WO2021004108A1 - 一种掺钕bgso混晶材料及其制备方法 - Google Patents

一种掺钕bgso混晶材料及其制备方法 Download PDF

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WO2021004108A1
WO2021004108A1 PCT/CN2020/084482 CN2020084482W WO2021004108A1 WO 2021004108 A1 WO2021004108 A1 WO 2021004108A1 CN 2020084482 W CN2020084482 W CN 2020084482W WO 2021004108 A1 WO2021004108 A1 WO 2021004108A1
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bgso
crystal
doped
neodymium
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李纳
徐军
徐晓东
宋青松
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南京同溧晶体材料研究院有限公司
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    • 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
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/20—Controlling or regulating
    • 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
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/16—Oxides
    • C30B29/22—Complex oxides

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  • the invention belongs to the technical field of laser materials, and relates to an infrared waveband laser crystal and a preparation method thereof, in particular to a neodymium-doped BGSO mixed crystal material and a preparation method thereof.
  • Nd:YCa 4 O(BO 3 ) 3 crystal achieves a slope efficiency of 57% at 1060nm and a laser output with an output power of 1900mW.
  • Nd:YAG achieves a laser output with a slope efficiency of 35% at 1300nm and an output power of 200mw.
  • BGO single crystal has the advantages of low thermal expansion coefficient (6.3 ⁇ 10 -6 /°C) and low effective phonon energy (400 cm -1 ), making it a promising laser matrix material.
  • Doping a small amount of SiO 2 in the BGO crystal to replace GeO 2 does not change its structure.
  • the crystals are mainly grown by the Czochralski method, the vertical Bridgman method and the micro pull-down method. Compared with other crystal growth methods, the micro pull-down method has the advantages of using less raw materials, fast growth speed, adjustable crystal diameter and short growth period.
  • the research on rare earth ion doped BGSO mixed crystal mainly focuses on the study of scintillation performance, such as: light yield, energy resolution and fluorescence decay time.
  • scintillation performance such as: light yield, energy resolution and fluorescence decay time.
  • the present invention provides a neodymium-doped BGSO mixed crystal material.
  • the chemical formula of the mixed crystal material is (Nd x Bi 1-x ) 4 (Ge 1-y Si y ) 3 O 12 , where the value range of x is 0.001-0.010, the value range of y is 0.05-0.5, and the unit cell parameter is
  • a method for preparing the above-mentioned mixed crystal material which adopts a micro pull-down method for growth, and the method mainly includes the following steps:
  • the initial raw materials are 5N purity Nd 2 O 3 , Bi 2 O 3 , GeO 2 and SiO 2 powders.
  • Second select Nd x Bi 1-x ) 4 (Ge 1-y Si y ) 3 O 12 carefully calculate the required mass of each raw material and weigh it accurately;
  • step (2) the time for grinding the raw materials is 40min-60min.
  • the heating rate is 75-155°C/h, and the temperature is kept at 700-850°C for 22-30h.
  • the pulling speed of the seed rod during seeding in step (4) is 0.25-0.65 mm/min, and the pulling speed is 5-8 mm/min when the crystal grows stably.
  • step (4) cooling process is 3-4 hours.
  • the present invention has the following advantages: (1) Compared with other crystal growth methods, the micro pull-down method of crystal growth has the advantages of less raw materials, fast growth rate, and short growth period. And the crystal diameter can be adjusted; (2) The micro pull-down method is used to grow the crystal, which can stably obtain the Nd:BGSO laser crystal with a diameter of 2mm and a length of 131mm, and the doping ratio of Nd ions and Si ions can be further adjusted Obtain near infrared laser output.
  • Figure 1 is a sample diagram of the mixed crystal material prepared by the present invention.
  • Figure 2 is an X-ray powder diffraction pattern of the sample of Example 1 prepared by the present invention.
  • Fig. 3 is a fluorescence diagram of the sample micro-area of Example 1 prepared by the present invention.
  • Figure 4 is a micro-area fluorescence image of a sample of Example 1 prepared by the present invention at a point taken along the diameter.
  • Figure 5 is the absorption spectrum of the sample of Example 1 prepared by the present invention at room temperature.
  • Fig. 6 is a refractive index diagram of a sample of Example 1 prepared by the present invention.
  • Figure 7 is the fluorescence spectrum of the sample of Example 1 prepared by the present invention.
  • Fig. 8 is a fluorescence lifetime diagram of a sample prepared in Example 1 of the present invention.
  • Example 1 Micro pull-down growth (Nd 0.003 Bi 0.997 ) 4 (Ge 0.95 Si 0.05 ) 3 O 12 was specifically prepared by the following method:
  • Nd 2 O 3 , Bi 2 O 3 , GeO 2 and SiO 2 powder as starting materials.
  • chemical formula (Nd 0.003 Bi 0.997 ) 4 (Ge 0.95 Si 0.05 ) 3 O 12 carefully calculate the required mass of each raw material and weigh it accurately.
  • the blank is sintered at a high temperature at a rate of 75°C/h and kept at 700°C for 30h After that, take it out and put it in a platinum crucible, and put it into a micro pull-down furnace for growth.
  • the growth program is adjusted so that the temperature in the furnace drops to room temperature after 4 hours, and the crystals are taken out.
  • the data obtained by experimenting with any selected crystal is shown in Figure 1-8.
  • the XRD diffraction peak of the crystal sample is consistent with the BGO standard card peak position, indicating that the grown crystal is pure BGO phase.
  • Through the micro-area fluorescence spectrum test it can be obtained that the Nd 3+ ion concentration distribution on the end face of the crystal is uniform.
  • the absorption cross section at 808 nm is 0.98 ⁇ 10 -20 cm 2 , and the half-height width is 17. nm.
  • the relatively large FWHM is more conducive to pumping with AlGaAs laser diodes.
  • Nd:BGSO crystal is a promising material for near-infrared laser output.
  • Example 2 Micro pull-down growth (Nd 0.005 Bi 0.995 ) 4 (Ge 0.95 Si 0.05 ) 3 O 12 is specifically prepared by the following method:
  • Example 3 Micro pull-down growth (Nd 0.007 Bi 0.993 ) 4 (Ge 0.95 Si 0.05 ) 3 O 12 was specifically prepared by the following method:

