CN101864595A - Erbium-doped gadolinium lithium fluoride crystal and growth method thereof - Google Patents
Erbium-doped gadolinium lithium fluoride crystal and growth method thereof Download PDFInfo
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- 239000013078 crystal Substances 0.000 title claims abstract 20
- UXWABHLCKSZTFY-UHFFFAOYSA-J lithium gadolinium(3+) tetrafluoride Chemical compound [Li+].[F-].[F-].[F-].[F-].[Gd+3] UXWABHLCKSZTFY-UHFFFAOYSA-J 0.000 title claims abstract 12
- 238000000034 method Methods 0.000 title claims abstract 7
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Inorganic materials [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims abstract 5
- 229910052691 Erbium Inorganic materials 0.000 claims abstract 3
- 229910005690 GdF 3 Inorganic materials 0.000 claims abstract 3
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 claims abstract 3
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 claims abstract 2
- 150000002500 ions Chemical class 0.000 claims abstract 2
- 239000000463 material Substances 0.000 claims abstract 2
- 239000011159 matrix material Substances 0.000 claims abstract 2
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract 2
- 150000002910 rare earth metals Chemical class 0.000 claims abstract 2
- 239000002994 raw material Substances 0.000 claims abstract 2
- 238000000137 annealing Methods 0.000 claims 1
- 238000002109 crystal growth method Methods 0.000 claims 1
- 238000002360 preparation method Methods 0.000 claims 1
- HIQSCMNRKRMPJT-UHFFFAOYSA-J lithium;yttrium(3+);tetrafluoride Chemical compound [Li+].[F-].[F-].[F-].[F-].[Y+3] HIQSCMNRKRMPJT-UHFFFAOYSA-J 0.000 abstract 2
- 238000002844 melting Methods 0.000 abstract 1
- 230000008018 melting Effects 0.000 abstract 1
- 230000005693 optoelectronics Effects 0.000 abstract 1
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Abstract
掺铒氟化钆锂晶体及其生长方法，属于光电子材料技术领域。现有掺铒氟化钇锂晶体因离子半径匹配方面的原因，掺杂浓度低；在生长这种晶体的过程中，由于氟化钇锂熔点高，原料挥发严重，难以生长出大尺寸的晶体。本发明之掺铒氟化钆锂晶体属于四方晶系，以稀土铒为激活离子，所述掺铒氟化钆锂晶体分子式为Er:LiGdF4，晶体基质为氟化钆锂；其生长方法特征在于LiF按LiF∶GdF3＝16.5～17∶7.76～8过量加入，晶体生长工艺参数确定为提拉速度：0.3～0.8mm/h，旋转速度：3～10rpm，生长温度：745～755℃。掺铒氟化钆锂晶体是一种激光晶体，适用于大功率固体激光器。
An erbium-doped gadolinium lithium fluoride crystal and a growth method thereof belong to the technical field of optoelectronic materials. The existing erbium-doped yttrium lithium fluoride crystal has a low doping concentration due to the matching of ionic radii; in the process of growing this crystal, due to the high melting point of yttrium lithium fluoride, the raw materials volatilize seriously, and it is difficult to grow large-sized crystals . The erbium-doped lithium gadolinium fluoride crystal of the present invention belongs to the tetragonal crystal system, and the rare earth erbium is used as the active ion. The molecular formula of the erbium-doped gadolinium lithium fluoride crystal is Er:LiGdF 4 , and the crystal matrix is lithium gadolinium fluoride; the characteristics of its growth method LiF is added in excess according to LiF:GdF 3 =16.5~17:7.76~8, and the crystal growth process parameters are determined as pulling speed: 0.3~0.8mm/h, rotation speed: 3~10rpm, growth temperature: 745~755°C. Erbium-doped gadolinium fluoride lithium crystal is a laser crystal suitable for high-power solid-state lasers.
Description
技术领域technical field
本发明涉及一种掺铒氟化钆锂晶体及其生长方法，掺铒氟化钆锂晶体是一种激光晶体，简式为Er:GLF，属于光电子材料技术领域。The invention relates to an erbium-doped gadolinium lithium fluoride crystal and a growth method thereof. The erbium-doped gadolinium lithium fluoride crystal is a laser crystal with a simplified formula of Er:GLF and belongs to the technical field of optoelectronic materials.
