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CN106932662A - A kind of device and method for detecting phase transformation ferroelectric ceramics remanent polarization - Google Patents

A kind of device and method for detecting phase transformation ferroelectric ceramics remanent polarization Download PDF

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CN106932662A
CN106932662A CN201511015643.4A CN201511015643A CN106932662A CN 106932662 A CN106932662 A CN 106932662A CN 201511015643 A CN201511015643 A CN 201511015643A CN 106932662 A CN106932662 A CN 106932662A
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pressure
integrating capacitor
electrometer
presser unit
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CN106932662B (en
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曹菲
陈建和
王根水
董显林
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Shanghai Institute of Ceramics of CAS
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    • G01MEASURING; TESTING
    • G01RMEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
    • G01R31/00Arrangements for testing electric properties; Arrangements for locating electric faults; Arrangements for electrical testing characterised by what is being tested not provided for elsewhere

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Abstract

The present invention relates to a kind of device and method for detecting phase transformation ferroelectric ceramics remanent polarization, the device includes:Sample, integrating capacitor, electrometer, presser unit, pressure sensing cell and control unit;The sample is placed in the presser unit, the sample is connected in parallel with the integrating capacitor and electrometer respectively, the control interface of the electrometer is connected to described control unit, and the pressure sensing cell is placed in the presser unit, and the pressure signal that will be detected is transferred to described control unit.The present invention enables phase transformation ferroelectric ceramics depolarization under stress field action, so as to measure the remanent polarization of ferroelectric ceramics.

Description

一种检测相变铁电陶瓷剩余极化强度的装置及方法A device and method for detecting remnant polarization of phase-change ferroelectric ceramics

技术领域 technical field

本发明涉及铁电材料的电学性能参数测量,具体地,涉及一种检测相变铁电陶瓷剩余极化强度的装置及方法。 The invention relates to the measurement of electrical performance parameters of ferroelectric materials, in particular to a device and method for detecting remnant polarization of phase-change ferroelectric ceramics.

背景技术 Background technique

剩余极化强度是评价铁电陶瓷储能特性的重要参数,有着重要的实用意义,因此需要建立一种测试装置及方法实现铁电陶瓷实际储存能量的测量。铁电陶瓷储存的能量通常用剩余极化强度来表示,目前常用测试方法有热退极化法。 Remanent polarization is an important parameter to evaluate the energy storage characteristics of ferroelectric ceramics, and has important practical significance. Therefore, it is necessary to establish a test device and method to measure the actual stored energy of ferroelectric ceramics. The energy stored in ferroelectric ceramics is usually represented by remanent polarization, and the commonly used test method is thermal depolarization method.

极化了的铁电陶瓷储存能量,在外场作用下会发生退极化,由于实际应用场合的不同,外场可以是温度场,也可以是应力场。铁电材料在应力场作用下会产生大电压或大电流,有着重要的应用价值,因此需要建立应力加载作用下材料剩余极化强度的检测装置及方法。 Polarized ferroelectric ceramics store energy, and depolarization will occur under the action of an external field. Due to different practical applications, the external field can be a temperature field or a stress field. Ferroelectric materials can generate large voltage or large current under the action of stress field, which has important application value. Therefore, it is necessary to establish a detection device and method for the remanent polarization of materials under stress loading.

发明内容 Contents of the invention

鉴于以上所述,本发明所要解决的技术问题在于提供一种检测相变铁电陶瓷剩余极化强度的装置及方法,使相变铁电陶瓷能在应力场作用下退极化,从而测得铁电陶瓷的剩余极化强度。 In view of the above, the technical problem to be solved by the present invention is to provide a device and method for detecting the remnant polarization of phase-change ferroelectric ceramics, so that phase-change ferroelectric ceramics can be depolarized under the action of a stress field, thereby measuring Remanent polarization of ferroelectric ceramics.

为了解决上述技术问题,一方面,本发明所提供的检测相变铁电陶瓷剩余极化强度的装置,包括:样品、积分电容、静电计、加压单元、压力检测单元、以及控制单元;所述样品置于所述加压单元中,所述样品分别与所述积分电容和静电计并联连接,所述静电计的控制接口接至所述控制单元,所述压力检测单元置于所述加压单元中,将检测到的压力信号传输给所述控制单元。 In order to solve the above technical problems, on the one hand, the device for detecting the remnant polarization of phase-change ferroelectric ceramics provided by the present invention includes: a sample, an integrating capacitor, an electrometer, a pressurizing unit, a pressure detecting unit, and a control unit; The sample is placed in the pressurizing unit, the sample is respectively connected in parallel with the integrating capacitor and the electrometer, the control interface of the electrometer is connected to the control unit, and the pressure detection unit is placed in the pressurizing unit. In the pressure unit, the detected pressure signal is transmitted to the control unit.

