tm 3+ , etc.) are very effective active media in the near-infrared region and are widely used in fiber amplifiers and other fields. However, spectral gaps still exist in the entire optical communication band. The near-infrared fluorescence of Bi-doped glass can cover 1000-1700 nm, and its fluorescence full width at half maximum exceeds 300 nm, which has potential advantages in realizing high-efficiency broadband fiber amplifiers. Since 2005, when Russian scientists first realized laser and amplifying output in Bi-doped fiber, Bi-doped silica fiber has attracted great attention from researchers. The use of Bi-doped fiber to achieve ultra-wideband amplification in the 1100-1700 nm band will greatly expand the bandwidth of optical communication, thereby increasing the optical communication capacity.
另一方面，虽然目前铋掺杂石英玻璃的荧光带宽比较宽，但是发光效率低，荧光强度弱，荧光峰形不平坦等问题限制了铋相关的超宽带光放大器以及超宽带光源方面等应用。On the other hand, although the fluorescence bandwidth of bismuth-doped quartz glass is relatively wide, the problems of low luminous efficiency, weak fluorescence intensity, and uneven fluorescence peak shape limit the application of bismuth-related ultra-broadband optical amplifiers and ultra-broadband light sources.
发明内容SUMMARY OF THE INVENTION
为解决上述技术问题，本发明的目的是提供一种提高铋掺杂石英玻璃的近红外荧光强度的方法，通过淬火调控铋掺杂石英玻璃光谱性质，对铋掺杂石英玻璃进行高温热处理至熔融状态后，再将熔融态的玻璃迅速放入冷却液中进行淬火处理。调节铋离子近红外活性中心的种类和比例，从而提高所覆盖光通讯波段的宽度，获得平坦的宽带近红外发光。In order to solve the above-mentioned technical problems, the purpose of the present invention is to provide a method for improving the near-infrared fluorescence intensity of bismuth-doped quartz glass, regulating the spectral properties of bismuth-doped quartz glass by quenching, and performing high temperature heat treatment on the bismuth-doped quartz glass until melting. After the state, the molten glass is quickly put into the cooling liquid for quenching treatment. The types and proportions of near-infrared active centers of bismuth ions are adjusted, thereby increasing the width of the covered optical communication band and obtaining flat broadband near-infrared luminescence.
为实现上述目的，本发明采用的技术方案为：To achieve the above object, the technical scheme adopted in the present invention is:
一种提高铋掺杂石英玻璃的近红外荧光强度的方法，其特点在于，包括以下步骤：A method for improving the near-infrared fluorescence intensity of bismuth-doped quartz glass, which is characterized by comprising the following steps:
(1)对铋掺杂石英玻璃表面进行清洁后，加热至熔融状态；(1) after cleaning the surface of the bismuth-doped quartz glass, heating to a molten state;
(2)将处于熔融状态的铋掺杂石英玻璃置于冷却液中急冷淬火；(2) placing the bismuth-doped quartz glass in the molten state in a cooling liquid for rapid cooling and quenching;
(3)将淬火后的铋掺杂石英玻璃取出，抛光、清洗烘干。(3) taking out the quenched bismuth-doped quartz glass, polishing, cleaning and drying.
优选的，步骤一：将制备好的掺Bi玻璃进行表面清洁，以防止熔融过程中杂质的引入；Preferably, step 1: the surface of the prepared Bi-doped glass is cleaned to prevent the introduction of impurities during the melting process;
优选的，步骤二：将玻璃片通过氢氧焰熔接在纯石英棒端面，并将其置于石墨炉或氢氧焰机床上旋转加热5分钟。Preferably, step 2: the glass sheet is welded on the end face of the pure quartz rod through an oxyhydrogen flame, and it is placed in a graphite furnace or an oxyhydrogen flame machine tool for rotary heating for 5 minutes.
优选的，步骤三：将经热处理后，处于1600-1800℃的熔融状态的铋掺杂石英玻璃迅速置于冷却液中。Preferably, step 3: the bismuth-doped quartz glass in a molten state of 1600-1800° C. after heat treatment is rapidly placed in a cooling liquid.
优选的，步骤四：将冷却后的玻璃取出，进行切割、双面抛光以及清洗烘干。Preferably, step 4: take out the cooled glass, perform cutting, double-sided polishing, cleaning and drying.
所述铋掺杂石英玻璃在加热至1600-1800℃的的熔融态时，再继续保温1-10分钟。When the bismuth-doped quartz glass is heated to a molten state of 1600-1800° C., the temperature is continued for 1-10 minutes.
