X切铌酸锂晶体铁电畴反转工艺研究

doi:10.19964/j.issn.1006-4990.2024-0670

摘要/Abstract

摘要：

铌酸锂晶体因其优异的电光、声光、热释电、压电及非线性光学特性，在多个领域具有广泛应用。以X切向铌酸锂晶体为研究对象，系统地开展了外加脉冲电场诱导铁电畴反转的实验研究，重点探讨实验过程中所遇到的工艺上的问题（极化不成功、电极粘附力差、光刻胶难以剥离）及畴反转质量的影响因素。铁电畴反转的成功率及质量受电场强度、极化次数和电极条件等多重因素共同影响。实验结果表明：选择Cr电极和优化磁控溅射功率（20 W）、沉积速率（12 nm/min），可解决电极粘附力弱的问题；使用稀释的二甲基亚砜剥离溶液取代丙酮，成功剥离光刻胶，得到理想电极图案；通过沿Z向施加极化电压，在410 V外加电压和4次重复极化周期下，畴结构反转完全、反转畴质量最好。通过建立优化的工艺参数体系，提升了畴反转的重复性和稳定性，有望推动其在光电器件、声波器件等领域的更广泛应用。

关键词: X切铌酸锂, 畴反转, 畴工程, 外加电场

Abstract:

Lithium niobate crystals are extensively applied in multiple fields，due to their excellent electro-optic，acousto-optic，pyroelectric，piezoelectric，and nonlinear optical properties.In this study，X-cut lithium niobate crystals were taken as the research object，and an experimental study on ferroelectric domain inversion induced by an external pulsed electric field was systematically carried out.The process issues encountered during the experiment（unsuccessful polarization，poor electrode adhesion，and difficulty in peeling off photoresist） and the factors affecting the quality of domain inversion were extensively discussed.The success rate and quality of ferroelectric domain inversion were jointly affected by multiple factors such as electric field strength，polarization times，and electrode conditions.The experimental results showed that selecting the Cr electrode and optimizing the magnetron sputtering power（20 W） and deposition rate（12 nm/min） solved the problem of weak electrode adhesion.Replacing acetone with a diluted dimethyl sulfoxide（DMSO） stripping solution successfully stripped the photoresist，resulting in an ideal electrode pattern.By applying a polarization voltage along the Z-direction，under an external voltage of 410 V and 4 repeated polarization cycles，the domain structure inversion was complete and the inverted domain quality was the best.By establishing an optimized process parameter system，the repeatability and stability of domain inversion were improved，which was expected to promote its wider application in optoelectronic devices，acoustic wave devices，and other fields.

Key words: X-cut lithium niobate, domain inversion, domain engineering, external electric field

中图分类号:

O487

陈宇能, 唐供宾, 陈昆峰, 薛冬峰. X切铌酸锂晶体铁电畴反转工艺研究[J]. 无机盐工业, 2025, 57(11): 31-35.

CHEN Yuneng, TANG Gongbin, CHEN Kunfeng, XUE Dongfeng. Study on ferroelectric domain inversion in X-cut lithium niobate crystals[J]. Inorganic Chemicals Industry, 2025, 57(11): 31-35.