本发明通过加压单元对相变铁电陶瓷施加压力,施压过程中,测量相变铁电陶瓷释放的电荷,从而得到陶瓷的剩余极化强度。由此,本发明可通过测量相变铁电陶瓷应力场下的退极化电荷,测得陶瓷的剩余极化强度。 The invention applies pressure to the phase-change ferroelectric ceramics through a pressure unit, and measures the electric charge released by the phase-change ferroelectric ceramics during the process of applying pressure, so as to obtain the remanent polarization intensity of the ceramics. Therefore, the present invention can measure the remanent polarization intensity of the ceramic by measuring the depolarization charge under the stress field of the phase-change ferroelectric ceramic.

又,在本发明中,也可以是,所述加压单元包括容纳有传压介质的静水压压力试验机,所述样品置于所述静水压压力试验机的传压介质中。 Moreover, in the present invention, it is also possible that the pressurizing unit includes a hydrostatic pressure testing machine containing a pressure transmission medium, and the sample is placed in the pressure transmission medium of the hydrostatic pressure testing machine.

根据本发明,可通过静水压压力试验机对相变铁电陶瓷施加压力,施压过程中,测量相变铁电陶瓷释放的电荷,从而得到陶瓷的剩余极化强度。 According to the present invention, pressure can be applied to the phase-change ferroelectric ceramics through a hydrostatic pressure testing machine, and during the process of applying pressure, the electric charge released by the phase-change ferroelectric ceramics can be measured, so as to obtain the remanent polarization intensity of the ceramics.

优选地,所述压力检测单元包括压力传感器,所述压力传感器通过A/D转换卡将检测到的压力信号传输给所述控制单元。 Preferably, the pressure detection unit includes a pressure sensor, and the pressure sensor transmits the detected pressure signal to the control unit through an A/D conversion card.

另一方面,本发明还提供了一种检测相变铁电陶瓷剩余极化强度的方法,包括下列步骤:测量样品的有效电极面积A,测量积分电容的电容值C;将所述样品置于加压单元中,所述样品分别与所述积分电容和静电计并联连接;用导线将所述积分电容两端短路连接;使所述加压单元进行加压,同时断开所述积分电容两端的短路导线;加压过程中,记录压力值;同时用所述静电计记录所述积分电容两端的电压值V,不断增大压力,直至电压值V基本不变,记录下此时的电压值V;将所述样品的有效电极面积A、所述积分电容的电容值C和所述电压值V代入公式Pr=C×V/A,计算得到陶瓷的剩余极化强度。 On the other hand, the present invention also provides a method for detecting the remnant polarization of phase-change ferroelectric ceramics, comprising the following steps: measuring the effective electrode area A of the sample, and measuring the capacitance C of the integral capacitance; placing the sample in In the pressurizing unit, the samples are respectively connected in parallel with the integrating capacitor and the electrometer; the two ends of the integrating capacitor are short-circuited with wires; The short-circuit wire at the end; during the pressurization process, record the pressure value; at the same time, use the electrometer to record the voltage value V at both ends of the integrating capacitor, and continuously increase the pressure until the voltage value V is basically unchanged, and record the voltage value at this time V: Substituting the effective electrode area A of the sample, the capacitance value C of the integral capacitor, and the voltage value V into the formula Pr=C×V/A to calculate the remanent polarization of the ceramic.

根据本发明,可通过测量相变铁电陶瓷应力场下的退极化电荷,测得陶瓷的剩余极化强度。 According to the invention, the residual polarization intensity of the ceramic can be measured by measuring the depolarization charge under the stress field of the phase-change ferroelectric ceramic.

又,在本发明中,也可以是,所述加压单元包括容纳有传压介质的静水压压力试验机,使所述加压单元进行加压的步骤包括设置所述静水压压力试验机的静水压加压范围,启动静水压加压程序。 Moreover, in the present invention, it is also possible that the pressurization unit includes a hydrostatic pressure testing machine containing a pressure transmission medium, and the step of pressurizing the pressurization unit includes setting the hydrostatic pressure test machine. The hydrostatic pressurization range of the machine, start the hydrostatic pressurization program.