所述冷却液包括但不限于去离子水、干冰、液氮和液氦等。The cooling liquid includes, but is not limited to, deionized water, dry ice, liquid nitrogen, liquid helium, and the like.
优选的，所述热处理源为H2/O2＝(1-4)的氢氧焰。Preferably, the heat treatment source is an oxyhydrogen flame with H 2 /O 2 =(1-4).
优选的，所述冷却液为液氦。Preferably, the cooling liquid is liquid helium.
与现有技术相比，本发明的有益效果：Compared with the prior art, the beneficial effects of the present invention:
1)通过在熔融温度快冷淬火，导致玻璃的假想温度增加，内部结构混乱度增加，非对称性增加，从而促进了Bi相关活性中心种类的增加。有利于提高掺Bi石英玻璃中铋相关活性中心的浓度，从而增强铋掺杂石英玻璃载近红外波段的荧光强度1) Through rapid cooling and quenching at the melting temperature, the fictive temperature of the glass increases, the internal structure disorder increases, and the asymmetry increases, thereby promoting the increase of Bi-related active center species. It is beneficial to increase the concentration of bismuth-related active centers in Bi-doped silica glass, thereby enhancing the fluorescence intensity in the near-infrared band of bismuth-doped silica glass.
2)高温氢氧焰加热时，提供了还原环境，有利于Bi的还原从而产生低价Bi，增加Bi活性中心数量，促进近红外发光。2) When heated by a high-temperature hydrogen-oxygen flame, a reducing environment is provided, which is beneficial to the reduction of Bi to generate low-priced Bi, increase the number of Bi active centers, and promote near-infrared luminescence.
3)本发明通过低含量铋掺杂，避免了高Bi含量掺杂而导致的在热处理及淬火过程中易产生玻璃变暗、透过率下降以及发光猝灭等现象。3) The present invention avoids the phenomenon of glass darkening, transmittance decrease and luminescence quenching, which are easily caused by high Bi content doping in the process of heat treatment and quenching by doping with low content of Bi.
4)快冷淬火后的铋掺杂石英玻璃可覆盖的宽带吸收峰，在500nm激发下，与原始未淬火玻璃相比，其荧光主峰由1170nm红移至1402nm，荧光半高宽可达356nm，大幅增加了其能够覆盖的通讯波长范围。4) The broadband absorption peak of the bismuth-doped quartz glass after rapid cooling and quenching can be covered. Under the excitation of 500nm, compared with the original unquenched glass, its fluorescence main peak is red-shifted from 1170nm to 1402nm, and the fluorescence half-height width can reach 356nm. It greatly increases the communication wavelength range that it can cover.
附图说明Description of drawings
图1是本发明Bi/P共掺石英玻璃急冷淬火前后的吸收光谱对比图。FIG. 1 is a comparison diagram of the absorption spectra of the Bi/P co-doped quartz glass of the present invention before and after quenching.
图2是本发明Bi/P共掺石英玻璃急冷淬火前后的荧光强度对比图。FIG. 2 is a comparison diagram of the fluorescence intensity of the Bi/P co-doped quartz glass of the present invention before and after quenching.
图3是本发明Bi/P共掺石英玻璃在不同加热方式下在1400nm附近的荧光强度对比折线图。FIG. 3 is a graph showing the comparison of fluorescence intensity near 1400 nm of the Bi/P co-doped quartz glass of the present invention under different heating modes.
图4是本发明Bi/P共掺石英玻璃在不同急冷淬火液中在1400nm附近的荧光强度对比折线图。Fig. 4 is a graph showing the comparison of fluorescence intensity of the Bi/P co-doped quartz glass of the present invention in the vicinity of 1400 nm in different quenching solutions.
具体实施方式Detailed ways
为了进一步了解本发明的特征、技术手段以及所达到的目的、功能。下面结合附图进一步描述本发明的具体实施例，但要求保护的范围并不局限于此In order to further understand the features, technical means, achieved goals and functions of the present invention. The specific embodiments of the present invention are further described below in conjunction with the accompanying drawings, but the scope of protection is not limited to this
实施例1：(参见图1、图2、图3和表1)Example 1: (See Figure 1, Figure 2, Figure 3 and Table 1)
本实施例Bi/P共掺石英玻璃的成份(摩尔百分比)为：0.1Bi2O3-10P2O5-89.9SiO2。The composition (molar percentage) of the Bi/P co-doped quartz glass in this embodiment is: 0.1Bi 2 O 3 -10P 2 O 5 -89.9SiO 2 .
