无籽固相生长工艺制备KNN基无铅压电单晶
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摘要
采用无籽固相生长技术,成功制备了低含量LiBiO_3(LB)掺杂的K_(0.5)Na_(0.5)NbO_3(KNN)单晶,并系统地研究LB的掺杂量和烧结工艺(烧结温度、保温时间)对KNN晶体生长行为的影响。研究结果表明:在较窄的烧结温度范围内,通过在KNN基陶瓷中引入微量的LB,可以从基体中成功获得大的KNN单晶颗粒;当在同一烧结温度和相同保温时间条件下,随着LB掺杂量的增加,KNN陶瓷基体的晶体异常长大的转化面积逐渐减少;当样品的成分和烧结温度相同时,延长保温时间,晶粒可以继续长大。所生长的铌酸钾钠单晶最大一维尺寸达到厘米级。掺杂量为0.45at%的KNN晶体的结构和电学性能被测试分析,结果表明:所制备的KNN晶体的综合性能高于目前大部分采用的布里奇曼法、顶部籽晶生长法、浮区法等溶液/熔体法生长的KNN晶体,具有极大的潜在应用价值。
K_(0. 5)Na_(0. 5)NbO_3( KNN) single crystals were successfully prepared by a seed-free solidstate growth method with low content of LiBiO_3( LB) as a sintering aid. The effects of LB doping content and sintering process including the dwelling temperature and time on the growth behavior of KNN single crystal were systematically studied. The research results show that within a narrow sintering temperature range,KNN single crystal grains can be successful obtained by doping low content of LB in the ceramic matrix. Under the same sintering temperature and holding time,the crystallization area of the KNN single crystals in the ceramic matrix gradually reduces with the increasing of LBcontent. For the samples with the same composition and sintering temperature,prolonging the dwelling time can make single crystal grain to continue growing. The largest size of KNN single crystal can reach centimeter-scale. In addition,the microstructure and electrical properties of KNN- 0. 45 at%LB single crystal were tested and analyzed. The comprehensive performance of KNN crystal prepared by seed-free solid-state growth method is higher than that of many KNN crystals prepared by other methods such as the solution or melt growth methods,including the Bridgman,the top-seeded solution growth,the floating zone method. This research shows that the KNN single crystal present in this paper has a great promising application in many relative devices.
K_(0. 5)Na_(0. 5)NbO_3( KNN) single crystals were successfully prepared by a seed-free solidstate growth method with low content of LiBiO_3( LB) as a sintering aid. The effects of LB doping content and sintering process including the dwelling temperature and time on the growth behavior of KNN single crystal were systematically studied. The research results show that within a narrow sintering temperature range,KNN single crystal grains can be successful obtained by doping low content of LB in the ceramic matrix. Under the same sintering temperature and holding time,the crystallization area of the KNN single crystals in the ceramic matrix gradually reduces with the increasing of LBcontent. For the samples with the same composition and sintering temperature,prolonging the dwelling time can make single crystal grain to continue growing. The largest size of KNN single crystal can reach centimeter-scale. In addition,the microstructure and electrical properties of KNN- 0. 45 at%LB single crystal were tested and analyzed. The comprehensive performance of KNN crystal prepared by seed-free solid-state growth method is higher than that of many KNN crystals prepared by other methods such as the solution or melt growth methods,including the Bridgman,the top-seeded solution growth,the floating zone method. This research shows that the KNN single crystal present in this paper has a great promising application in many relative devices.
引文
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[2]ZHANG S J,LI F.High performance ferroelectric relaxor-PbTiO3single crystals:Status and perspective[J].Journal of Applied Physics,2012,111(031301):1-50.
[3]张利民,张波萍,李敬锋,等.无铅压电陶瓷铌酸钾钠的常压烧结及其电学性能[J].硅酸盐学报,2007,35(1):1-5.
[4]孙勇,肖定全,吴浪,等.铌酸钾钠基无铅压电陶瓷制备技术新进展[J].功能材料,2007,38(8):1225-1228.
[5]CHEN K,XU G S,YANG D F,et al.Dielectric and piezoelectric properties of lead-free 0.95(K0.5Na0.5)NbO3-0.05LiNbO3crystals grown by the Bridgman method[J].Journal of Applied Physics,2007,101(044103):1-4.
[6]INAGAKI Y,KAKIMOTO K,KAGOMIYA I.Crystal growth and ferroelectric property of Na0.5K0.5NbO3and Mn-doped Na0.5K0.5NbO3crystals grown by floating zone method[J].Journal of The European Ceramic Society,2010,30(2):301-306.
[7]TIAN H,HU C P,MENG X D,et al.Top-seeded solution growth and properties of K1-xNaxNbO3crystals[J].Crystal Growth&Design,2015,15(3):1180-1185.
[8]SARAVANAN R,RAJESH D,RAJASEKARAN S V,et al.Crystal structure,dielectric properties of(K0.5Na0.5)Nb O3single crystal grown by flux method using B2O3flux[J].Crystal Research and Technology,2013,48(1):22-28.
[9]KANG S J,PARK J H,KO S Y,et al.Solid-state conversion of single crystals:The principle and the state of the art[J].Journal of The American Ceramic Society,2015,98(2):347-360.
[10]FISHER J G,BENCAN A,GODNJACEC J,et al.Growth behaviour of potassium sodium niobate single crystals grown by solid-state crystal growth using K4Cu Nb8O23as a sintering aid[J].Journal of The European Ceramic Society,2008,28(8):1657-1663.
[11]江民红,刘心宇,邓满姣,等.铌酸钾钠织构陶瓷与铌酸钾钠单晶的制备方法[P].中国:发明专利,201010247474.8.
[12]JIANG M H,RANDALL C A,GUO H Z,et al.Seed-free solid-state growth of large lead-free piezoelectric single crystals:(Na1/2K1/2)Nb O3[J].Journal of The American Ceramic Society,2015,98(10):2988-2996.
[13]KIZAKI Y,NOGUCHI Y,MIYAYAMA M.Defect control for low leakage current in K0.5Na0.5NbO3single crystals[J].Applied Physics Letters,2006,89:142910.
[14]WILLIAM D C.Materials Science and Engineering:An Introduction[M].New York:John Wiley&Sons Inc,2012.
[15]HURELE D T J.Handbook of Crystal Growth,Fundamentals,Part A,Thermodynamics and Kinetics[M].Amsterdam:Elsevier Science Publishers,1993.
[16]明保全,王矜奉,臧国忠,等.铌酸钾钠基无铅压电陶瓷的X射线衍射与相变分析[J].物理学报,2008,57(9):5962-5967.
[17]GUPTA S,PRIYA S.Ferroelectric properties and dynamic scaling of 100 oriented(K0.5Na0.5)Nb O3single crystals[J].Applied Physics Letters,2011,98(242906):1-3.