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CN101718810B - Method for measuring ferroelectric hysteresis loop of leakage ferroelectric film - Google Patents

Method for measuring ferroelectric hysteresis loop of leakage ferroelectric film Download PDF

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CN101718810B
CN101718810B CN200910199381XA CN200910199381A CN101718810B CN 101718810 B CN101718810 B CN 101718810B CN 200910199381X A CN200910199381X A CN 200910199381XA CN 200910199381 A CN200910199381 A CN 200910199381A CN 101718810 B CN101718810 B CN 101718810B
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江安全
刘骁兵
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Abstract

本发明属于固态电介质性能测试技术领域,具体为一种测量漏电铁电薄膜电滞回线的方法。本发明方法首先在漏电极化的铁电薄膜上施加同极性的外加电压,测定并记录薄膜两端不同电压下通过铁电薄膜的漏电流,经曲线拟合,得到漏电流和施加电压的函数方程,进而计算得到电畴翻转的极化电流随时间的变化关系。最后将位移电流对时间积分,计算出该外加电压下铁电薄膜产生的位移电荷密度。重复以上的测量和计算过程,得到该铁电薄膜的不同电压下所对应的电位移,从而测得整个漏电铁电薄膜的电滞回线。本发明解决了漏电铁电薄膜电学表征的难题,特别是为超薄铁电漏电薄膜电学性能研究提供了有力手段。

Figure 200910199381

The invention belongs to the technical field of solid-state dielectric performance testing, in particular to a method for measuring the hysteresis loop of a leakage ferroelectric thin film. In the method of the present invention, firstly, an applied voltage of the same polarity is applied on the drain polarized ferroelectric thin film, the leakage current passing through the ferroelectric thin film under different voltages at both ends of the thin film is measured and recorded, and the leakage current and the applied voltage are obtained through curve fitting. The function equation is used to calculate the variation relationship of the polarization current of the domain flipping with time. Finally, the displacement current is integrated with time, and the displacement charge density generated by the ferroelectric film under the applied voltage is calculated. Repeat the above measurement and calculation process to obtain the corresponding electric displacement of the ferroelectric thin film under different voltages, so as to measure the hysteresis loop of the entire leakage ferroelectric thin film. The invention solves the difficult problem of electrical characterization of the leakage ferroelectric thin film, and especially provides a powerful means for the research on the electrical properties of the ultra-thin ferroelectric leakage thin film.

Figure 200910199381

Description

一种测量漏电铁电薄膜电滞回线的方法A Method for Measuring the Hysteresis Loop of Leakage Ferroelectric Thin Film

技术领域 technical field

本发明属于固态电介质性能测试技术领域,具体涉及漏电铁电薄膜电滞回线的测试方法。The invention belongs to the technical field of solid-state dielectric performance testing, and in particular relates to a testing method for a hysteresis loop of a leakage ferroelectric film.

背景技术 Background technique

铁电薄膜材料具有较高的自发极化强度和较大的介电常数可应用于非挥发随机读取存储器(FRAM)、动态随机读取存储器(DRAM)、非制冷红外探测器、薄膜介质电容器、电场调制的微波器件、AC电致发光器件和薄膜传感器等。随着器件集成密度的提高,器件单元尺寸大幅缩小,接近了原子或分子水平,预计未来的FRAM和DRAM的存储密度可达~Tb/in2量级,接近目前运用垂直技术制造的磁记录硬盘水平。Ferroelectric thin film materials have high spontaneous polarization and large dielectric constant and can be applied to non-volatile random access memory (FRAM), dynamic random access memory (DRAM), uncooled infrared detectors, thin film dielectric capacitors , microwave devices modulated by electric field, AC electroluminescent devices and thin film sensors, etc. With the improvement of device integration density, the device unit size has been greatly reduced, approaching the atomic or molecular level. It is expected that the storage density of FRAM and DRAM in the future will reach the order of ~Tb/in 2 , which is close to the current magnetic recording hard disk manufactured by vertical technology. level.