Bi/P共掺杂石英玻璃的淬火过程包括：The quenching process of Bi/P co-doped quartz glass includes:
(1)先用丙酮或者酒精清洗玻璃表面，避免高温热处理时导致杂质的引入；(1) Clean the glass surface with acetone or alcohol first to avoid the introduction of impurities during high temperature heat treatment;
(2)将铋掺杂石英玻璃熔接在纯石英玻璃管一侧的端面上。经H2/O2＝1的氢氧焰加热至1600-1800℃的熔融状态；(2) The bismuth-doped quartz glass is welded on the end face of one side of the pure quartz glass tube. It is heated to a molten state of 1600-1800 ℃ by a hydrogen-oxygen flame with H 2 /O 2 =1;
(3)将处于熔融状态的掺铋石英玻璃迅速置于25℃的去离子水中并完全浸泡，进行快速淬火处理；(3) The bismuth-doped quartz glass in the molten state is rapidly placed in deionized water at 25°C and completely soaked, and then rapidly quenched;
(4)将淬火后的样品取出，加工成预定尺寸，双面抛光，然后清洗烘干。(4) The quenched sample is taken out, processed into a predetermined size, polished on both sides, and then cleaned and dried.
测试结果如图1和图2所示。显著区别在于，淬火后的BiP共掺石英玻璃在430nm的吸收显著增强。并在820以及1400nm附近出现了硅相关的铋活性中心吸收峰。采用氙灯以500nm进行激发，经淬火后的掺Bi/P共掺石英玻璃的发光主峰由1170nm红移至1402nm，半高宽由254增加至356nm。发射带可覆盖1000-1700nm。The test results are shown in Figure 1 and Figure 2. The notable difference is that the absorption at 430 nm of the quenched BiP co-doped silica glass is significantly enhanced. The silicon-related bismuth active center absorption peaks appeared around 820 and 1400 nm. Xenon lamp was used to excite at 500nm, and the main luminescence peak of the quenched Bi/P co-doped quartz glass was red-shifted from 1170nm to 1402nm, and the full width at half maximum increased from 254 to 356nm. The emission band can cover 1000-1700nm.
实施例2：(参见图1、图2、图3和表1)Example 2: (See Figure 1, Figure 2, Figure 3 and Table 1)
本实施例Bi/P共掺石英玻璃的成份(摩尔百分比)为：0.1Bi2O3-10P2O5-89.9SiO2。The composition (molar percentage) of the Bi/P co-doped quartz glass in this embodiment is: 0.1Bi 2 O 3 -10P 2 O 5 -89.9SiO 2 .
Bi/P共掺杂石英玻璃的淬火过程包括：The quenching process of Bi/P co-doped quartz glass includes:
(1)先用丙酮或者酒精清洗玻璃表面，避免高温热处理时导致杂质的引入；(1) Clean the glass surface with acetone or alcohol first to avoid the introduction of impurities during high temperature heat treatment;
(2)将铋掺杂石英玻璃熔接在纯石英玻璃管一侧的端面上。经石墨炉加热至16001800℃的熔融状态；(2) The bismuth-doped quartz glass is welded on the end face of one side of the pure quartz glass tube. It is heated to a molten state of 1600-1800 ℃ by a graphite furnace;
(3)将处于熔融状态的掺铋石英玻璃迅速置于25℃的去离子水中并完全浸泡，进行快速淬火处理；(3) The bismuth-doped quartz glass in the molten state is rapidly placed in deionized water at 25°C and completely soaked, and then rapidly quenched;
(4)将淬火后的样品取出，加工成预定尺寸，双面抛光，然后清洗烘干(4) Take out the quenched sample, process it into a predetermined size, polish both sides, and then clean and dry
实施例3：(参见图1、图2、图3和表1)Example 3: (see Figure 1, Figure 2, Figure 3 and Table 1)
本实施例Bi/P共掺石英玻璃的成份(摩尔百分比)为：0.1Bi2O3-10P2O-589.9SiO2。The composition (molar percentage) of the Bi/P co-doped quartz glass in this embodiment is: 0.1Bi 2 O 3 -10P 2 O- 5 89.9SiO 2 .
