Bi_（4-x）Nd_xTi_3O_（12）的紫外光辐照化学合成工艺研究
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摘要
本文采用溶胶-凝胶法(Sol-gel)通过紫外光辐照合成了钕掺杂钛酸铋BNT (Bi4-xNdxTi3O12, x=0, 0.25, 0.5, 0.75)粉体和薄膜。通过热重-差热分析(TG-DTA)、X射线衍射(XRD)、扫描电子显微镜(SEM)、原子力显微镜(AFM)等技术手段对Sol-gel法制备的BNT粉体和薄膜进行了表征。
BNT溶胶胶体制备工艺优化过程表明,采用醋酸铋和硝酸钕及钛酸四丁酯为原始组分,乙酸和乙二醇分别为催化剂和溶剂,可获得BNT透明溶胶。在凝胶过程中,经紫外光辐照下制备的BNT(x=0.25)干凝胶粉体,在350-400℃煅烧时主物相是Bi2O3和Bi2O3CO2,而在450℃煅烧处理可获得单一钙钛矿相BNT。紫外光辐照显著地的降低了BNT的晶化温度。研究表明,紫外光辐照促进了凝胶在晶化过程中的化学反应:
通过溶胶-凝胶法在Pt(111)/Ti/SiO2/Si结构的基片上旋涂沉积BNT薄膜,经紫外光辐照的薄膜于300℃除去有机物,后经500℃随炉热处理可得到均匀致密的钙钛矿相BNT薄膜。薄膜平整致密,厚度约为400nm。薄膜择优取向随着Nd掺杂含量的增加趋向于c轴,其中以x=0.5,c轴择优取向最为明显。所得薄膜具有较小的粗糙度,均在2-4nm范围内。铁电性能测试结果表明,剩余极化强度(Pr)和矫顽场(Ec)都随着Nd掺杂比例的增大而减小。
Bi4-xNdxTi3O12(x=0.25, 0.5, 0.75)薄膜的剩余极化值分别为2.75μC/cm2,11.59μC/cm2,10.24μC/cm2,其中钕掺杂量x=0.5的薄膜表现出良好的铁电性能。
With the help of ultraviolet irradiation, the ferroelectric BNT(Bi4-xNdxTi3O12, x=0, 0.25, 0.5, 0.75) powders and thin films were successfully synthesized by a sol-gel method. The crystallization process and structural characteristics of obtained BNT powders and thin films were analyzed by using TG-TDA, XRD, SEM and AFM methods.
The transparent BNT solutions were prepared by using Bi(CH3COO)3 and Nd(NO3)3·5H2O, and Ti(C4H9O)4 as source materials, ethylene alcohol as a solvent and acetic acid (HOAc) as a catalyst. Under the condition of ultraviolet irradiation, the main constitutions of the BNT gel calcined at the range of 350°C to 400°C are Bi2O3 and Bi2O3CO2. The phase-pure BNT with layered pervoskite structure can be obtained at as lower as 450°C. It indicates that the ultraviolet irradiation play a very important role in the crystallization process of the dried gel. It is considered that the ultraviolet irradiation promotes the chemical reactions as follows.
In the case of preparation of BNT thin films, also under the condition of ultraviolet irradiation, the organic matter was burned at 300°C. After the heat-treatment at 500°C, the phase-pure ferroelectric thin films can be synthesized with a dense surface. The typical thickness of the thin films was 400nm. With the increasing of Nd content, the optimal orientation of BNT thin films was adapted to c axis. In particular, the Bi3.5Nd0.5Ti3O12 thin film is more (00l)-orientated than other thin films. Accordingly, the thin films were homogenously, and have small roughness at a level of 2-4 nm. With the change of chemical constitution of Nd and technical conditions, the optimal BNT thin film (x=0.5) has the residual polarization of 11.59μC/cm2, which is good enough for applications in the future.
