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The melting point of Ti:MgAl2O4 crystal is as high as 2130 °C, it is a challenge to obtain a large-sized and high-quality laser crystal. By optimizing the crystal growth process, Ti:MgAl2O4 crystal with a size of 30 mm× 70 mm is successfully grown by the Czochralski method under the condition of weak reducing atmosphere. The X-ray diffraction pattern is studied, and the x-ray rocking curve indicates that the grown crystal has a high crystalline quality in terms of the lower full width at half maximum(FWHM) intensity, which provides a material basis for the next laser output experiment. In a range of 100–1000 cm–1, there are four Raman vibration peaks located at 312, 410, 675 cm–1 and 771 cm–1 respectively. The grown crystal has an absorption cutoff range of 250–318 nm and two wide absorption bands of 395–495 nm and 550–1100 nm. Excited by 271 nm, the grown crystal shows a strong broadband emission ina range of 340–650 nm with a peak centered at 480 nm. After annealing in hydrogen atmosphere, shape of the transmittance spectrum and emission spectrum are both unchanged, but the fluorescent emission intensity is significantly reduced. After annealing in air atmosphere, the original two absorption bands disappear while none of the characteristics of fluorescence emission in a 340–650 nm range changes significantly. In addition, a new fluorescence emission peak near 725 nm is observed. Combining with the ESR spectrum, what we canconfirm is that the Ti:MgAl2O4 as-grown crystal contains Ti3+ and Ti4+ ions, and no ESR signal of Ti3+ is observed after annealing in air atmosphere. Moreover, excitationspectrum is also recorded. The fluorescence lifetime is 14 μs at room temperature, which is 4–5 times that of Ti:Al2O3 crystal and Ti:BeAl2O4 crystal. Furthermore, the emission cross section of the grown Ti:MgAl2O4 crystal is calculated from the Füchtbauer-Ladenburg (F-L) formula and its value is 2 × 10–20 cm2, large emission cross section which is beneficial for realizing laser oscillation. All the above results show that the Ti:MgAl2O4 crystal is a potential crystal material for realizing broadband tunable blue laser output.
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Keywords:
- Czochralski method /
- crystal growth /
- Ti:MgAl2O4 crystal /
- blue luminescence
[1] 章佶, 孙真荣, 王祖赓, 司继良, 王静雅, 杭寅, 徐军 2005 人工晶体学报 34 657
Google Scholar
Zhang J, Sun Z R, Wang Z G, Si J L, Wang J Y, Hang Y, Xu J 2005 J. Synth. Cryst. 34 657
Google Scholar
[2] Gourier D, Colle L, Lejus A M, Vivein D, Moncorge R 1988 J. Appl. Phys. 63 1144
Google Scholar
[3] 夏海平, 徐铁峰, 张新民, 王金浩, 章践立 2009 光学技术 35 307
Google Scholar
Xia H P, Xu T F, Zhang X M, Wang J H, Zhang J L 2009 Opt. Tech. 35 307
Google Scholar
[4] Basun S A, Danger T, Kaplyanskii A A, McClure D S, Petermann K, Wong W C 1996 Phys. Rev. B 54 6141
Google Scholar
[5] Bausa l E, Vergara I, Garcia-Sole J, Strek W, Deren P J 1990 J. Appl. Phys. 68 736
Google Scholar
[6] Sato T, Shirai M, Tanaka K, Kawabe Y, Hanamura E 2005 J. Lumin. 114 155
Google Scholar
[7] Jouini A, Sato H, Yoshikawa A, Fukuda T 2006 J. Mater. Res. 21 2337
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[8] Kuleshov N V, Shcherbitsky V G, Mikhailov V P, Kiick S, Koetke J, Petermann K, Huber G 1997 J. Lumin. 71 265
Google Scholar
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Google Scholar
[10] Jouini A, Yoshikawa A, Fukuda T, Boulon G 2006 J. Cryst. Growth 293 517
Google Scholar
[11] Lombard P, Boizot B, Ollier N, Jouini A, Yoshikawa A 2009 J. Cryst. Growth 311 899
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[12] Wood D L, Imbusch G F, Macfarlane R M, Kisliuk P, Larkin D M 1968 J. Chem. Phys. 48 5255
Google Scholar
[13] 王成思, 沈锡田, 刘云贵, 张倩 2019 光谱学与光谱分析 39 109
Wang C S, Shen X T, Liu Y G, Zhang Q 2019 Spectrosc. Spect. Anal. 39 109
[14] O'Horo M P, Frisillo A L, White W B 1973 J. Phys. Chem. Solids 34 23
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[15] Takahashi S, Kan A, Ogawa H 2017 J. Eur. Ceram. Soc. 37 1001
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[16] Frass L W, Moore J E, Salzberg J B 1973 J. Chem. Phys. 58 3585
Google Scholar
[17] Simeone D, Dodane-Thiriet C, Gosset D, Daniel P, Beauvy M 2002 J. Nucl. Mater. 300 151
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[18] Dash S, Sahoo R K, Das A, Bajpai S, Debasish D, Singh S K 2017 J. Alloy. Compd. 726 1186
Google Scholar
[19] Watterich A, Hofstaetter A, Wuerz’ R and Scharmann A 1996 Solid State Commun. 100 513
Google Scholar
[20] Jiang Y Q, Halliburton L E, Roth M, Tseitlin M, Angert N, 2007 Physica B 400 190
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[21] Dong S Y, Wang X Y, Shen L F, Li H S, Wang J, Nie P, Wang J J, Zhang X G 2015 J. Electroanal. Chem. 757 1
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图 1 尺寸为Ø30 mm × 70 mm的Ti:MgAl2O4晶体
Figure 1. As-grown Ti:MgAl2O4 crystal with the size of
Ø30 mm × 70 mm. 