背景技术Background technique
掺铒激光具有大气传输特性好、烟雾穿透能力强、保密性好等特点，被应用于激光测距、激光雷达、光电干扰、遥感、环境监测、光通讯等领域。另外，掺铒激光在水中有较强吸收，从而不仅对人眼安全，而且能够精确介入生物组织，因此，在医疗领域如眼科手术也有应用价值。Erbium-doped laser has the characteristics of good atmospheric transmission characteristics, strong smoke penetration ability, and good confidentiality. It is used in laser ranging, lidar, photoelectric interference, remote sensing, environmental monitoring, optical communication and other fields. In addition, the erbium-doped laser has strong absorption in water, so it is not only safe for human eyes, but also can accurately intervene in biological tissues. Therefore, it is also valuable in medical fields such as ophthalmic surgery.
掺铒激光所用激光材料为掺铒晶体，包括氟化物晶体，如Er:LiYF4，属于四方晶系，其折射率温度系数较小，升温造成的折射率减小可以部分抵消因热膨胀引起的光程增大，因而热透镜效应很小。激光振荡阈值大为降低，增益明显提高，具有吸收峰宽、荧光寿命长、热效应小等特点。尽管Er:LiYF4激光晶体性能优异，但是，因铒、钇离子半径匹配方面的原因，掺杂浓度低，只有20at.％。The laser material used in the erbium-doped laser is erbium-doped crystal, including fluoride crystal, such as Er:LiYF 4 , which belongs to the tetragonal crystal system, and its temperature coefficient of refractive index is small. The distance increases, so the thermal lens effect is small. The laser oscillation threshold is greatly reduced, the gain is significantly increased, and it has the characteristics of wide absorption peak, long fluorescence lifetime, and small thermal effect. Although the Er:LiYF 4 laser crystal has excellent performance, the doping concentration is low, only 20 at.%, due to the matching of erbium and yttrium ion radii.
现有Er:LiYF4晶体的生长方法如下：The existing Er: LiYF 4 crystal growth method is as follows:
1、生长料制备1. Preparation of growth material
理论上LiF∶YF3＝1∶1，实际上LiF按LiF∶YF3＝13∶12过量加入，再配合晶体生长工艺参数，方能生长出晶格完整的晶体。因此，原料中各组分的配比如下，ErF3为x摩尔、YF3为(1-x)摩尔，LiF为1.083(1-x)摩尔，其中x的取值范围为：0.005mol≤x≤0.2mol。将所述组分充分混合，通过HF气氛处理，用液压机压块得块状生长料。Theoretically, LiF:YF 3 =1:1, in fact, LiF is added in excess according to LiF:YF 3 =13:12, and combined with the crystal growth process parameters, the crystal with complete lattice can be grown. Therefore, the ratio of each component in the raw material is as follows, ErF 3 is x moles, YF 3 is (1-x) moles, LiF is 1.083(1-x) moles, and the value range of x is: 0.005mol≤x ≤0.2mol. The components are fully mixed, treated with HF atmosphere, and pressed into blocks by a hydraulic press to obtain a block growth material.
2、晶体生长2. Crystal growth
采用提拉法生长Er:LiYF4晶体。将所制备的生长料装入单晶炉，抽真空，充入氩气，晶体生长的主要参数确定为：提拉速度1mm/h，旋转速度5rpm，生长温度810℃。Er:LiYF 4 crystals were grown by pulling method. The prepared growth material was loaded into a single crystal furnace, vacuumed and filled with argon, and the main parameters of crystal growth were determined as follows: pulling speed 1mm/h, rotation speed 5rpm, growth temperature 810°C.
3、退火3. Annealing
晶体生长完毕后，采用原位退火的方式缓慢将炉温降至室温，取出晶体。After the crystal growth is completed, the furnace temperature is slowly lowered to room temperature by in-situ annealing, and the crystal is taken out.
所述晶体生长方法也有其不足，在生长Er:LiYF4晶体的过程中，由于LiYF4熔点高，如810℃，因而原料挥发严重，难以生长出大尺寸的Er:LiYF4晶体，如晶体尺寸只有Φ13mm×20mm。The crystal growth method also has its shortcomings. In the process of growing Er: LiYF4 crystals, due to the high melting point of LiYF4 , such as 810°C, the raw materials volatilize seriously, and it is difficult to grow large-sized Er: LiYF4 crystals, such as the crystal size Only Φ13mm×20mm.
