掺质Ca_3（VO_4）_2晶体生长与光谱性质的研究
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摘要
钒酸钙晶体（Ca3(VO4)2）是目前少有的几种高居里点铁电体之一，铁电相变温度为1110℃。它的非线性系数可与KDP晶体相比。因此，它很有希望成为激光基质或激光自倍频基质。
本文尝试了液相,固相合成,固液结合三种方法合成原料,并用红外光谱，差热分析和X-射线粉末衍射对合成的产物进行了表征，结果表明，只有固相合成法才能生成纯度较高的Ca3(VO4)2原料。用Czochraski法（提拉法）生长了不同掺杂浓度的Yb: Ca3(VO4)2和Yb:Er: Ca3(VO4)2晶体，对晶体生长条件，气氛以及开裂原因进行了研究。
测试了不同掺杂浓度的Yb: Ca3(VO4)2晶体的偏振吸收光谱，非偏振吸收光谱，荧光光谱，计算了Yb3+的2F7/2-2F5/2能级跃迁的发射截面，辐射跃迁几率，辐射寿命等光谱参数。同时测试了Yb:Er: Ca3(VO4)2晶体的偏振吸收光谱与非偏振荧光光谱，用J-O理论计算了Er3+各能级跃迁的光谱参数，并讨论了Yb3+- Er3+之间的能量转移过程。
The Ca3(VO4)2 crystal is one of ferroelectricity crystal with a high Curie temperature,Tc , of 1100℃. Its nonline coefficient is as big as KDP ceystal.So, it is a promiseful laser host material or a laser host material whose frequency can be doubled by itself.
In this thesis , the materials synthesis of Ca3(VO4)2 with the way of liquid phase, solid phase and the way which includes not only liquid phase but also solid phase are presented, and the raw materials of synthesis with these way were detected with infrared absorption spectrum，differential thermal analysis and X-ray diffractionmethod. The results show the high purity starting materials of calcium orthovanadate can only be prepared with the way of solid phase reaction.The Ca3(VO4)2 crystal with various doped concentration was grown by Czoochraskl method.The growth condition, atmosphere and the reason of crystal crack were investigated.
The polarization absorption spectra , the non-polarization absorption spectra and fluorescence spectra of Yb: Ca3(VO4)2 crystal were measured. The spectra parameters of these crystals can be calculated. And the polarization absorption spectra and non-fluorescence spectra of Yb:Er: Ca3(VO4)2 crystal were also measured.The spectra parameters can be calculated according to the J-O theory. Energy transfer between Yb3+ and Er3+ were investigated.
本文尝试了液相,固相合成,固液结合三种方法合成原料,并用红外光谱，差热分析和X-射线粉末衍射对合成的产物进行了表征，结果表明，只有固相合成法才能生成纯度较高的Ca3(VO4)2原料。用Czochraski法（提拉法）生长了不同掺杂浓度的Yb: Ca3(VO4)2和Yb:Er: Ca3(VO4)2晶体，对晶体生长条件，气氛以及开裂原因进行了研究。
测试了不同掺杂浓度的Yb: Ca3(VO4)2晶体的偏振吸收光谱，非偏振吸收光谱，荧光光谱，计算了Yb3+的2F7/2-2F5/2能级跃迁的发射截面，辐射跃迁几率，辐射寿命等光谱参数。同时测试了Yb:Er: Ca3(VO4)2晶体的偏振吸收光谱与非偏振荧光光谱，用J-O理论计算了Er3+各能级跃迁的光谱参数，并讨论了Yb3+- Er3+之间的能量转移过程。
The Ca3(VO4)2 crystal is one of ferroelectricity crystal with a high Curie temperature,Tc , of 1100℃. Its nonline coefficient is as big as KDP ceystal.So, it is a promiseful laser host material or a laser host material whose frequency can be doubled by itself.
In this thesis , the materials synthesis of Ca3(VO4)2 with the way of liquid phase, solid phase and the way which includes not only liquid phase but also solid phase are presented, and the raw materials of synthesis with these way were detected with infrared absorption spectrum，differential thermal analysis and X-ray diffractionmethod. The results show the high purity starting materials of calcium orthovanadate can only be prepared with the way of solid phase reaction.The Ca3(VO4)2 crystal with various doped concentration was grown by Czoochraskl method.The growth condition, atmosphere and the reason of crystal crack were investigated.
The polarization absorption spectra , the non-polarization absorption spectra and fluorescence spectra of Yb: Ca3(VO4)2 crystal were measured. The spectra parameters of these crystals can be calculated. And the polarization absorption spectra and non-fluorescence spectra of Yb:Er: Ca3(VO4)2 crystal were also measured.The spectra parameters can be calculated according to the J-O theory. Energy transfer between Yb3+ and Er3+ were investigated.
引文
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[4] 曹余惠,稀土激光晶体的发展.
[5] 唐有其,当代化学前沿,中国致公出版社,第二版,1997:944
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[7] Johnson l f,geusic j e and van uitert l g ,coherent oscillations from Tm,Ho,Yb,ErI ions in YAG ,appt.phys.lettl,1965,7(5):127.
[8] paul-henri haumesser,romain gaume,jean-marie benitez,et al,caodhralski growth of sex Yb-doped double borate and silicate laser materials,journal of crystal growth 233（2001）233－242
[9] H.r.xia,l.x.li,h.j.zhamg,et al,roman spectra and laser properties of Yb-doped yttrium orthovanadate crystals,journal of applied physics,2000,87:269-273.
[10] xuelu zou and hisayoshi toratani,evaluation of spectroscopic properties 0f Yb-doped glasses,physical review b,1995,52:15889-15897.