根据本发明,通过静水压压力试验机向相变铁电陶瓷施加应力,加至超过材料的相变应力,加压过程中通过测量相变铁电陶瓷释放出的电荷,得到其剩余极化强度。 According to the present invention, the stress is applied to the phase-change ferroelectric ceramics by a hydrostatic pressure testing machine, and the stress is added to exceed the phase-transition stress of the material. strength.

根据下述具体实施方式并参考附图,将更好地理解本发明的上述内容及其它目的、特征和优点。 The above contents and other objects, features and advantages of the present invention will be better understood according to the following detailed description and with reference to the accompanying drawings.

附图说明 Description of drawings

图1 示出了根据本发明一实施形态的检测相变铁电陶瓷剩余极化强度的装置的结构示意图; Fig. 1 shows a schematic structural view of a device for detecting the remnant polarization of a phase-change ferroelectric ceramic according to an embodiment of the present invention;

图2示出了采用图1所示装置及方法测得的相变铁电陶瓷PZT静水压下积分电容测得电压-应力关系曲线; Fig. 2 shows the voltage-stress relationship curve measured by the phase-change ferroelectric ceramic PZT under hydrostatic pressure integrating capacitance measured by the device and method shown in Fig. 1;

图3示出了采用图1所示装置及方法测得的相变铁电陶瓷PZT静水压下剩余极化强度-应力关系曲线。 Fig. 3 shows the remanent polarization-stress relationship curve of the phase-change ferroelectric ceramic PZT under hydrostatic pressure measured by using the device and method shown in Fig. 1 .

附图标记: Reference signs:

1、样品, 1. Sample,

2、积分电容, 2. Integral capacitance,

3、静电计, 3. Electrometer,

4、传压介质, 4. Pressure transmission medium,

5、静水压压力试验机, 5. Hydrostatic pressure testing machine,

6、压力检测单元, 6. Pressure detection unit,

7、A/D转换卡, 7. A/D conversion card,

8、控制单元。 8. Control unit.

具体实施方式 detailed description

以下结合附图和下述实施方式进一步说明本发明,应理解,附图及下述实施方式仅用于说明本发明,而非限制本发明。 The present invention will be further described below in conjunction with the drawings and the following embodiments. It should be understood that the drawings and the following embodiments are only used to illustrate the present invention rather than limit the present invention.

为了应对检测铁电陶瓷剩余极化强度的需求,本发明提供了一种检测相变铁电陶瓷剩余极化强度的装置及方法,该装置包括:样品、积分电容、静电计、加压单元、压力检测单元、以及控制单元;所述样品置于所述加压单元中,所述样品分别与所述积分电容和静电计并联连接,所述静电计的控制接口接至所述控制单元,所述压力检测单元置于所述加压单元中,将检测到的压力信号传输给控制单元。 In order to meet the demand for detecting the remanent polarization of ferroelectric ceramics, the present invention provides a device and method for detecting the remanent polarization of phase-change ferroelectric ceramics, the device includes: samples, integrating capacitors, electrometers, pressurization units, A pressure detection unit and a control unit; the sample is placed in the pressurizing unit, the sample is connected in parallel with the integrating capacitor and the electrometer respectively, the control interface of the electrometer is connected to the control unit, and the The pressure detection unit is placed in the pressurization unit, and the detected pressure signal is transmitted to the control unit.

具体地,图1 示出了根据本发明一实施形态的检测相变铁电陶瓷剩余极化强度的装置的结构示意图。如图1所示,本实施形态的检测相变铁电陶瓷剩余极化强度的装置包括:样品1、积分电容2、静电计3、容纳有传压介质4的静水压压力试验机5、压力检测单元6、A/D转换卡7以及控制单元8。 Specifically, Fig. 1 shows a schematic structural diagram of a device for detecting the remnant polarization of a phase-change ferroelectric ceramic according to an embodiment of the present invention. As shown in Figure 1, the device for detecting the remanent polarization of phase-change ferroelectric ceramics in this embodiment includes: a sample 1, an integrating capacitor 2, an electrometer 3, a hydrostatic pressure testing machine 5 containing a pressure transmission medium 4, A pressure detection unit 6 , an A/D conversion card 7 and a control unit 8 .