图/表 9

图1

表1

图2

表2

图3

图4

图5

图6

图7

参考文献 30

[1]	CHEN Kunfeng， LI Yanlu， PENG Chao，et al.Microstructure and defect characteristics of lithium niobate with different Li concentrations［J］.Inorganic Chemistry Frontiers，2021，8（17）：4006-4013.
[2]	LIU Feng， CHEN Kunfeng， XUE Dongfeng.How to fast grow large-size crystals［J］.The Innovation，2023，4（4）：100458.
[3]	BOES A， CHANG Lin， LANGROCK C，et al.Lithium niobate photonics：Unlocking the electromagnetic spectrum［J］.Science，2023，379（6627）：eabj4396.
[4]	WU T H， LEDEZMA L， FREDRICK C，et al.Visible-to-ultraviolet frequency comb generation in lithium niobate nanophotonic waveguides［J］.Nature Photonics，2024，18（3）：218-223.
[5]	史国强，陈昆峰，唐供宾，等.铌酸锂晶体缺陷研究中的介尺度团簇演变［J］.硅酸盐学报，2023，51（6）：1425-1438.
	SHI Guoqiang， CHEN Kunfeng， TANG Gongbin，et al.Evolution of mesoscale clusters in study of defects in lithium niobate crystals［J］.Journal of the Chinese Ceramic Society，2023，51（6）：1425-1438.
[6]	YU Mengjie， CHENG R， REIMER C，et al.Integrated electro-optic isolator on thin-film lithium niobate［J］.Nature Photonics，2023，17（8）：666-671.
[7]	陈宇能，陈昆峰，薛冬峰.铌酸锂晶体铁电畴调控及器件应用研究进展［J］.无机盐工业，2024，56（6）：1-13.
	CHEN Yuneng， CHEN Kunfeng， XUE Dongfeng.Research progress of preparation and device application of lithium niobate crystal ferroelectric domain［J］.Inorganic Chemicals Industry，2024，56（6）：1-13.
[8]	WANG Wenjia， ZHU Yunzhong， WANG Biao.Interface diagnostics：In-situ prediction of constitutional supercooling and backmelting by growth interface electromotive force［J］.Materials & Design，2023，232：112070.
[9]	ZHENG Weitao， ZHU Yunzhong， JIANG Xianlong，et al.Interface diagnostics：Equivalent circuit characterization for a growing bulk single crystal［J］.Crystal Growth & Design，2024，24（23）：10046-10053.
[10]	郑远林，陈险峰.薄膜铌酸锂集成非线性光学：走向全光信息时代的新路径［J］.物理，2024，53（1）：22-32.
	ZHENG Yuanlin， CHEN Xianfeng.Integrated nonlinear photonics on thin-film lithium niobate：A route to an all-optical information era［J］.Physics，2024，53（1）：22-32.
[11]	HONG Lihong， QIU Yating， LI Xiaoni，et al.Analytical solution to incident angle quasi-phase-matching engineering for second har-monic generation in a periodic-poled lithium niobate crystal［J］.Chinese Physics B，2024，33（2）：020301.
[12]	YANG Fengyan， LU Juanjuan， SHEN Mohan，et al.Symmetric second-harmonic generation in sub-wavelength periodically poled thin film lithiumniobate［J］.Optica，2024，11（8）：1050-1055.
[13]	THIELE F， BRUCH F VOM， QUIRING V，et al.Cryogenic electro-optic polarisation conversion in titanium in-diffused lithium niobate waveguides［J］.Optics Express，2020，28（20）：28961-28968.
[14]	RAMBU A P， TIRON V， ONICIUC E，et al.Spontaneous polarization reversal induced by proton exchange in Z-cut lithium niobate α-phase channel waveguides［J］.Materials，2021，14（23）：7127.
[15]	LIU Qilu， WANG Fulei， WANG Dongzhou，et al.Temperature dependent domain-wall moving dynamics of lithium niobate during high electric field periodic poling［J］.Journal of Applied Physics，2020，128（22）：224101.
[16]	XU Xiaoyi， WANG Tianxin， CHEN Pengcheng，et al.Femtosecond laser writing of lithium niobate ferroelectric nanodomains［J］.Nature，2022，609（7927）：496-501.
[17]	QIAN Yuezhao， ZHANG Ziqing， LIU Yuezhou，et al.Graphical direct writing of macroscale domain structures with nanoscale spatial resolution in nonpolar-cut lithium niobate on insulators［J］.Physical Review Applied，2022，17（5）：054049.
[18]	KOKHANCHIK L S， EMELIN E V， SIROTKIN V V.Morphology features of ferroelectric submicron domains written by E-beam under a metal film in LiNbO₃ ［J］.Coatings，2022，12（12）：1881.
[19]	ZHAO Jie， RÜSING M， ROEPER M，et al.Poling thin-film X-cut lithium niobate for quasi-phase matching with sub-micrometer periodicity［J］.Journal of Applied Physics，2020，127（19）：193104.
[20]	QIN Zhenhui， YAN Hao， HAO Chenbei，et al.Double-layer LiNbO₃ longitudinally excited shear wave resonators with ultra-large electromechanical coupling coefficient and spurious-free performance［J］.Applied Physics Letters，2025，126（19）：193503.
[21]	LIU Peisen， FU Sulei， SU Rongxuan，et al.A near spurious-free 6 GHz LLSAW resonator with large electromechanical coupling on X-cut LiNbO₃/SiC bilayer substrate［J］.Applied Physics Letters，2023，122（10）：103502.
[22]	SUN Dehui， ZHANG Yunwu， WANG Dongzhou，et al.Microstructure and domain engineering of lithium niobate crystal films for integrated photonic applications［J］.Light：Science & Applications，2020，9：197.
[23]	BOES A， CORCORAN B， CHANG Lin，et al.Status and potential of lithium niobate on insulator（LNOI） for photonic integrated circuits［J］.Laser & Photonics Reviews，2018，12（4）：1700256.
[24]	周秀敏.近化学计量比铌酸锂晶体生长及准相位匹配器件研究［D］.哈尔滨：哈尔滨工业大学，2010。
	ZHOU Xiumin.Study of the growth of near stoichiometric lithium niobate crystal and quasi-phase matching component［D］.Harbin：Harbin Institute of Technology，2010.
[25]	ZHANG Honghu， ZHU Houbin， LI Qingyun，et al.Reversed domains in x-cut lithium niobate thin films［J］.Optical Materials，2020，109：110364.
[26]	ZHANG Honghu， LI Qingyun， ZHU Houbin，et al.Optimization of periodic poling of x-cut lithium niobate thin film［J］.Optical Materials，2022，131：112562.
[27]	张煜晨，李三兵，许京军，等.铌酸锂导电畴壁及其应用［J］.人工晶体学报，2024，53（3）：395-409.
	ZHANG Yuchen， LI Sanbing， XU Jingjun，et al.Conductive domain wall and its applications in lithium niobate［J］.Journal of Synthetic Crystals，2024，53（3）：395-409.
[28]	LEE D， GOPALAN V， PHILLPOT S R.Depinning of the ferroelectric domain wall in congruent LiNbO₃ ［J］.Applied Physics Letters，2016，109（8）：082905.
[29]	MILLER G D.Periodically poled lithium niobate：Modeling，fabrication，and nonlinear optical performance［M］.Redwood City：Stanford University，1998.
[30]	KURODA A， KURIMURA S， UESU Y.Domain inversion in ferroelectric MgO：LiNbO₃ by applying electric fields［J］.Applied Physics Letters，1996，69（11）：1565-1567.

首页

全国无机盐信息中心

中国化工学会

无机酸碱盐专业委员会