[11] lacovara p,choi h k,wang c a,et al.,room-temperature diode-pumped Yb:YAG laser,opt.lett.,1991,16(14):1089.
[12] fan t y,aperture guiding in quasi-three level lasers,opt.leet,1994.19(8):544
[13] sumida d s and fan t y,room-temperature 50mj/pulse side-diode-pumped Yb:YAG
laser ,opt.lett.,1991,20(23)2384.
[14] brauch u,giesen a,karszewski m,et al.,multiwatt diode-pumped Yb:YAG thin disk laser comtinuously tunable between 1018 a nd 1013nm,opt.lett,1995,20(7):713
[15]bresselbac h and sumide d s,65-w0average-power Yb-YAGlaser,opt.lett, 1995,
21(7):480
[16] tiara t,kobayaski t,tulloch w m ,et al,single axial-mode oscillation of a coupled cavity Yb:YAG laser,advanced solid –state laser,1996,1:14-15
[17] bibeau c,beach r j,Mitchell s c,et al.,high-avarage-power 1-1mperformence and frequency comversion of a diode-end-pumped Yb:YAG laser,ieee j.quantum electron.,1998,34(10):2010.
[18] louts g b and chai b h t ,the growth of high quality crystals of FAP and its isomorphs ,SPIE,1994,1863:31.
[19] orth c,breach r ,bibeau c,etal,design modeling of 100 j-diode-pumped solid-state lasers for project mercury,spie,1998,3265:114.
[20] schaffeers k I ,deloach l d and payne s a,crystal growth ,frequency doubling and infrared laser performance of Yb:BaCaBO3F,ieee j.quantum electron,1996,3295):741.
[21] Chai b h et al ,laseing,secong harmonic converstion and self-frequency doubling of Yb:YCOB osa topicsl conference on advanced solid state lasers, 1998,posteadline,
11-2.
[22]孟宪林，张怀金，祝莉等， Yb:YCa4O(BO3)3晶体及其激光器研究，中国激光，1999，26（1）：108。
[23] 田丽莉，王据阳，魏景谦等，Yb:YAB晶体的生长以及性质研究， 人工晶体学报，1998，27（3）：325。
[23] honninger c,zhang g,keller u,et al, femtosecong Yb:YAG laser using semiconductor saturable absorber,opt.lett,1995,20(23)2402
[24] honninger c,kartner f x,zhang g,et al , femtosecong mode locked Yb:YAG laser,advanced solid-state lasers ,1996,1:16.
[25] ausder au j,schaser s f,paschotta r,et al,high-power diopde-pumped passively mode-locked Yb:YAG laser,opt.lett,1999,24(18):1281.
[26] 龙晓，等，锁模Yb:SFAP激光器，光子学报，1997，26（11）：1008
[30] The Structure of Ca3(VO4)2, Zeitschrift fur Kristallographie,1973,137:67
[31] Glass A M,Abrahams S C and Ballman A A, Calcium Orthovanadate, Ca3(VO4)2- A New High Temperature Ferroelectric,Ferroelectrics,1978,17:579-582。
[33] Bechthold P S ,et al.linear and noliner optical properties of Ca3(VO4)2, optics communications,1978,27(3):393.
[34] 赵志伟，姜彦岛。生长正钒酸钙晶体Ca3(VO4)2的原料制备[J].人工晶体学报，1999，28（4）：350。
[35] 赵志伟，姜彦岛。正钒酸钙晶体的生长与退火的研究, [J].人工晶体学报，2000,29(1):34.
[36] Brixner L H and flourniy p a and keith bab cock,note on calcium- Orthovanadate,journal of the electrochemical Society, joly, 1964, 111(7):873-874.
[37] 卢绍芳,何美云,黄金陵, 硼酸钡低温相的晶体结构,物理学报, 1982,(31),948
[38] Lieberty j,stahr s,zur tiefte mperaturphase von BaB2O4, Z,kristallogr,1983,
(91):34
[39] Brixner L H and Flournoy P A. Calcium Orthovanadate Ca3(VO4)2-A New Laser Host Crystal.Journal of the electrochemical Society,March 1965,112(3):201-
298。
[40] Redden Martha j and buerger martin j,note on the symmetry and cell of calcium orthovanadate, Zeitschrift fur Kristallographie,1978,17:579-582.
[42] 赵志伟，姜彦岛。(Nd3+ Yb3+): Ca3(VO4)2晶体的极化研究, [J].人工晶体学报，2000,29(2),164-167.
[43] 赵志伟，姜彦岛。 稀土掺质 Ca3(VO4)2晶体的缺陷研究, [J]. 人工晶体学报.
[44] Brixner L H and Flournoy P A. K B, Note on Calcium Orthovanadate. Journal of the electrochemical Society, 1964,111(7):873
[45] 赵志伟，姜彦岛。 (Nd3+ Yb3+): Ca3(VO4)2晶体的电荷补尝与分凝系数的关系. [J].人工晶体学报，2000,29(2),143-146.
[46] 吕坚，提拉法生长的晶体的原料制备，人工晶体学报，24（增刊）1994。
[47] paoder diffraction file,sets 16-18,1979。
[48] Brixner L H and Flournoy P A. Calcium Orthovanadate Ca3(VO4)2-A New Laser Host Crystal.Journal of the electrochemical Society,March 1965,112(3):201-
298。
[49] 赵志伟，姜彦岛。生长正钒酸钙晶体Ca3(VO4)2的原料制备[J].人工晶体学报，1999，28（4）：350。
[50] 位民，李敢生，诸月梅，等。钒酸钇（Nd3+:YVO4）晶体的原料合成[J].人工晶体学报，1998，27（5）：178。
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