BNT溶胶胶体制备工艺优化过程表明,采用醋酸铋和硝酸钕及钛酸四丁酯为原始组分,乙酸和乙二醇分别为催化剂和溶剂,可获得BNT透明溶胶。在凝胶过程中,经紫外光辐照下制备的BNT(x=0.25)干凝胶粉体,在350-400℃煅烧时主物相是Bi2O3和Bi2O3CO2,而在450℃煅烧处理可获得单一钙钛矿相BNT。紫外光辐照显著地的降低了BNT的晶化温度。研究表明,紫外光辐照促进了凝胶在晶化过程中的化学反应:
通过溶胶-凝胶法在Pt(111)/Ti/SiO2/Si结构的基片上旋涂沉积BNT薄膜,经紫外光辐照的薄膜于300℃除去有机物,后经500℃随炉热处理可得到均匀致密的钙钛矿相BNT薄膜。薄膜平整致密,厚度约为400nm。薄膜择优取向随着Nd掺杂含量的增加趋向于c轴,其中以x=0.5,c轴择优取向最为明显。所得薄膜具有较小的粗糙度,均在2-4nm范围内。铁电性能测试结果表明,剩余极化强度(Pr)和矫顽场(Ec)都随着Nd掺杂比例的增大而减小。
Bi4-xNdxTi3O12(x=0.25, 0.5, 0.75)薄膜的剩余极化值分别为2.75μC/cm2,11.59μC/cm2,10.24μC/cm2,其中钕掺杂量x=0.5的薄膜表现出良好的铁电性能。
With the help of ultraviolet irradiation, the ferroelectric BNT(Bi4-xNdxTi3O12, x=0, 0.25, 0.5, 0.75) powders and thin films were successfully synthesized by a sol-gel method. The crystallization process and structural characteristics of obtained BNT powders and thin films were analyzed by using TG-TDA, XRD, SEM and AFM methods.
The transparent BNT solutions were prepared by using Bi(CH3COO)3 and Nd(NO3)3·5H2O, and Ti(C4H9O)4 as source materials, ethylene alcohol as a solvent and acetic acid (HOAc) as a catalyst. Under the condition of ultraviolet irradiation, the main constitutions of the BNT gel calcined at the range of 350°C to 400°C are Bi2O3 and Bi2O3CO2. The phase-pure BNT with layered pervoskite structure can be obtained at as lower as 450°C. It indicates that the ultraviolet irradiation play a very important role in the crystallization process of the dried gel. It is considered that the ultraviolet irradiation promotes the chemical reactions as follows.
In the case of preparation of BNT thin films, also under the condition of ultraviolet irradiation, the organic matter was burned at 300°C. After the heat-treatment at 500°C, the phase-pure ferroelectric thin films can be synthesized with a dense surface. The typical thickness of the thin films was 400nm. With the increasing of Nd content, the optimal orientation of BNT thin films was adapted to c axis. In particular, the Bi3.5Nd0.5Ti3O12 thin film is more (00l)-orientated than other thin films. Accordingly, the thin films were homogenously, and have small roughness at a level of 2-4 nm. With the change of chemical constitution of Nd and technical conditions, the optimal BNT thin film (x=0.5) has the residual polarization of 11.59μC/cm2, which is good enough for applications in the future.
引文
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3 S. E. Cummins, L.E.Cross. Crystal Symmetry, Opti-Cal Properties, and Ferroelectric Polarization of Bi4Ti3O12 Single Crystals. Appl Phys Lett. 1967, 10: 14~16
4 P. C. Jochi, S.B.Krupanidhi. Switching, Fatigue, and Retention in Freeoelectric Bi4Ti3O12 Thin Film. Appl Phys Lett. 1993, 62: 1928~1 933
5 T. Kijima, M.Ushikubo, H.Matsunaga. New Low Temperature Processing of Metal-Organic Chemicalvapor Deposition Bi4Ti3O12 Thin Films Using Biobufferlayer. Jpn J Appl Phys. 1999, 38: 127~130
6毛翔宇,陈小兵.高取向Bi4Ti3O12陶瓷样品的制备.扬州大学学报(自然科学版). 2004, 7: 80~84