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  • Crystallography & Structural Chemistry (AREA)
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  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

一种掺钕BGSO混晶材料及其制备方法，该晶体的化学式为(Nd xBi 1-x) 4(Ge 1-ySi y) 3O 12，其中x的取值范围为0.001-0.01，y的取值范围是0.05-0.5，晶胞参数为a=b=c=10.513Å。使用纯度为5N的Nd 2O 3，Bi 2O 3，GeO 2和SiO 2粉末作为原料，经过充分研磨之后压制成棒，在700-850摄氏度下高温烧结22-30小时。采用微下拉生长掺钕BGSO混晶。

Description

一种掺钕BGSO混晶材料及其制备方法 技术领域
本发明属于激光材料技术领域，涉及一种红外波段激光晶体及其制备方法，特别涉及一种掺钕BGSO混晶材料及其制备方法。
背景技术
近年来，激光二极管泵浦固体激光器由于其在医疗、非线性光学和科学研究中的广泛应用而得以快速发展。激光材料是固体激光器的重要组成部分。其中，钕离子掺杂的激光晶体材料由于其具有较长的荧光寿命，较大的吸收截面和发射截面已获得瓦级激光输出。比如:Nd:YCa 4O(BO 3) 3晶体在1060nm实现斜率效率为57％，输出功率为1900mW的激光输出。Nd:YAG在1300nm实现斜率效率为35％，输出功率为200mw的激光输出。
近来，BGO单晶由于具有较低的热膨胀系数(6.3×10 -6/℃)和较低的有效声子能量(400cm -1)等优点使其成为一种极具发展前景的激光基质材料。在BGO晶体中掺入少量的SiO 2以取代GeO 2并不会改变其结构。目前，国内外已经有很多BGSO混晶的报道。晶体主要通过提拉法，垂直布里奇曼法和微下拉法进行生长。相比于其它晶体生长方法，微下拉法具有使用原料少，生长速度快，晶体直径可调和生长周期短等优点。关于稀土离子掺杂BGSO混晶的研究主要集中在闪烁性能的研究，例如：光产额，能量分辨率及荧光衰减时间等。然而，有关Nd 3+掺杂BGSO晶体的制备方法以及光谱性能的研究并没有相关报道。
发明内容
为了解决现有技术中制备BGSO混晶材料时用料多、生长速率慢及周期长等的缺陷，本发明提供了一种掺钕BGSO混晶材料，该混晶材料的化学式为(Nd xBi 1-x) 4(Ge 1-ySi y) 3O 12，其中x的取值范围为0.001-0.010，y的取值范围是0.05-0.5，晶胞参数为
Figure PCTCN2020084482-appb-000001
同时，还提供了一种上述混晶材料的制备方法，采用微下拉法进行生长，该方法主要包括以下步骤：
(1)初始原料为5N纯度的Nd 2O 3，Bi 2O 3，GeO 2和SiO 2粉末，先选定Nd离子掺杂取代Bi离子，Si离子取代Ge离子中Nd和Si离子合适浓度之后，按照化学式(Nd xBi 1-x) 4(Ge 1-ySi y) 3O 12仔细计算每种原料所需的质量，并准确称量；
