低温烧结PZT-PbO·WO_3压电陶瓷性能研究
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摘要
为了降低PZT压电陶瓷的烧结温度,同时提高其综合性能,本论文以固态氧化物为原料,通过添加具有改性作用的低熔点化合物PbO·WO_3,采用一次合成工艺制备PZT-PbO·WO_3压电陶瓷。陶瓷材料在较低温度下实现液相烧结,液相烧结的过程有利于晶粒的致密化,提高材料的体积密度。实验主要研究PbO·WO_3含量、准同型相界附近锆含量对陶瓷介电性能、压电性能、居里温度的影响,然后在此基础上进行了烧结温度、保温时间、极化工艺对材料性能影响的研究。粉末在900℃合成并保温2h,得到钙钛矿结构。研究发现:PbO·WO_3最佳掺杂量为0.5% , Zr含量为52%时材料处于准同型相界内;Pb_(1.05)(Zr_(0.52)Ti_(0.48))O_3- 0.5mol%(5PbO·WO_3)压电陶瓷在1100℃保温时间为2小时条件下烧结而成,在120℃硅油中,2500V/mm场强下持续极化30分钟,样品达最佳性能。测得的最佳性能参数为:介电常数ε33T/ε0=1593,介电损耗tanδ=0.019,压电系数d_(33)=363PC/N ,机电耦合系数KP=0.60,机械品质因数Qm=66,电阻率ρ_v=5.65×10~(12)Ω·cm,居里温度T_c=361-367℃。通过和传统温度(1260℃)下烧结而成的PZT压电陶瓷综合性能的比较,本实验不仅降低了其烧结温度,而且提高了材料的综合性能。论文后期对陶瓷的低温液相烧结和改性原理进行了深入地探讨。
本文通过X射线衍射(XRD)对合成后材料的晶相进行了分析;用扫描电子显微镜(SEM)观察样品表面的显微结构。
In order to abate the sintered temperature of piezoelectric ceramics and improve its complex capability, the material is doped by low melting point chemical compound PbO·WO3.As a result, ceramic materials can be sintered at 1100℃in liquid phase. This process is in favor of improving the densification of grain. In the paper, PZT-0.5%PbO·WO3 piezoelectric ceramic were prepared by using one-stage technique with solid oxides as raw materials. The effects of PbO·WO_3 contents, Zr contents, sintering temperature, soaking time and polarize technology on properties of ceramic was studied. The results showed that pure perovskitic structure was obtained at calcination of 900℃for 2h. It exhibited a well-situated property at morphotropic phase boundary when Zr content is 0.52 and PbO·WO_3 content is 0.5mol%. Pb_(1.05)(Zr_(0.52),Ti_(0.48))O_3-0.5mol%(5PbO·WO_3) piezoelectric ceramic is sintered at 1110℃for 2h and polarized under 2500V/mm of electric field in 120℃for 30min.The optimized results ofε33T/ε0 (1593),tanδ(0.019),d33 (363PC/N), Kp (0.60),Qm (66),ρv(5.65×1012Ω·cm) and Tc(361-367℃) were obtained. In comparison of the properties of PZT sintered at traditional temperature(1260℃), this experiment abate the sintering temperature and improve its complex capability. In the final paper, there have a profound research on the principle of low temperature sintering and improving properties.
In the paper, XRD is used to analyze the lattice structure of synthetic power, SEM is used to observe the surface of the ceramic.
本文通过X射线衍射(XRD)对合成后材料的晶相进行了分析;用扫描电子显微镜(SEM)观察样品表面的显微结构。
In order to abate the sintered temperature of piezoelectric ceramics and improve its complex capability, the material is doped by low melting point chemical compound PbO·WO3.As a result, ceramic materials can be sintered at 1100℃in liquid phase. This process is in favor of improving the densification of grain. In the paper, PZT-0.5%PbO·WO3 piezoelectric ceramic were prepared by using one-stage technique with solid oxides as raw materials. The effects of PbO·WO_3 contents, Zr contents, sintering temperature, soaking time and polarize technology on properties of ceramic was studied. The results showed that pure perovskitic structure was obtained at calcination of 900℃for 2h. It exhibited a well-situated property at morphotropic phase boundary when Zr content is 0.52 and PbO·WO_3 content is 0.5mol%. Pb_(1.05)(Zr_(0.52),Ti_(0.48))O_3-0.5mol%(5PbO·WO_3) piezoelectric ceramic is sintered at 1110℃for 2h and polarized under 2500V/mm of electric field in 120℃for 30min.The optimized results ofε33T/ε0 (1593),tanδ(0.019),d33 (363PC/N), Kp (0.60),Qm (66),ρv(5.65×1012Ω·cm) and Tc(361-367℃) were obtained. In comparison of the properties of PZT sintered at traditional temperature(1260℃), this experiment abate the sintering temperature and improve its complex capability. In the final paper, there have a profound research on the principle of low temperature sintering and improving properties.
In the paper, XRD is used to analyze the lattice structure of synthetic power, SEM is used to observe the surface of the ceramic.