样品1置于静水压压力试验机5的传压介质4中,样品1分别与积分电容2和静电计3并联连接,静电计3的控制接口接至控制单元8。压力检测单元6置于传压介质4中,通过A/D转换卡7将检测到的压力信号传输给控制单元8。上述压力检测单元6例如可以是压力传感器等用于检测压力的器件。 Sample 1 is placed in the pressure transmission medium 4 of the hydrostatic pressure testing machine 5 , the sample 1 is connected in parallel with the integrating capacitor 2 and the electrometer 3 , and the control interface of the electrometer 3 is connected to the control unit 8 . The pressure detection unit 6 is placed in the pressure transmission medium 4 , and the detected pressure signal is transmitted to the control unit 8 through the A/D conversion card 7 . The above-mentioned pressure detection unit 6 may be, for example, a device for detecting pressure such as a pressure sensor.

利用上述装置实现相变铁电陶瓷剩余极化强度的方法,该方法包括以下步骤: A method for realizing the remanent polarization of phase-change ferroelectric ceramics by using the above-mentioned device, the method includes the following steps:

首先,测量样品1的有效电极面积值A;并测量积分电容2的电容值C。 First, measure the effective electrode area value A of the sample 1; and measure the capacitance value C of the integrating capacitor 2.

随后,按图1所示的装置结构示意图连接好整个检测装置,并将样品1置于静水压压力试验机5的传压介质4中。 Subsequently, connect the entire detection device according to the schematic diagram of the device structure shown in FIG. 1 , and place the sample 1 in the pressure transmission medium 4 of the hydrostatic pressure testing machine 5 .

然后,打开上述装置中的各部件电源,各部件开始工作。 Then, turn on the power supply of each component in the above-mentioned device, and each component starts to work.

接着,用导线将积分电容2两端短路连接;并设置静水压加压范围,启动静水压加压程序,同时断开积分电容2两端的短路导线。 Next, short-circuit the two ends of the integrating capacitor 2 with wires; set the hydrostatic pressure range, start the hydrostatic pressure program, and disconnect the short-circuit wires at both ends of the integrating capacitor 2 at the same time.

在加压过程中,记录应力值;同时用静电计3记录积分电容2两端的电压值V,不断增大压力,直至电压值V基本不变,记录下此时的电压值V。 During the pressurization process, record the stress value; at the same time, use the electrometer 3 to record the voltage value V at both ends of the integrating capacitor 2, and continuously increase the pressure until the voltage value V is basically unchanged, and record the voltage value V at this time.

最后,将样品1的有效电极面积A、积分电容2的电容值C和电压值V代入公式Pr=C×V/A,计算得到陶瓷的剩余极化强度。 Finally, the effective electrode area A of sample 1, the capacitance value C and voltage value V of the integral capacitor 2 were substituted into the formula Pr=C×V/A, and the remanent polarization of the ceramic was calculated.

本发明通过静水压压力试验机向相变铁电陶瓷施加应力,加至超过材料的相变应力,加压过程中通过测量相变铁电陶瓷释放出的电荷,得到其剩余极化强度。 The invention applies stress to the phase-change ferroelectric ceramics through a hydrostatic pressure testing machine until the stress exceeds the phase-transition stress of the material, and measures the electric charge released by the phase-change ferroelectric ceramics during the pressurization process to obtain its residual polarization intensity.

本测量装置及方法实现了应力场加载作用下相变铁电陶瓷剩余极化强度的测量。 The measuring device and method realize the measurement of the remnant polarization intensity of the phase-change ferroelectric ceramics under the action of stress field loading.

下面结合优选的具体实施例,进一步阐述本发明。应理解,这些实施例仅用于说明本发明而不用于限制本发明的范围。 Below in conjunction with preferred specific embodiment, further elaborate the present invention. It should be understood that these examples are only used to illustrate the present invention and are not intended to limit the scope of the present invention.

实施例1 Example 1

按照图1所示的装置结构示意图进行接线,对相变铁电陶瓷样品进行剩余极化强度测量。图2示出了采用图1所示装置及方法测得的相变铁电陶瓷PZT静水压下积分电容测得电压-应力关系曲线;图3示出了采用图1所示装置及方法测得的相变铁电陶瓷PZT静水压下剩余极化强度-应力关系曲线。 Connect according to the schematic diagram of the device structure shown in Figure 1, and measure the remnant polarization of the phase-change ferroelectric ceramic samples. Fig. 2 shows the voltage-stress relationship curve measured by the integrated capacitance of the phase-change ferroelectric ceramic PZT under hydrostatic pressure measured by the device and method shown in Fig. 1; The obtained phase-change ferroelectric ceramic PZT remanent polarization-stress relationship curve under hydrostatic pressure.