7 B. E. Watts, F. Leccabue, S. Guerri, C. Morandi. A Comparison of Ti/Pt and TiN/Pt Electrodes Used with Ferroelectric SrBi2Ta2O9 Films. Thin Solid Films. 2002,40: 23-29
8苗鸿雁,李永强,夏傲. Bi4Ti3O12粉体的性能、应用及制备.陕西科技大学学报. 2003, 21: 54~58
9张未涛,孙宏丽,闫正,张子生,赵庆勋,刘保亭.钛酸铋系铁电薄膜的制备及研究进展.河北大学学报(自然科学版). 2006, 26: 219~224
10丁子上,翁文敛.溶胶-凝胶技术制备材料的进展.硅酸盐学报. 1993, 21: 443~446
11李青,黄元龙.溶胶-凝胶法与金属表面改性.电镀与涂饰. 1997, 16: 47~55
12 B. Sonuparlak. Sol-Gel Processing of Infrared Transparent Mullite. Advanced Ceramic Materials. 1988, 3: 263~267
13 B. E. Yoldas. Preparation of Glass and Ceramics From Metal Organic Compounds. J.Mater. Sci. 1977, 12: 1203~1208
14 J. Zarazyoki, S.R.Gurkovich. Sol-Gel Derived PbTiO3. J.Mater. Sci. 1985, 20:4479~4483
15 J. Zarzyoki. Synthesis of Glass From Gels: the Problem of Monolithic Gels. J.Mater. Sci. 1982, 17: 3371~3379
16申林,肖定全,余萍.溶胶-凝胶技术制备(Bi4-La)Ti3O12陶瓷的工艺技术研究.功能材料. 2002, 33: 422~42
17 B. K. Park, B. S. Kang, D.Bus. Lanthanum Substituted Bismuth Titanate for Use in Non-Volatile Memories. Nature. 1999, 401: 682~684
18 C. Uong, K.im.K.Bum, H.M.Jang. Fatigue-Free Samarium-Modified Bismuth Titanate (Bi4-smti3o12) Filmcapacitors Having Large Spontaneous Polarizations. Appl Phys Lett. 2001, 79: 3137~3139
19 M. Hirofmi, I.sachiko, I.takashi. Uniform Field-Induced Strain in A/B-Aes-Oriented Bi3.9Pr0.1Ti3O12 Thick Films on Iro2/Si Substrates for Lead-Free Piezoelectric Microdevice Applications. Appl Phys Lett. 2004, 85: 1220~ 1222
20 J. H. Li, Y.qiao, L.Liu. Microstructure and Ferroelectric Properties of Sol-Gel Derived Bi3.15Nd0.85Ti3O12. Thin Films on Pt/Ti/Sio2/Si(100). Appl Phys Lett. 2004, 85: 3193~3195
21 S. T. Zhang, Y. F. Chen, J. Wang. Ferroelectric Properties of La and Zr Substituted Bi4Ti3O12 Tin Films. Appl Phys Lett. 2004, 84: 3660~3662
22 S. E. Cummins, L. E. Cross. Crystal Symmetry, Optical Properties, and Ferroelectric Polarization of Bi4Ti3O12 Single Crystals. Appl.Phys.Lett. 1967, 10: 14~16
23 B. H. Park, B. S. Kang, Bu.S. D. Lanthanum-Substituted Bismuth Titanate for Use in non-Volatile Memories. Nature (Lon-don). 1999, 401: 682-684
24 H. Wang, M.F.Ren. Low Temperature Synthesis and Ferroelectric Properties of Lasubstituted Bi4Ti3O12 Thin Tilms by Sol–gel Materials Science and Engineering B. 2005, 122: 201~205
25 K. T. Kim, C. I. Kim. Effect of Bi4Ti3O12 Seeding Layer on the Structural and Ferroelectric Properties of Bi3.25La0.75Ti3O12 Thin Films Fabricated by A Metalorganic Decomposition Method. Thin Solid Films. 2004, (447-448): 413~417
26陈敏,刘祖黎.稀土掺杂的钛酸铋铁电材料的研究华中科技大学博士论文. 2004:114
27 L. Zhong, J. B. Wang, Y. C. Zhou. Orientation Dependence of FerroelectricProperties of Pulsed-Laser-AblatedBi4- NdTi3O12 Films. Journal of Crystal Growth. 2002, 89: 2413~2416
28 U. Chon, H. M. Jang, M. G. Kim. Room-Temperature Ferroelectromagnetism in Titanate-Based Layered Perovskites. Phs Rev Lett. 2005, 277: 233~237