发明内容Contents of the invention
为了提高掺铒氟化物晶体的掺杂浓度，并且生长出大尺寸的晶体，我们提出一种掺铒氟化钆锂晶体及其生长方法的方案，其中须根据钆、钇的不同确定适宜的生长方案，所生长的掺铒氟化钆锂晶体不仅具有与Er:LiYF4相似的光谱，而且掺杂浓度高、尺寸大，能够用于大功率固体激光器。In order to increase the doping concentration of erbium-doped fluoride crystals and grow large-sized crystals, we propose a plan for erbium-doped gadolinium fluoride lithium fluoride crystals and their growth methods, in which the appropriate growth must be determined according to the difference between gadolinium and yttrium. According to the scheme, the grown erbium-doped gadolinium lithium fluoride crystal not only has a spectrum similar to that of Er:LiYF 4 , but also has high doping concentration and large size, which can be used in high-power solid-state lasers.
本发明之掺铒氟化钆锂晶体属于四方晶系，以稀土铒为激活离子，其特征在于，所述掺铒氟化钆锂晶体分子式为Er:LiGdF4，晶体基质为氟化钆锂。The erbium - doped lithium gadolinium fluoride crystal of the present invention belongs to the tetragonal crystal system, and the rare earth erbium is used as the active ion.
本发明之生长方法其步骤包括生长料制备、晶体生长以及退火，其特征在于，LiF按LiF∶GdF3＝16.5～17∶7.76～8过量加入；晶体生长工艺参数确定为提拉速度：0.3～0.8mm/h，旋转速度：3～10rpm，生长温度：745～755℃。The steps of the growth method of the present invention include the preparation of growth material, crystal growth and annealing. It is characterized in that LiF is added in excess according to LiF:GdF 3 =16.5～17:7.76～8; the crystal growth process parameters are determined as pulling speed: 0.3～ 0.8mm/h, rotation speed: 3-10rpm, growth temperature: 745-755°C.
本发明其效果在于，Er:LiGdF4晶体属于四方晶系且无缺陷，由于铒、钆离子半径匹配，掺杂浓度最高可达100at.％，根据需要，控制实际的、最佳的掺杂浓度，这一高掺杂效果能够从附图即本发明之掺铒氟化钆锂晶体荧光光谱图中的峰值看出。LiGdF4熔点为750℃，晶体的生长温度与之相适应，因此，原料挥发减轻，从而能够容易生长出大尺寸的晶体，如Φ30mm×50mm。The effect of the present invention is that the Er:LiGdF 4 crystal belongs to the tetragonal crystal system and has no defects. Due to the matching of erbium and gadolinium ion radii, the doping concentration can reach up to 100 at.%, and the actual and optimal doping concentration can be controlled according to the needs. , this high doping effect can be seen from the attached figure, that is, the peak in the fluorescence spectrum of the erbium-doped gadolinium lithium fluoride crystal of the present invention. The melting point of LiGdF 4 is 750°C, and the crystal growth temperature is suitable for it. Therefore, the volatilization of raw materials is reduced, so that large-sized crystals can be easily grown, such as Φ30mm×50mm.
附图说明Description of drawings
附图是本发明之掺铒氟化钆锂晶体荧光光谱图，该图兼作为摘要附图。Accompanying drawing is the fluorescence spectrogram of erbium-doped gadolinium lithium fluoride crystal of the present invention, and this figure also serves as abstract accompanying drawing.
具体实施方式Detailed ways
本发明之掺铒氟化钆锂晶体属于四方晶系，以稀土铒为激活离子，所述掺铒氟化钆锂晶体分子式为Er:LiGdF4，晶体基质为氟化钆锂，铒的掺入浓度为20～50at.％。The erbium-doped lithium gadolinium fluoride crystal of the present invention belongs to the tetragonal crystal system, and the rare earth erbium is used as the active ion. The concentration is 20-50 at.%.