Bi/P共掺杂石英玻璃的淬火过程包括：The quenching process of Bi/P co-doped quartz glass includes:
(1)先用丙酮或者酒精清洗玻璃表面，避免高温热处理时导致杂质的引入；(1) Clean the glass surface with acetone or alcohol first to avoid the introduction of impurities during high temperature heat treatment;
(2)将铋掺杂石英玻璃熔接在纯石英玻璃管一侧的端面上。经H2/O2＝2的氢氧焰加热至1600-1800℃的熔融状态；(2) The bismuth-doped quartz glass is welded on the end face of one side of the pure quartz glass tube. It is heated to a molten state of 1600-1800 ℃ by a hydrogen-oxygen flame with H 2 /O 2 =2;
(3)将处于熔融状态的掺铋石英玻璃迅速置于25℃的去离子水中并完全浸泡，进行快速淬火处理；(3) The bismuth-doped quartz glass in the molten state is rapidly placed in deionized water at 25°C and completely soaked, and then rapidly quenched;
(4)将淬火后的样品取出，加工成预定尺寸，双面抛光，然后清洗烘干(4) Take out the quenched sample, process it into a predetermined size, polish both sides, and then clean and dry
实施例4：(参见图1、图2、图3和表1)Example 4: (See Figure 1, Figure 2, Figure 3 and Table 1)
本实施例Bi/P共掺石英玻璃的成份(摩尔百分比)为：0.1Bi2O3-10P2O5-89.9SiO2。The composition (molar percentage) of the Bi/P co-doped quartz glass in this embodiment is: 0.1Bi 2 O 3 -10P 2 O 5 -89.9SiO 2 .
Bi/P共掺杂石英玻璃的淬火过程包括：The quenching process of Bi/P co-doped quartz glass includes:
(1)先用丙酮或者酒精清洗玻璃表面，避免高温热处理时导致杂质的引入；(1) Clean the glass surface with acetone or alcohol first to avoid the introduction of impurities during high temperature heat treatment;
(2)将铋掺杂石英玻璃熔接在纯石英玻璃管一侧的端面上。经H2/O2＝4的氢氧焰加热至1600-1800℃的熔融状态；(2) The bismuth-doped quartz glass is welded on the end face of one side of the pure quartz glass tube. It is heated to a molten state of 1600-1800 ° C by a hydrogen-oxygen flame with H 2 /O 2 =4;
(3)将处于熔融状态的掺铋石英玻璃迅速置于25℃的去离子水中并完全浸泡，进行快速淬火处理；(3) The bismuth-doped quartz glass in the molten state is rapidly placed in deionized water at 25°C and completely soaked, and then rapidly quenched;
(4)将淬火后的样品取出，加工成预定尺寸，双面抛光，然后清洗烘干(4) Take out the quenched sample, process it into a predetermined size, polish both sides, and then clean and dry
不同加热方式下淬火得到的玻璃荧光谱归一化结果如图3。显著区别在于氢氧焰促进了Bi的还原从而产生低价Bi，从而促进Bi活性中心数量的增加，促进近红外荧光强度的增加。但是过度还原会导致Bi透过率下降以及发光猝灭簇的产生，导致荧光强度的下降。The normalized results of the fluorescence spectra of the glass quenched under different heating methods are shown in Figure 3. The significant difference is that the oxyhydrogen flame promotes the reduction of Bi to generate low-valent Bi, thereby promoting the increase of the number of Bi active centers and the increase of the near-infrared fluorescence intensity. However, excessive reduction will lead to the decrease of Bi transmittance and the generation of luminescence quenching clusters, resulting in the decrease of fluorescence intensity.
实施例5：(参见图4和表1)Example 5: (see Figure 4 and Table 1)
本实施例Bi/P共掺石英玻璃的成份(摩尔百分比)为：0.1Bi2O3-10P2O5-89.9SiO2。The composition (molar percentage) of the Bi/P co-doped quartz glass in this embodiment is: 0.1Bi 2 O 3 -10P 2 O 5 -89.9SiO 2 .
Bi/P共掺杂石英玻璃的淬火过程包括：The quenching process of Bi/P co-doped quartz glass includes:
(1)先用丙酮或者酒精清洗玻璃表面，避免高温热处理时导致杂质的引入；(1) Clean the glass surface with acetone or alcohol first to avoid the introduction of impurities during high temperature heat treatment;
(2)将铋掺杂石英玻璃熔接在纯石英玻璃管一侧的端面上。经H2/O2＝2的氢氧焰加热至1600-1800℃的熔融状态；(2) The bismuth-doped quartz glass is welded on the end face of one side of the pure quartz glass tube. It is heated to a molten state of 1600-1800 ℃ by a hydrogen-oxygen flame with H 2 /O 2 =2;
(3)将处于熔融状态的掺铋石英玻璃迅速置于干冰中并完全浸泡，进行快速淬火处理；(3) quickly place the bismuth-doped quartz glass in the molten state in dry ice and soak it completely, and carry out rapid quenching treatment;
(4)将淬火后的样品取出，加工成预定尺寸，双面抛光，然后清洗烘干(4) Take out the quenched sample, process it into a predetermined size, polish both sides, and then clean and dry
实施例6：(参见图4和表1)Example 6: (see Figure 4 and Table 1)
本实施例Bi/P共掺石英玻璃的成份(摩尔百分比)为：0.1Bi2O3-10P2O5-89.9SiO2。The composition (molar percentage) of the Bi/P co-doped quartz glass in this embodiment is: 0.1Bi 2 O 3 -10P 2 O 5 -89.9SiO 2 .