29 F. Hou, M. R. Shen, W. W. Cao. Ferroelectric Properties of Neodymium-Doped Bi4Ti3O12 Thin Films Crystallized in Different Environments. Thin Solid Films. 2005, 471: 35~39
30 Z. Garg, H. Barbr, M. Bawber. Leakage Current and Ferroelectric Memory in Nd and Smsubstituted Bi4Ti3O12 Films. Appl Phys Lett. 2003, 83: 2414
31 M. S. Tomar, R. E. Melgarejo. Electrical Properties of Nd-Substituted Bi4Ti3O12 Thin Films fabricated by Chemical Solution Deposition. Microelectronics Journal. 2005, 36: 574~577
32 H. Matsuda, S. Ito, T. Lijima. Design and Ferroelectric Properties of Polar-Ais-Oriented PolycrystallineBi4-xPrTi3O12 Thick Films on Ir?Si Substrates. Appl Phys Lett. 2003, 83:5023~5025
33 U.Chon, J. S. Shim, H.M.Jang. Ferroelectric Properties and Crystal Structure of Praseodymium-Modified Bismuth Titanate. Appl Phys. 2003, 93:4769~4771
34 M. hen, Z. L. Liu, Y. Wang. Ferroelectric Properties of Pr6O11-Doped Bi4Ti3O12. Solid State Communications. 2004,130: 735
35 S. S. Kim, W. J. Kim. Ferroelectric Properties of Randomly Oriented Bi4-PrTi3O12 Thin Films Fabricated by a Sol–Gel Method. Thin Solid Films. 2005, 484: 303~ 309
36 K. T. Lim, K. T. Kim, D. P. Kim. South Korea:IEEE International Conference on Plasma Science. 2003: 403
37 W. J. Kima, S. S. Kima. Ferroelectric Bi3.4Eu0.6Ti3O12 Thin Films Deposited on Si(100)and Pt/Ti/SiO2/Si(100) Substrates by a Sol–Gel Process. Journal of Crystal Growth. 2004, 262: 327~333
38 H. C. Liu, B. Wang, R. Wang, R. Liu. Eparation and Electric Characteristics of Gadolinium-Substituted Bismuth Itanate Ferroelectric Thin Films. Materials Letters. 2007, 61: 457~2459
39 C. Hong, L. B. Wang. Microstructure and Ferroelectric Properties of Dysprosium-Doped Ismuth Titanate Thin Films. Materials Letters. 2007, 61: 2457~2459
40 S. S. Kim, J.S. Songb, S. C. Kwon. Ferroelectric (Bi,Dy)4Ti3O12 Thin Films Deposited on t(111)/Ti/SiO2/Si and P-Type Si(100) Substrates. Journal of Crystal Growth. 2004, 271: 90~98
41 C. Cheng, M. T. Leakage Current and Ferroelectric Memory in Nd and Sm Subtituted Bi4Ti3O12 Films. Materials Letters. 2005, 36: 74~577
42 C. P. Cheng, M. H. Tang. Structure Evolution and Ferroelectric Properties of Bi3.4Yb0.6Ti3O12 Thin Films Crystallized Under a Moderate Temperature. Materials Letters. 2007, 61: 90~98
43 U. Chong, K. B. Kim, H. M. Jang. Fatigue-Free Samarium-Modified Bismuth Titanate Bi4-SmTi3O12 Film Apacitors Having Large Spontaneous Polarizations Appl Phys Lett. 2001, 79: 3137~3139
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47阐艳梅,王佩玲,李永祥,程一兵.工艺参数对熔盐法制备钦酸秘粉体影响的研究.无机材料学报. 2002, 17:1063~1067
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51申林,肖定全,余萍.溶胶-凝胶技术制备(Bi4-La)Ti3O12陶瓷的工艺技术研究.功能材料. 2002, 33: 422~425
2 R. Dat, J. K. Lee, O. Auciello. Pulsed Laser Ablation Synthesis and Characterization of Layered Pt/SrBi2Ta2O9/Pt Ferroelectric Capacitors with Practically No Polarization Fatigue. Appl Phys Lett. 1995, 67: 572~574