本发明之生长方法具体如下：Growth method of the present invention is specifically as follows:
1、生长料制备1. Preparation of growth material
LiF按LiF∶GdF3＝16.5～17∶7.76～8过量加入。原料中各组分的配比如下，ErF3为x摩尔、GdF3为(1-x)摩尔，LiF为2.125(1-x)摩尔，其中x的取值范围为：0.005mol≤x≤1mol。将所述组分充分混合，通过HF气氛处理，用液压机压块得块状生长料。LiF was added in excess according to LiF:GdF 3 =16.5~17:7.76~8. The proportion of each component in the raw material is as follows, ErF 3 is x moles, GdF 3 is (1-x) moles, LiF is 2.125 (1-x) moles, and the value range of x is: 0.005mol≤x≤1mol . The components are fully mixed, treated with HF atmosphere, and pressed into blocks by a hydraulic press to obtain a block growth material.
2、晶体生长2. Crystal growth
采用提拉法生长Er:LiGdF4晶体。将所制备的生长料装入单晶炉，抽真空，充入氩气，晶体生长的主要参数确定为：提拉速度：0.3～0.8mm/h；旋转速度：3～10rpm，生长温度：745～755℃。Er:LiGdF 4 crystals were grown by pulling method. Put the prepared growth material into the single crystal furnace, vacuumize and fill with argon, the main parameters of crystal growth are determined as follows: pulling speed: 0.3-0.8mm/h; rotation speed: 3-10rpm, growth temperature: 745 ~755°C.
3、退火3. Annealing
晶体生长完毕，采用原位退火的方式缓慢将炉温降至室温，取出晶体。After the crystal growth is completed, the furnace temperature is slowly lowered to room temperature by in-situ annealing, and the crystal is taken out.
下面是一个具体例子，LiF按LiF∶GdF3＝17∶8过量加入。取x＝0.3，原料中各组分的配比如下，ErF30.3摩尔、GdF30.7摩尔，LiF1.4875摩尔。将所述组分充分混合，通过HF气氛处理，用液压机压块得块状生长料。采用提拉法生长Er:LiGdF4晶体。将所制备的生长料装入铱坩埚并放入中频感应加热单晶炉，抽真空至10-4Pa，充入氩气。晶体生长的主要参数确定为：提拉速度：0.5mm/h，旋转速度：7rpm，生长温度：750℃。晶体生长完毕，采用原位退火的方式缓慢将炉温降至室温，取出晶体。该晶体为掺铒氟化钆锂晶体，属于四方品系，晶体质量较好，尺寸为Φ30mm×50mm。经测试，铒的掺入浓度为30at.％。经光谱测试，本发明之掺铒氟化钆锂晶体与现有掺铒氟化钇锂晶体相比，荧光峰值波长相近，荧光峰值有所提高，见附图所示。The following is a specific example, LiF is added in excess according to LiF:GdF 3 =17:8. Taking x=0.3, the proportion of each component in the raw material is as follows, ErF 3 0.3 mole, GdF 3 0.7 mole, LiF 1.4875 mole. The components are fully mixed, treated with HF atmosphere, and pressed into blocks by a hydraulic press to obtain a block growth material. Er:LiGdF 4 crystals were grown by pulling method. The prepared growth material was put into an iridium crucible and placed in a medium frequency induction heating single crystal furnace, vacuumed to 10 -4 Pa, and filled with argon. The main parameters of crystal growth were determined as follows: pulling speed: 0.5mm/h, rotation speed: 7rpm, growth temperature: 750°C. After the crystal growth is completed, the furnace temperature is slowly lowered to room temperature by in-situ annealing, and the crystal is taken out. The crystal is an erbium-doped gadolinium lithium fluoride crystal, belonging to the Sifang strain, with good crystal quality and a size of Φ30mm×50mm. After testing, the doping concentration of erbium is 30 at.%. According to the spectrum test, compared with the existing erbium-doped yttrium lithium fluoride crystal, the fluorescence peak wavelength of the erbium-doped gadolinium lithium fluoride crystal of the present invention is similar, and the fluorescence peak value is improved, as shown in the attached drawing.
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| CN102321482A (en) * | 2011-05-24 | 2012-01-18 | 南京航空航天大学 | Photoluminescence material with frequency synergistic light conversion and preparation method as well as use thereof |
| CN103820854A (en) * | 2014-02-20 | 2014-05-28 | 宁波大学 | A kind of Ce3 + ion-doped gadolinium lithium fluoride ultraviolet laser crystal and preparation method thereof |
| CN104099665A (en) * | 2014-07-09 | 2014-10-15 | 北京雷生强式科技有限责任公司 | Yttrium lithium fluoride composite crystal and preparation method thereof |
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