漏电铁电薄膜电学测量上的困难源于薄膜局部区域处的缺陷、空洞或薄膜的不连续性生长,如岛状、棒状等,导致整个薄膜的漏电或平行板电容器上下电极间的短路,使得目前典型的商用铁电测试仪如Radiant PremierI/II和aixACCT TF2000analyzer等对这些漏电薄膜的电学表征无能为力,开发必要的新型铁电测试技术对超薄薄膜的电学研究尤为迫切。随着市场的发展和微电子器件集成度的提高,器件的尺寸按摩尔定律以每2年缩小1倍的速度高速发展,逐步逼近原子或分子的水平,如目前Intel公司正在研究开发的16纳米尺寸以下的MOS器件和我国“十一五”期间启动的“极大规模集成电路装备和成套工艺”重大专项中22nm以下功能器件的研究计划都是朝着这个目标迈进。因此,积极发展先进的薄膜测试技术从市场应用角度上考虑也非常紧迫。着手原子层量级的铁电薄膜生长的研究对于电畴成核和生长的动力学理论的发展也具有积极意义。从理论上看,电畴的翻转是从形成临界尺寸的反向子核开始,最初源于薄膜的表面或缺陷的聚积区。最新的密度泛函(DFT)计算给出,这种临界子核的尺寸约为三个单胞的数量级,也就是说只有那些大于该尺寸的子核才会对电畴的翻转有贡献。但是,当薄膜的厚度逼近或低于这种临界尺寸时,其翻转机理必有所不同,对其机理的认识人们目前还很不清楚,影响了器件功能的进一步开发。另外,随着膜厚的减小,量子隧穿电流相应增加。一方面,这种隧穿电流会随着电畴的重新取向而发生变化,可运用于高密度FRAM存储单元中逻辑信号的非破坏性读取,具有积极意义;另一方面,它也进一步提高了漏电流,加深了薄膜电学测量上的困难。也就是说,即使我们能够生长出完美无缺的薄膜晶体,也不可能利用现有的商业设备完成这些薄膜的电学表征。因而,本发明所设计的漏电铁电薄膜测试方法以及应用这一原理设计的漏电铁电薄膜电学性能测试系统为铁电薄膜材料的研究和应用提供了有力的工具。The difficulty in the electrical measurement of leakage ferroelectric thin films stems from the defects, cavities, or discontinuous growth of the thin film in the local area of the thin film, such as islands, rods, etc., which lead to the leakage of the entire thin film or the short circuit between the upper and lower electrodes of the parallel plate capacitor, making Currently typical commercial ferroelectric testers such as Radiant PremierI/II and aixACCT TF2000analyzer are powerless for the electrical characterization of these leaky thin films. It is especially urgent to develop the necessary new ferroelectric test technology for the electrical research of ultra-thin thin films. With the development of the market and the improvement of the integration of microelectronic devices, the size of the device is developing at a speed of 1 times every 2 years according to Moore's law, gradually approaching the level of atoms or molecules, such as the 16nm microelectronics that Intel is currently researching and developing. The MOS devices below the size and the research plan of functional devices below 22nm in the major special project of "very large scale integrated circuit equipment and complete process" launched during the "Eleventh Five-Year Plan" period of our country are all moving towards this goal. Therefore, it is very urgent to actively develop advanced thin film testing technology from the perspective of market application. The research on the growth of ferroelectric thin films at the atomic level is also of positive significance for the development of the kinetic theory of domain nucleation and growth. Theoretically, the flipping of the electric domain starts from the formation of the reverse sub-nuclei of the critical size, which initially originates from the surface of the film or the accumulation area of defects. The latest density functional (DFT) calculations show that the size of this critical sub-nucleus is on the order of three unit cells, that is to say, only those sub-nuclei larger than this size will contribute to the flipping of electric domains. However, when the thickness of the film is close to or lower than the critical dimension, the flip mechanism must be different, and the understanding of the mechanism is still unclear, which affects the further development of device functions. In addition, as the film thickness decreases, the quantum tunneling current increases accordingly. On the one hand, this tunneling current will change with the reorientation of the electrical domain, which can be applied to the non-destructive reading of logic signals in high-density FRAM memory cells, which is of positive significance; on the other hand, it also further improves Leakage current is reduced, which deepens the difficulty of thin film electrical measurement. That is, even if we were able to grow flawless thin-film crystals, it would be impossible to complete the electrical characterization of these thin films with existing commercial equipment. Therefore, the leakage ferroelectric thin film test method designed in the present invention and the leakage ferroelectric thin film electrical performance test system designed by applying this principle provide a powerful tool for the research and application of ferroelectric thin film materials.