(2)将称量后的粉末原料放入玛瑙研钵中充分研磨使原料混合均匀，然后使用油压机压成棒状料胚，高温烧结，取出放入铂金坩埚，装入微下拉炉中进行生长；
(3)选取合适籽晶，在进行装炉过程要保证籽晶、坩埚底部小孔中心和线圈中心处于同一竖直线上；
(4)在1.2-2.5小时内升温到0.45-0.052KW并恒温0.2-0.4小时以保证坩埚内原料全部熔化，再引晶并控制拉速以使晶体稳定生长，生长结束后慢慢进行降温过程，当降至室温时，取出成品晶体。
作为改进，步骤(2)将原料研磨的时间为40min-60min。
作为改进，步骤(2)对原料高温烧结时，升温速率为75-155℃/h，并在700-850℃恒温22-30h。
作为改进，步骤(3)中当保证籽晶、坩埚底部小孔中心和线圈中心处于同一竖直线上时，采用旋转籽晶杆，籽晶摆幅不超过1mm。
作为改进，步骤(4)引晶时籽晶杆的拉速为0.25-0.65mm/min，晶体稳定生长时拉速为5-8mm/min。
作为改进，步骤(4)降温过程的时间为3-4小时。
有益效果：本发明与现有技术相比，优点为：(1)采用的微下拉法的晶体生长方法，相对于其他晶体生长方法而言，其具有使用原料少，生长速率快，生长周期短和晶体直径可调控等优点；(2)采用微下拉法生长获得晶体，能够稳定地获得直径为2mm，长度为131mm的Nd：BGSO激光晶体，且可进一步调节Nd离子和Si离子的掺杂比例获得近红外激光输出。
附图说明
图1是本发明制备的混晶材料的样品图。
图2是本发明制备的实施例1样品X射线粉末衍射图谱。
图3是本发明制备的实施例1样品微区荧光图。
图4是本发明制备的实施例1样品的沿直径所取个点的微区荧光图。
图5是本发明制备的实施例1样品在室温下的吸收光谱。
图6是本发明制备的实施例1样品的折射率图。
图7是本发明制备的实施例1样品的荧光光谱。
图8是本发明制备的实施例1样品的荧光寿命图。
具体实施方式
下面对本发明附图和具体实施例作出进一步说明。
其中坩埚内原料全部熔化话，再进行引晶，控制拉速，开始控制拉速0.25-0.65mm/min保证熔料慢慢结晶后，再增加拉速到5-8mm/min，保证晶体能够稳定生长。
实施例1：微下拉法生长(Nd 0.003Bi 0.997) 4(Ge 0.95Si 0.05) 3O 12具体通过以下方法制备：
用5N纯度的Nd 2O 3，Bi 2O 3，GeO 2和SiO 2粉末作为初始原料。按照化学式(Nd 0.003Bi 0.997) 4(Ge 0.95Si 0.05) 3O 12仔细计算每种原料所需的质量并准确称量。将粉末原料放入玛瑙研钵中充分研磨，研磨40min使原料混合均匀，然后使用油压机压成棒状料胚，对料胚进行高温烧结，升温速率为75℃/h，且在700℃下恒温30h后，取出放入铂金坩埚，装入微下拉炉中进行生长。