图 2 Ti:MgAl2O4晶体的粉末衍射图和MgAl2O4晶体的标准谱图(JCPDS, no. 77-0435)
Figure 2. X-ray diffraction patterns of the as-grown Ti:MgAl2O4 crystal and MgAl2O4 standard patterns (JCPDS, no. 77-0435).
图 3 Ti:MgAl2O4晶体(100)面的摇摆曲线
Figure 3. X-ray rocking curve of (100) plane of the as-grown Ti:MgAl2O4 crystal.
图 4 Ti:MgAl2O4晶体的拉曼谱图
Figure 4. Raman spectra of the as-grown Ti:MgAl2O4 crystal.
图 5 退火前后Ti:MgAl2O4晶体在250−1200 nm范围内的透过光谱
Figure 5. Transmittance spectra of the as-grown Ti:MgAl2O4 crystal before and after annealing in the range of 250−1200 nm.
图 6 退火前后Ti:MgAl2O4晶体在271 nm波长激发下的室温荧光发射光谱
Figure 6. Emission spectra of the as-grown Ti:MgAl2O4 crystal before and after annealing excited by 271 nm at room temperature.
图 7 Ti:MgAl2O4晶体在130 K时的ESR谱
Figure 7. ESR spectrum of the as-grown Ti:MgAl2O4 crystal before and after annealing at 130 K.
图 8 退火前后Ti:MgAl2O4晶体480 nm发射的激发光谱
Figure 8. Excitation spectra of the as-grown Ti:MgAl2O4 crystal before and after annealing with 480 nm as monitoring.
图 9 室温下Ti:MgAl2O4晶体的荧光衰减曲线
Figure 9. Emission decay curve of the as-grown Ti:MgAl2O4 crystal at room temperature.
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[1] 章佶, 孙真荣, 王祖赓, 司继良, 王静雅, 杭寅, 徐军 2005 人工晶体学报 34 657
Google Scholar
Zhang J, Sun Z R, Wang Z G, Si J L, Wang J Y, Hang Y, Xu J 2005 J. Synth. Cryst. 34 657
Google Scholar
[2] Gourier D, Colle L, Lejus A M, Vivein D, Moncorge R 1988 J. Appl. Phys. 63 1144
Google Scholar
[3] 夏海平, 徐铁峰, 张新民, 王金浩, 章践立 2009 光学技术 35 307
Google Scholar
Xia H P, Xu T F, Zhang X M, Wang J H, Zhang J L 2009 Opt. Tech. 35 307
Google Scholar
[4] Basun S A, Danger T, Kaplyanskii A A, McClure D S, Petermann K, Wong W C 1996 Phys. Rev. B 54 6141
Google Scholar
[5] Bausa l E, Vergara I, Garcia-Sole J, Strek W, Deren P J 1990 J. Appl. Phys. 68 736
Google Scholar
[6] Sato T, Shirai M, Tanaka K, Kawabe Y, Hanamura E 2005 J. Lumin. 114 155
Google Scholar
[7] Jouini A, Sato H, Yoshikawa A, Fukuda T 2006 J. Mater. Res. 21 2337
Google Scholar
[8] Kuleshov N V, Shcherbitsky V G, Mikhailov V P, Kiick S, Koetke J, Petermann K, Huber G 1997 J. Lumin. 71 265
Google Scholar
[9] Tomita A, Sato T, Tanaka K, Kawabe Y, Shirai M, Tanaka K, Hanamura E 2004 J. Lumin. 109 19
Google Scholar
[10] Jouini A, Yoshikawa A, Fukuda T, Boulon G 2006 J. Cryst. Growth 293 517
Google Scholar
[11] Lombard P, Boizot B, Ollier N, Jouini A, Yoshikawa A 2009 J. Cryst. Growth 311 899
Google Scholar
[12] Wood D L, Imbusch G F, Macfarlane R M, Kisliuk P, Larkin D M 1968 J. Chem. Phys. 48 5255
Google Scholar
[13] 王成思, 沈锡田, 刘云贵, 张倩 2019 光谱学与光谱分析 39 109
Wang C S, Shen X T, Liu Y G, Zhang Q 2019 Spectrosc. Spect. Anal. 39 109
[14] O'Horo M P, Frisillo A L, White W B 1973 J. Phys. Chem. Solids 34 23
Google Scholar
[15] Takahashi S, Kan A, Ogawa H 2017 J. Eur. Ceram. Soc. 37 1001
Google Scholar
[16] Frass L W, Moore J E, Salzberg J B 1973 J. Chem. Phys. 58 3585
Google Scholar
[17] Simeone D, Dodane-Thiriet C, Gosset D, Daniel P, Beauvy M 2002 J. Nucl. Mater. 300 151
Google Scholar
[18] Dash S, Sahoo R K, Das A, Bajpai S, Debasish D, Singh S K 2017 J. Alloy. Compd. 726 1186
Google Scholar
[19] Watterich A, Hofstaetter A, Wuerz’ R and Scharmann A 1996 Solid State Commun. 100 513
Google Scholar
[20] Jiang Y Q, Halliburton L E, Roth M, Tseitlin M, Angert N, 2007 Physica B 400 190
Google Scholar
[21] Dong S Y, Wang X Y, Shen L F, Li H S, Wang J, Nie P, Wang J J, Zhang X G 2015 J. Electroanal. Chem. 757 1
Google Scholar
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