3 S. E. Cummins, L.E.Cross. Crystal Symmetry, Opti-Cal Properties, and Ferroelectric Polarization of Bi4Ti3O12 Single Crystals. Appl Phys Lett. 1967, 10: 14~16
4 P. C. Jochi, S.B.Krupanidhi. Switching, Fatigue, and Retention in Freeoelectric Bi4Ti3O12 Thin Film. Appl Phys Lett. 1993, 62: 1928~1 933
5 T. Kijima, M.Ushikubo, H.Matsunaga. New Low Temperature Processing of Metal-Organic Chemicalvapor Deposition Bi4Ti3O12 Thin Films Using Biobufferlayer. Jpn J Appl Phys. 1999, 38: 127~130
6毛翔宇,陈小兵.高取向Bi4Ti3O12陶瓷样品的制备.扬州大学学报(自然科学版). 2004, 7: 80~84
7 B. E. Watts, F. Leccabue, S. Guerri, C. Morandi. A Comparison of Ti/Pt and TiN/Pt Electrodes Used with Ferroelectric SrBi2Ta2O9 Films. Thin Solid Films. 2002,40: 23-29
8苗鸿雁,李永强,夏傲. Bi4Ti3O12粉体的性能、应用及制备.陕西科技大学学报. 2003, 21: 54~58
9张未涛,孙宏丽,闫正,张子生,赵庆勋,刘保亭.钛酸铋系铁电薄膜的制备及研究进展.河北大学学报(自然科学版). 2006, 26: 219~224
10丁子上,翁文敛.溶胶-凝胶技术制备材料的进展.硅酸盐学报. 1993, 21: 443~446
11李青,黄元龙.溶胶-凝胶法与金属表面改性.电镀与涂饰. 1997, 16: 47~55
12 B. Sonuparlak. Sol-Gel Processing of Infrared Transparent Mullite. Advanced Ceramic Materials. 1988, 3: 263~267
13 B. E. Yoldas. Preparation of Glass and Ceramics From Metal Organic Compounds. J.Mater. Sci. 1977, 12: 1203~1208
14 J. Zarazyoki, S.R.Gurkovich. Sol-Gel Derived PbTiO3. J.Mater. Sci. 1985, 20:4479~4483
15 J. Zarzyoki. Synthesis of Glass From Gels: the Problem of Monolithic Gels. J.Mater. Sci. 1982, 17: 3371~3379
16申林,肖定全,余萍.溶胶-凝胶技术制备(Bi4-La)Ti3O12陶瓷的工艺技术研究.功能材料. 2002, 33: 422~42
17 B. K. Park, B. S. Kang, D.Bus. Lanthanum Substituted Bismuth Titanate for Use in Non-Volatile Memories. Nature. 1999, 401: 682~684
18 C. Uong, K.im.K.Bum, H.M.Jang. Fatigue-Free Samarium-Modified Bismuth Titanate (Bi4-smti3o12) Filmcapacitors Having Large Spontaneous Polarizations. Appl Phys Lett. 2001, 79: 3137~3139
19 M. Hirofmi, I.sachiko, I.takashi. Uniform Field-Induced Strain in A/B-Aes-Oriented Bi3.9Pr0.1Ti3O12 Thick Films on Iro2/Si Substrates for Lead-Free Piezoelectric Microdevice Applications. Appl Phys Lett. 2004, 85: 1220~ 1222
20 J. H. Li, Y.qiao, L.Liu. Microstructure and Ferroelectric Properties of Sol-Gel Derived Bi3.15Nd0.85Ti3O12. Thin Films on Pt/Ti/Sio2/Si(100). Appl Phys Lett. 2004, 85: 3193~3195
21 S. T. Zhang, Y. F. Chen, J. Wang. Ferroelectric Properties of La and Zr Substituted Bi4Ti3O12 Tin Films. Appl Phys Lett. 2004, 84: 3660~3662
22 S. E. Cummins, L. E. Cross. Crystal Symmetry, Optical Properties, and Ferroelectric Polarization of Bi4Ti3O12 Single Crystals. Appl.Phys.Lett. 1967, 10: 14~16
23 B. H. Park, B. S. Kang, Bu.S. D. Lanthanum-Substituted Bismuth Titanate for Use in non-Volatile Memories. Nature (Lon-don). 1999, 401: 682-684
24 H. Wang, M.F.Ren. Low Temperature Synthesis and Ferroelectric Properties of Lasubstituted Bi4Ti3O12 Thin Tilms by Sol–gel Materials Science and Engineering B. 2005, 122: 201~205
25 K. T. Kim, C. I. Kim. Effect of Bi4Ti3O12 Seeding Layer on the Structural and Ferroelectric Properties of Bi3.25La0.75Ti3O12 Thin Films Fabricated by A Metalorganic Decomposition Method. Thin Solid Films. 2004, (447-448): 413~417