选取合适的籽晶，进行装炉。在装炉过程要确保籽晶、坩埚底部小孔中心和线圈中心处于同一竖直线上，旋转籽晶杆，籽晶摆幅不超过1mm，一般优选为0-0.25mm。在2小时内升温到0.045KW并恒温0.3小时以保证坩埚内原料全部熔化，再开始引晶，控制拉速0.5mm/min保证熔料慢慢结晶，再增加拉速到5mm/min时晶体可以稳定生长。生长结束后调整生长程序使炉内温度在4小时后降至室温，取出晶体。任一选取获得晶体进行实验获得数据见图1-8所示，如图2所示，晶体样品的XRD衍射峰与BGO标准卡片峰位一致，表明生长所得的晶体为纯的BGO相。通过微区荧光光谱测试可得，晶体端面Nd 3+离子浓度分布均匀。在808nm处的 吸收截面为0.98×10 -20cm 2，半高宽为17.nm。相对较大的半高宽更有利于用AlGaAs激光二极管泵浦。通过JO理论计算得到在1063nm处的截面为3.15×10 -20cm 2，荧光量子效率为82.7％(荧光寿命为248微妙)。以上结果表明，Nd：BGSO晶体是一种很有希望的近红外激光输出的材料。
实施例2：微下拉法生长(Nd 0.005Bi 0.995) 4(Ge 0.95Si 0.05) 3O 12具体通过以下方法制备：
用5N纯度的Nd 2O 3，Bi 2O 3，GeO 2和SiO 2粉末作为初始原料，按照化学式(Nd 0.005Bi 0.995) 4(Ge 0.95Si 0.05) 3O 12仔细计算每种原料所需的质量并准确称量。将粉末原料放入玛瑙研钵中充分研磨，研磨50min使原料混合均匀，然后使用油压机压成棒状料胚，对料胚进行高温烧结，升温速率为100℃/h，且在850℃下恒温24h后，取出放入铂金坩埚，装入微下拉炉中进行生长。
选取合适的籽晶，进行装炉。在装炉过程要确保籽晶、坩埚底部小孔中心和线圈中心处于同一竖直线上，旋转籽晶杆，籽晶摆幅不超过1mm，一般优选为0-0.2mm。在1.2小时内升温到0.05KW并恒温0.4小时以保证坩埚内原料全部熔化，再开始引晶，控制拉速0.25mm/min保证熔料慢慢结晶，再增加拉速到8mm/min时晶体可以稳定生长。生长结束后调整生长程序使炉内温度在3小时后降至室温，取出晶体。
实施例3：微下拉法生长(Nd 0.007Bi 0.993) 4(Ge 0.95Si 0.05) 3O 12具体通过以下方法制备：
用5N纯度的Nd 2O 3，Bi 2O 3，GeO 2和SiO 2粉末作为初始原料，按照化学式(Nd 0.007Bi 0.993) 4(Ge 0.95Si 0.05) 3O 12仔细计算每种原料所需的质量并准确称量。将粉末原料放入玛瑙研钵中充分研磨，研磨60min使原料混合均匀，然后使用油压机压成棒状料胚，对料胚进行高温烧结，升温速率为155℃/h，且在755℃下恒温22h后，取出放入铂金坩埚，装入微下拉炉中进行生长。
选取合适的籽晶，进行装炉。在装炉过程要确保籽晶、坩埚底部小孔中心和线圈中心处于同一竖直线上，旋转籽晶杆，籽晶摆幅不超过1mm，一般优选为0-0.15mm。在2.5小时内升温到0.052KW并恒温0.2小时以保证坩埚内原料全部熔化，再开始引晶，控制拉速0.65mm/min保证熔料慢慢结晶，再增加拉速到6.5mm/min时晶体可以稳定生长。生长结束后调整生长程序使炉内温度在3.2小时后降至室温，取出晶体。
以上所述实施例仅表达了本发明的几种实施方式，其描述较为具体和详细，但并不能因此而理解为对发明专利范围的限制。应当指出的是，对于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进，这些都属于本发明的保护范围。因此，本发明专利的保护范围应以所附权利要求为准。