发明内容 Contents of the invention

本发明的目的在于提出一种测量漏电铁电薄膜电滞回线的方法,以便于对漏电铁电薄膜的性能进行研究。The purpose of the present invention is to provide a method for measuring the hysteresis loop of the leakage ferroelectric thin film, so as to study the performance of the leakage ferroelectric thin film.

本发明方法的具体步骤如下:The concrete steps of the inventive method are as follows:

(1)利用脉冲发生器首先产生一脉冲,以使所测漏电铁电薄膜内在所加电压下可逆电畴完全翻转。(1) Use a pulse generator to generate a pulse first, so that the reversible electric domain in the leakage ferroelectric film under test is completely reversed under the applied voltage.

(2)在电流稳定后测量通过漏电同极性铁电薄膜的电流,由于此时铁电畴极化方向和外界电场方向一致,测量过程在电容器完成充电后进行,所测电流只包含漏电流部分,即测得通过漏电铁电薄膜的漏电流值。(2) After the current is stable, measure the current passing through the ferroelectric film with the same polarity as the leakage current. Since the polarization direction of the ferroelectric domain is consistent with the direction of the external electric field at this time, the measurement process is carried out after the capacitor is fully charged, and the measured current only includes the leakage current. Part, that is, the measured leakage current value through the leakage ferroelectric film.

(3)改变脉冲幅值(包括方向),测量不同电压下通过漏电铁电薄膜的漏电流值。(3) Change the pulse amplitude (including the direction), and measure the leakage current value passing through the leakage ferroelectric film under different voltages.

(4)根据以上所测数据,并由公式(4) According to the above measured data, and by the formula

VF=V-ILRV F =VI L R

(其中R为系统总电阻,V为测量脉冲幅值,IL为通过漏电铁电薄膜和串联电阻上的漏电流,VF为施加在铁电薄膜上的电压。)做出漏电流IL和薄膜两端电压VF的曲线,进行多项式拟合,求出漏电流IL以薄膜两端电压VF为自变量的方程IL=F(VF)。(Wherein R is the total resistance of the system, V is the measurement pulse amplitude, I L is the leakage current through the leakage ferroelectric film and the series resistance, and V F is the voltage applied to the ferroelectric film.) Make the leakage current I L and the curve of the voltage V F at both ends of the film, and perform polynomial fitting to obtain the equation IL = F(V F ) of the leakage current I L with the voltage V F at both ends of the film as an independent variable.

(5)外加电压和电畴取向的极性相反。由示波器记录整个串联电阻上的总电流随时间的变化I(t),求出铁电薄膜中的真实电压随时间变化VF(t).由以上漏电流-电压的函数关系,计算出铁电薄膜中漏电流随时间变化的关系IL=F[VF(t)],并从I(t)中进行扣除,得到位移电流随时间变化关系I(t)-F[VF(t)]。(5) The polarities of the applied voltage and domain orientation are opposite. Record the change I(t) of the total current on the entire series resistance with time by an oscilloscope, and obtain the change V F (t) of the real voltage in the ferroelectric film with time. From the above leakage current-voltage function relationship, calculate the ferroelectric The relationship of the leakage current changing with time in the electric film I L =F[V F (t)], and deducted from I(t), to obtain the relationship of the displacement current changing with time I(t)-F[V F (t )].