Bi/P共掺杂石英玻璃的淬火过程包括：The quenching process of Bi/P co-doped quartz glass includes:
(1)先用丙酮或者酒精清洗玻璃表面，避免高温热处理时导致杂质的引入；(1) Clean the glass surface with acetone or alcohol first to avoid the introduction of impurities during high temperature heat treatment;
(2)将铋掺杂石英玻璃熔接在纯石英玻璃管一侧的端面上。经H2/O2＝2的氢氧焰加热至1600-1800℃的熔融状态；(2) The bismuth-doped quartz glass is welded on the end face of one side of the pure quartz glass tube. It is heated to a molten state of 1600-1800 ℃ by a hydrogen-oxygen flame with H 2 /O 2 =2;
(3)将处于熔融状态的掺铋石英玻璃迅速置于液氮中并完全浸泡，进行快速淬火处理；(3) quickly place the bismuth-doped quartz glass in molten state in liquid nitrogen and soak it completely, and carry out rapid quenching treatment;
(4)将淬火后的样品取出，加工成预定尺寸，双面抛光，然后清洗烘干(4) Take out the quenched sample, process it into a predetermined size, polish both sides, and then clean and dry
实施例7：(参见图4和表1)Example 7: (see Figure 4 and Table 1)
本实施例Bi/P共掺石英玻璃的成份(摩尔百分比)为：0.1Bi2O3-10P2O5-89.9SiO2。The composition (molar percentage) of the Bi/P co-doped quartz glass in this embodiment is: 0.1Bi 2 O 3 -10P 2 O 5 -89.9SiO 2 .
Bi/P共掺杂石英玻璃的淬火过程包括：The quenching process of Bi/P co-doped quartz glass includes:
(1)先用丙酮或者酒精清洗玻璃表面，避免高温热处理时导致杂质的引入；(1) Clean the glass surface with acetone or alcohol first to avoid the introduction of impurities during high temperature heat treatment;
(2)将铋掺杂石英玻璃熔接在纯石英玻璃管一侧的端面上。经H2/O2＝2的氢氧焰加热至1600-1800℃的熔融状态；(2) The bismuth-doped quartz glass is welded on the end face of one side of the pure quartz glass tube. It is heated to a molten state of 1600-1800 ℃ by a hydrogen-oxygen flame with H 2 /O 2 =2;
(3)将处于熔融状态的掺铋石英玻璃迅速置于液氦中并完全浸泡，进行快速淬火处理；(3) quickly place the bismuth-doped quartz glass in molten state in liquid helium and soak it completely, and carry out rapid quenching treatment;
(4)将淬火后的样品取出，加工成预定尺寸，双面抛光，然后清洗烘干(4) Take out the quenched sample, process it into a predetermined size, polish both sides, and then clean and dry
不同冷却液淬火得到样品的荧光归一化结果如图4。显著区别在于不同的冷却速率下导致玻璃的假想温度增加，内部结构混乱度增加，非对称性增加，从而促进了Bi相关活性中心种类和浓度的增加幅度不同。冷却速率越大，其荧光强度提升越明显。The fluorescence normalization results of the samples obtained by quenching with different coolants are shown in Figure 4. The significant difference is that different cooling rates lead to an increase in the fictive temperature of the glass, an increase in the disorder of the internal structure, and an increase in asymmetry, which promotes different increases in the types and concentrations of Bi-related active centers. The higher the cooling rate, the more obvious the increase in the fluorescence intensity.
表1实施例1-7的加热源和冷却方式与原始样品相比，在1170nm以及1400nm附近的荧光强度提升百分比Table 1 The heating source and cooling method of Examples 1-7 compared with the original sample, the percentage of fluorescence intensity improvement near 1170nm and 1400nm
本领域的技术人员容易理解，以上所述仅为本发明的较佳实施例，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改以及等同替换和改进，均应包含在本发明的保护范围之内。Those skilled in the art can easily understand that the above are only preferred embodiments of the present invention, and are not intended to limit the present invention. Any modifications, equivalent replacements and improvements made within the spirit and principles of the present invention shall be Included in the protection scope of the present invention.
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