Claims (7)

  1. 一种掺钕BGSO混晶材料，其特征在于，该混晶材料的化学式为(Nd xBi 1-x) 4(Ge 1-ySi y) 3O 12，其中x的取值范围为0.001-0.010，y的取值范围是0.05-0.5，晶胞参数为
    Figure PCTCN2020084482-appb-100001
  2. 一种如权利要求1所述的掺钕BGSO混晶材料的制备方法，其特征在于，采用微下拉法进行生长，该方法主要包括以下步骤：
    (1)初始原料为5N纯度的Nd 2O 3，Bi 2O 3，GeO 2和SiO 2粉末，先选定Nd离子掺杂取代Bi离子，Si离子取代Ge离子中Nd和Si离子合适浓度之后，按照化学式(Nd xBi 1-x) 4(Ge 1-ySi y) 3O 12仔细计算每种原料所需的质量，并准确称量；
    (2)将称量后的粉末原料放入玛瑙研钵中充分研磨使原料混合均匀，然后使用油压机压成棒状料胚，高温烧结，取出放入铂金坩埚，装入微下拉炉中进行生长；
    (3)选取合适籽晶，在进行装炉过程要保证籽晶、坩埚底部小孔中心和线圈中心处于同一竖直线上；
    (4)在1.2-2.5小时内升温到0.045-0.052KW并恒温0.2-0.4小时以保证坩埚内原料全部熔化，再引晶并控制拉速以使晶体稳定生长，生长结束后慢慢进行降温过程，当降至室温时，取出成品晶体。
  3. 根据权利要求2所述的一种掺钕BGSO混晶材料及其制备方法，其特征在于，步骤(2)将原料研磨的时间为40min-60min。
  4. 根据权利要求2所述的掺钕BGSO混晶材料的制备方法，其特征在于，步骤(2)对原料高温烧结时，升温速率为75-155℃/h，并在700-850℃恒温22-30h。
  5. 根据权利要求2所述的掺钕BGSO混晶材料的制备方法，其特征在于，步骤(3)中当保证籽晶、坩埚底部小孔中心和线圈中心处于同一竖直线上时，采用旋转籽晶杆，籽晶摆幅不超过1mm。
  6. 根据权利要求2所述的掺钕BGSO混晶材料的制备方法，其特征在于，步骤(4)引晶时籽晶杆的拉速为0.25-0.65mm/min，晶体稳定生长时拉速为5-8mm/min。
  7. 根据权利要求2所述的掺钕BGSO混晶材料的制备方法，其特征在于，步骤(4)降温过程的时间为3-4小时。
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