(6)将位移电流曲线对时间进行积分,并除以电极面积就得到该外加电压下漏电铁电薄膜两端电压引起的极化电荷密度(电位移)。(6) Integrate the displacement current curve with respect to time and divide it by the electrode area to obtain the polarized charge density (electrical displacement) caused by the voltage across the leakage ferroelectric film under the applied voltage.

(7)改变外加电压,重复以上的测量和计算,得到不同电压下铁电薄膜的电位移,即整个漏电铁电薄膜的电滞回线。(7) Change the applied voltage, repeat the above measurement and calculation, and obtain the electric displacement of the ferroelectric film under different voltages, that is, the hysteresis loop of the entire leakage ferroelectric film.

上述方法中,步骤(1)中利用脉冲发生器产生的脉冲宽度要足以使全部可逆铁电畴完全转向,其宽度应由具体测试样品而定。In the above method, the pulse width generated by the pulse generator in step (1) should be sufficient to completely turn all the reversible ferroelectric domains, and the width should be determined by the specific test sample.

上述方法中,步骤(2)中测量电流应在电容器充电完成后进行,由于此时铁电畴极化方向和外界电场方向一致,通过系统的电流中不包含位移电流的成分,所测电流是通过漏电铁电薄膜的漏电流。In the above method, the measurement current in step (2) should be carried out after the capacitor is charged. Since the direction of the ferroelectric domain polarization is consistent with the direction of the external electric field at this time, the current passing through the system does not contain the component of the displacement current. The measured current is Leakage current through a leaky ferroelectric film.

上述方法中,步骤(3)中脉冲幅值的大小应包含由0V到±V中的全部电压(考虑到内电阻的分压有V>Vs,具体值取决于实际测量系统,Vs为使样品极化饱和的电压,其取决于铁电薄膜样品本身的电学特征。)In the above method, the magnitude of the pulse amplitude in step (3) should include all voltages from 0V to ±V (considering that the divided voltage of the internal resistance is V>V s , the specific value depends on the actual measurement system, V s is The voltage to saturate the sample polarization depends on the electrical characteristics of the ferroelectric thin film sample itself.)

上述方法中,步骤(4)中铁电薄膜两端电压VF与总电流I的关系写作公式VF=V-ILR是由于此时位移电流为零I=IL,在整个电流弛豫过程中应写为VF=V-IR,V为脉冲幅值。In the above method, the relationship between the voltage V F at both ends of the ferroelectric thin film and the total current I in step (4) is written as the formula V F = VI L R because the displacement current is zero I = I L at this time, and in the whole current relaxation process It should be written as V F =V-IR, V is the pulse amplitude.

上述方法中,步骤(5)中通过铁电薄膜的漏电流与铁电薄膜两端电压的关系应用于整个电流弛豫过程是基于一个普遍适用假设,即通过铁电薄膜的漏电流只与铁电薄膜两端电压有关,电畴的极化状态对漏电没有影响。In the above method, the relationship between the leakage current of the ferroelectric thin film and the voltage across the ferroelectric thin film in step (5) is applied to the whole current relaxation process based on a generally applicable assumption, that is, the leakage current through the ferroelectric thin film is only related to the ferroelectric thin film. The voltage at both ends of the electric film is related, and the polarization state of the electric domain has no effect on the leakage.

附图说明 Description of drawings

图1漏电铁电薄膜电滞回线测量系统组成简图。Figure 1 is a schematic diagram of the measurement system for leakage ferroelectric thin film hysteresis loops.

图2在总的测试电流中扣除漏电流的示意图。Figure 2 is a schematic diagram of deducting the leakage current from the total test current.

图3测量得到的漏电流与漏电铁电薄膜两端电压关系曲线。Fig. 3 is the relationship curve between the measured leakage current and the voltage across the leakage ferroelectric film.