26陈敏,刘祖黎.稀土掺杂的钛酸铋铁电材料的研究华中科技大学博士论文. 2004:114
27 L. Zhong, J. B. Wang, Y. C. Zhou. Orientation Dependence of FerroelectricProperties of Pulsed-Laser-AblatedBi4- NdTi3O12 Films. Journal of Crystal Growth. 2002, 89: 2413~2416
28 U. Chon, H. M. Jang, M. G. Kim. Room-Temperature Ferroelectromagnetism in Titanate-Based Layered Perovskites. Phs Rev Lett. 2005, 277: 233~237
29 F. Hou, M. R. Shen, W. W. Cao. Ferroelectric Properties of Neodymium-Doped Bi4Ti3O12 Thin Films Crystallized in Different Environments. Thin Solid Films. 2005, 471: 35~39
30 Z. Garg, H. Barbr, M. Bawber. Leakage Current and Ferroelectric Memory in Nd and Smsubstituted Bi4Ti3O12 Films. Appl Phys Lett. 2003, 83: 2414
31 M. S. Tomar, R. E. Melgarejo. Electrical Properties of Nd-Substituted Bi4Ti3O12 Thin Films fabricated by Chemical Solution Deposition. Microelectronics Journal. 2005, 36: 574~577
32 H. Matsuda, S. Ito, T. Lijima. Design and Ferroelectric Properties of Polar-Ais-Oriented PolycrystallineBi4-xPrTi3O12 Thick Films on Ir?Si Substrates. Appl Phys Lett. 2003, 83:5023~5025
33 U.Chon, J. S. Shim, H.M.Jang. Ferroelectric Properties and Crystal Structure of Praseodymium-Modified Bismuth Titanate. Appl Phys. 2003, 93:4769~4771
34 M. hen, Z. L. Liu, Y. Wang. Ferroelectric Properties of Pr6O11-Doped Bi4Ti3O12. Solid State Communications. 2004,130: 735
35 S. S. Kim, W. J. Kim. Ferroelectric Properties of Randomly Oriented Bi4-PrTi3O12 Thin Films Fabricated by a Sol–Gel Method. Thin Solid Films. 2005, 484: 303~ 309
36 K. T. Lim, K. T. Kim, D. P. Kim. South Korea:IEEE International Conference on Plasma Science. 2003: 403
37 W. J. Kima, S. S. Kima. Ferroelectric Bi3.4Eu0.6Ti3O12 Thin Films Deposited on Si(100)and Pt/Ti/SiO2/Si(100) Substrates by a Sol–Gel Process. Journal of Crystal Growth. 2004, 262: 327~333
38 H. C. Liu, B. Wang, R. Wang, R. Liu. Eparation and Electric Characteristics of Gadolinium-Substituted Bismuth Itanate Ferroelectric Thin Films. Materials Letters. 2007, 61: 457~2459
39 C. Hong, L. B. Wang. Microstructure and Ferroelectric Properties of Dysprosium-Doped Ismuth Titanate Thin Films. Materials Letters. 2007, 61: 2457~2459
40 S. S. Kim, J.S. Songb, S. C. Kwon. Ferroelectric (Bi,Dy)4Ti3O12 Thin Films Deposited on t(111)/Ti/SiO2/Si and P-Type Si(100) Substrates. Journal of Crystal Growth. 2004, 271: 90~98
41 C. Cheng, M. T. Leakage Current and Ferroelectric Memory in Nd and Sm Subtituted Bi4Ti3O12 Films. Materials Letters. 2005, 36: 74~577
42 C. P. Cheng, M. H. Tang. Structure Evolution and Ferroelectric Properties of Bi3.4Yb0.6Ti3O12 Thin Films Crystallized Under a Moderate Temperature. Materials Letters. 2007, 61: 90~98
43 U. Chong, K. B. Kim, H. M. Jang. Fatigue-Free Samarium-Modified Bismuth Titanate Bi4-SmTi3O12 Film Apacitors Having Large Spontaneous Polarizations Appl Phys Lett. 2001, 79: 3137~3139
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