引文
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[4] Tao Li, Adam M.Scotch and Helen M.Chan, Single crystals of Pb(Mg1/3Nb2/3)O3- 35mol%PbTiO3 from polycrystalline precursors, Ferroelectrics,2000,27[3] 49-57
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[7] 高春华,黄新友. 稀土氧化物在功能陶瓷中的应用分析. 陶瓷科学与艺术, 2002, 114(16)
[8] Fu Jan( 傅 剑 ), Li Cheng’en( 李 承 恩 ), et al. Progress in research on low-temperature sintering of PZT piezoelectric ceramics [J]. Materials Review(材料导报), 2000; 14(1): 38~40
[9] 周桃生,彭炜,等. 低温烧结压电陶瓷及其应用[J].湖北大学学报, 2000,22(1):49~53
[10] D. L. Corker, R. W. Whatmore, et al. Liquid-phase sintering of PZT ceramics[J]. Journal of the European ceramic society, 2000; 20: 2039~2045
[11] E. R. Nielsen, E. Ringgaard, M. Kosec. Liquid-phase sintering of Pb(Zr, Ti)O3 using PbO-WO3 additive[J]. Journal of the European ceramic society, 2002; 22: 1847~1855
[12] Nathalie Texier, Christian Courtois, et al. Powder process influence on the characteristics of Mn, W, Sb, Ni-doped PZT[J]. Journal of the European ceramic society, 2001; 21: 1499~1502
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[15] 李景德,邓人忠,压电陶瓷中的空间电荷,无机材料学报,1998,13[2]:167-170.
[16] 刘梅冬,许毓春,压电铁电材料与器件,武汉:华中理工大学出版社 1992
[17] 严继康,甘国友,孙加林等,串联 2-2 型复合材料的进一步研究,压电与声光,2000,22[4] 262-265
[18] 严继康,张建成,陈杰等,串联 2-2 型复合材料的介电和压电性,压电与声光,1998,20[6]: 428-431
[19] K.Sumi,H. Qiu and H. Kamei.Structural,compositional and piezoelectric properties of the Sol-Gel Pb(Zr0.56Ti0.44)0.80(Mg1/3Nb2/3)O3/ Pb(Zr0.56Ti0.44)0.80 composite films,Thin Solid Films,1999 [349]: 270-275
[20] 张勇,李龙土,桂治轮等,压电复合材料,压电与声光,1997,19[2]: 130-134
[21] 邹小平,良莹,姚熹等,压电复合材料 PT-P(VDF/TeFE)的静水压压电性,压电与声光,1996,18[5] :346-348
[22] G.H.Hertling,C.E.Land ,Hot Pressed PLZT Ferroelectric Ceramics for Electro-optic Applications,J.Am.Ceram.Soc,1971 54[1] :1-11
[23] B.Stojanovic,M.Kosec,J.Pirs, Application of PLZT Ceramics foe Ekectro- optic Shutters,Ceramics for Electronics ,Part II,Pardubice Pardubice,1988:205-209
[24] S.R.Shannigrahi,R.N.P.Choudhary,H.N.Acharya,Synthesis and characterization of cesium doped PLZT(8/60/64)ceramics,Materials Chemistry and physics ,1999 (58):204-211
[25] B.D.Stojanovic C.R.Foschini and M.Cilense.,Structural characterization of organometallic-derived 9.5/65/35 PLZT ceramics,Materials Chemistry and Physics,2001[68]:136-141
[26] Ahmed Boutarfaia, Study of solid state reaction and the morphotropic phase boundary in Pb(Zr,Ti)O3-Pb(Fe1/5,Ni1/5,Sb3/5)O3 ceramics,Ceramics International , 2001, 27 ,91-97
[27] Jaffe B,Cook W R,Jaffe h Piezoelectric Ceramics,New York:Academi Press,1971
[28] Gupta,S.M.and Viehland,D,Tetragonal to rhombohedral transformation in the lead zirconium titanate lead magnesium niobate-lead titanate crystalline solution. J.Appl.Phys,1998 83[1] 407-414
[29] Isopov.V.A.Characteristics of coexistence of tetragonal rhombohedral phases in piezoelectric ceramics based on PbTiO3 and PbZrO3.Soy.Phys.Solid State,1976, 18[4]:529-532
[30] Mabud,S.A.The morphotropic phase boundary in PZT solid solutions,J.Appl. Cryst,1980,13.211-216
[31] 李全禄,压电与压磁声电转换材料的研究与应用,压电与声光,1995,17[2]:43-51
[32] 董敦妁,陈旭明等.低温烧结 PZT 压电陶瓷材料.电子元件与材料.1980,(81):58
[33] 姚熹.《精细功能陶瓷动态与展望》.西安交通大学出版社,1991.
[34] Sadayuki Takahashi. Sintering Pb(Zr,Ti)O3 ceramics at low temperature Jpn J Applphys,1980,19(4):771
[35] D.E 。 Wittmer and R.C.Buchanan. Low-temperature densification of lead zirconate titanate with vanadium pentoxide additive. J Am Ceram Soc,1981, 64(8):485
[36] S.Y.Cheng, S.L.Fu,et al. Theproperties of low-temperature fired piezoelectric ceramics. J Mater Sci,1986,21:571
[37] 柴京鹤,李龙土等.低温烧结 PZT 压电陶瓷的研究.清华大学学报(自然科学版),1988,28(3):1
[38] Gui Zhilun, Li Longtu, et al. Low temperature sintering of lead magnesium nickel niobate zirconate titanate piezoelectric ceramic with high performances. Ferroelectrics,1990,101:93
[39] Gui Zhilun, Li Longtu, et al. Low temperature sintering of lead-based piezoelectric ceramics. J Am Ceram Soc,1989,72(3):486
[40] 江迎鹤,熊茂仁等.PZT-BF-MCX 系压电陶瓷的烧结和电性能.电子元件与材料,1992,11(3):19
[41] S.L.Swartz, T.R.Shrout, et al. Dielectric properties of lead magnesium niobate ceramics. J Am Ceram Soc,1984,67(1):2
[42] K.Kakegawa, J.Mohri, et al. Prepation of Pb(Zr,Ti)O3 by oxalate method in ethanol solution. J Ceram Soc Jpn,1986,94:470
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