图4由高阶多项式拟合得到的漏电流与漏电铁电薄膜两端电压函数曲线。Fig. 4 is the function curve of the leakage current and the voltage across the leakage ferroelectric film obtained by fitting a high-order polynomial.

图5使用漏电铁电薄膜测试系统对模拟漏电电容(将标准电容与任意电阻并联构成模拟漏电电容)测试的结果。Fig. 5 is the test result of the simulated leakage capacitance (connecting the standard capacitance and any resistance in parallel to form the simulated leakage capacitance) by using the leakage ferroelectric film test system.

图6使用漏电铁电薄膜测试系统对模拟漏电铁电薄膜(将标准铁电电容与任意电阻并联构成模拟漏电铁电薄膜)的测试结果。Fig. 6 is the test result of a simulated leakage ferroelectric film (a standard ferroelectric capacitor connected in parallel with an arbitrary resistor to form a simulated leakage ferroelectric film) using a leakage ferroelectric film test system.

具体实施方式 Detailed ways

测试所需的脉冲信号都是用Agilent 81150A任意波形信号发生器信编辑,电流由LCWR6200A示波器记录,系统内阻50欧姆。The pulse signals required for the test are all edited by the Agilent 81150A arbitrary waveform signal generator, the current is recorded by the LCWR6200A oscilloscope, and the internal resistance of the system is 50 ohms.

测量由标准铁电电容和电阻并联组成的模拟漏电铁电薄膜系统。Measure a simulated leakage ferroelectric thin film system consisting of a standard ferroelectric capacitor and resistor in parallel.

(1)利用脉冲发生器首先产生一足够宽的脉冲,以使所测漏电铁电薄膜内在所加电压下可逆电畴完全翻转。(1) Use a pulse generator to first generate a pulse with a sufficient width so that the reversible electric domain in the measured leakage ferroelectric film is completely reversed under the applied voltage.

(2)在电流稳定后测量通过漏电同极性铁电薄膜的电流,由于此时铁电畴极化方向和外界电场方向一致,测量过程在电容器完成充电后进行,所测电流只包含漏电流部分,即测得通过漏电铁电薄膜的漏电流值。(2) After the current is stable, measure the current passing through the ferroelectric film with the same polarity as the leakage current. Since the polarization direction of the ferroelectric domain is consistent with the direction of the external electric field at this time, the measurement process is carried out after the capacitor is fully charged, and the measured current only includes the leakage current. Part, that is, the measured leakage current value through the leakage ferroelectric film.

(3)改变脉冲幅值(0至±10V),测量不同电压下通过漏电铁电薄膜的漏电流值。(3) Change the pulse amplitude (0 to ±10V), and measure the leakage current value passing through the leakage ferroelectric film under different voltages.

(4)根据以上所测数据,并由公式(4) According to the above measured data, and by the formula

VF=V-ILRV F =VI L R

(其中R为系统总电阻,V为测量脉冲幅值,IL为通过漏电铁电薄膜和串联电阻上的漏电流,VF为施加在铁电薄膜上的电压。)做出漏电流I和薄膜两端电压VF的曲线,进行多项式拟合,求出漏电流IL以薄膜两端电压VF为自变量的方程IL=F(VF)。(Wherein R is the total resistance of the system, V is the measurement pulse amplitude, I L is the leakage current through the leakage ferroelectric film and the series resistance, and V F is the voltage applied on the ferroelectric film.) Make the leakage current I and Polynomial fitting is performed on the curve of the voltage V F across the film, and the equation IL = F(V F ) of the leakage current IL with the voltage V F across the film as an independent variable is obtained.

(5)外加电压和电畴取向的极性相反。由示波器记录整个串联电阻上的总电流随时间的变化I(t),求出铁电薄膜中的真实电压随时间变化VF(t).由以上漏电流-电压的函数关系,计算出铁电薄膜中漏电流随时间变化IL=F[VF(t)],并从I(t)中进行扣除,得到位移电流随时间变化关系I(t)-F[VF(t)]。(5) The polarities of the applied voltage and domain orientation are opposite. Record the change I(t) of the total current on the entire series resistance with time by an oscilloscope, and obtain the change V F (t) of the real voltage in the ferroelectric film with time. From the above leakage current-voltage function relationship, calculate the ferroelectric The leakage current in the electric film changes with time I L =F[V F (t)], and is deducted from I(t) to obtain the relationship of displacement current with time I(t)-F[V F (t)] .

(6)对位移电流曲线进行积分,并除以电极面积就得到该外加电压下漏电铁电薄膜两端电压引起的极化电荷密度(电位移)。(6) Integrate the displacement current curve and divide it by the electrode area to obtain the polarization charge density (electric displacement) caused by the voltage across the leakage ferroelectric film under the applied voltage.

(7)改变外加电压,重复以上的测量和计算,得到不同电压下铁电薄膜的电位移,即整个漏电铁电薄膜的电滞回线。(7) Change the applied voltage, repeat the above measurement and calculation, and obtain the electric displacement of the ferroelectric film under different voltages, that is, the hysteresis loop of the entire leakage ferroelectric film.

图4和图5分别给出了,使用漏电铁电薄膜测试系统分别对模拟漏电电容和模拟漏电铁电薄膜进行测量得到的电容极化曲线和铁电薄膜电滞回线。由两图中的模拟漏电情况和理想情况结果对比可以证明,本发明方法可以有效对漏电铁电薄膜样品的电学性能进行测量。Figure 4 and Figure 5 respectively show the capacitance polarization curve and the hysteresis loop of the ferroelectric film obtained by measuring the simulated leakage capacitance and the simulated leakage ferroelectric film by using the leakage ferroelectric film test system. It can be proved by the comparison of the simulated leakage situation and the ideal situation in the two figures that the method of the present invention can effectively measure the electrical properties of the leakage ferroelectric thin film sample.

Claims (1)

1. method of measuring ferroelectric hysteresis loop of leakage ferroelectric film is characterized in that concrete steps are following:
(1) utilize pulse producer at first to produce a pulse, the width of this pulse can make the institute the electric ferroelectric thin film that leaks hunting under institute's making alive reversible electricdomain overturn fully;
(2) after current stabilization, measure the electric current that passes through electric leakage same polarity ferroelectric thin film, record leakage current value through the electric leakage ferroelectric thin film;
(3) change pulse amplitude, measure different electric and depress leakage current value through the electric leakage ferroelectric thin film;
(4) according to the above data of surveying, and by formula
V F=V-I LR
Make leakage current I LWith film voltage V FCurve, carry out fitting of a polynomial, obtain leakage current I LWith film voltage V FEquation I for independent variable L=F (V F), wherein R is system's all-in resistance, V is for measuring pulse amplitude, I LFor passing through the leakage current on electric leakage ferroelectric thin film and the resistance in series, V FFor being applied to the voltage on the ferroelectric thin film;
(5) polarity of impressed voltage and electric domain orientation is opposite, and by the I (t) over time of the total current on the whole resistance in series of oscillograph recording, the real voltage of obtaining in the ferroelectric thin film changes V in time F(t); By above leakage current I LWith voltage V FRelation curve, calculate the time dependent relations I of leakage current in the ferroelectric thin film L=F [V F(t)], and from I (t), deduct, obtain displacement current variation relation I (t)-F [V in time F(t)];
(6) the displacement current curve is carried out integration about the time, and just obtain the electric displacement that electric leakage ferroelectric thin film voltage causes under this impressed voltage divided by electrode area;
(7) change impressed voltage, repeat above measurements and calculations, obtain the electric displacement that different electric is depressed ferroelectric thin film, be the ferroelectric hysteresis loop of whole electric leakage ferroelectric thin film.
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