测量参数如下:样品有效电极面积281.25mm2,厚度2mm,积分电容的电容值10μF,施加静水压压力范围0~300MPa。测试结果如图2、图3所示。随着静水压压力的增加,样品逐步释放出电荷,不断增大压力,直至积分电容两端电压值V基本不变,此时积分电容两端电压为0.61V。将样品面积281.25mm2,积分电容电容值10μF和电容器两端电压10.3V,代入公式Pr=C×V/A,得到剩余极化强度Pr为36.6μC/cm2The measurement parameters are as follows: the effective electrode area of the sample is 281.25mm 2 , the thickness is 2mm, the capacitance value of the integral capacitor is 10μF, and the applied hydrostatic pressure ranges from 0 to 300MPa. The test results are shown in Figure 2 and Figure 3. With the increase of the hydrostatic pressure, the sample gradually releases the charge, and the pressure continues to increase until the voltage value V across the integrating capacitor is basically unchanged, and the voltage across the integrating capacitor is 0.61V at this time. Substituting the sample area of 281.25mm 2 , the integral capacitance of 10μF and the voltage across the capacitor of 10.3V into the formula Pr=C×V/A, the remanent polarization Pr is 36.6μC/cm 2 .

测试结果表明:相变铁电陶瓷随施加的静水压压力的增大而逐渐释放电荷,当压力增大至相变压力时,电荷急剧增大,继续增大压力,电荷基本不变。施加的静水压压力超过相变压力后,释放电荷基本保证不变,该基本不变的数值为该样品在应力加载作用下的退极化电荷,从而计算得到剩余极化强度。 The test results show that phase-change ferroelectric ceramics gradually release charges as the applied hydrostatic pressure increases. When the pressure increases to the phase-change pressure, the charge increases sharply, and the charge remains basically unchanged when the pressure continues to increase. After the applied hydrostatic pressure exceeds the phase transition pressure, the released charge is basically guaranteed to be unchanged, and the basically constant value is the depolarization charge of the sample under stress loading, so as to calculate the remanent polarization.

最后有必要在此说明的是:以上实施例只用于对本发明的技术方案作进一步详细地说明,不能理解为对本发明保护范围的限制,本领域的技术人员根据本发明的上述内容作出的一些非本质的改进和调整均属于本发明的保护范围。 Finally, it is necessary to explain here that: the above examples are only used to further describe the technical solutions of the present invention in detail, and cannot be interpreted as limiting the protection scope of the present invention. Non-essential improvements and adjustments all belong to the protection scope of the present invention.

Claims (5)

1. it is a kind of detect phase transformation ferroelectric ceramics remanent polarization device, it is characterised in that including:
Sample, integrating capacitor, electrometer, presser unit, pressure sensing cell and control unit;
The sample is placed in the presser unit, the sample is connected in parallel with the integrating capacitor and electrometer respectively, the control interface of the electrometer is connected to described control unit, and the pressure sensing cell is placed in the presser unit, and the pressure signal that will be detected is transferred to described control unit.
2. device according to claim 1, it is characterised in that the presser unit includes accommodating the hydrostatic pressing pressure testing machine of transmission medium, the sample is placed in the transmission medium of the hydrostatic pressing pressure testing machine.
3. device according to claim 1 and 2, it is characterised in that the pressure sensing cell includes pressure sensor, the pressure sensor is transferred to described control unit by the pressure signal that A/D transition cards will be detected.
4. it is a kind of detect phase transformation ferroelectric ceramics remanent polarization method, it is characterised in that comprise the following steps:
The effective electrode area A of sample is measured, the capacitance C of integrating capacitor is measured;
The sample is placed in presser unit, the sample is connected in parallel with the integrating capacitor and electrometer respectively;
The terminal shortcircuit of the integrating capacitor two is connected with wire;
The presser unit is pressurizeed, simultaneously switch off the short-circuit conductors at the integrating capacitor two ends;
In pressure process, pressure value is recorded;
The magnitude of voltage V at the integrating capacitor two ends is recorded with the electrometer simultaneously, constantly increases pressure, until magnitude of voltage V is basically unchanged, record magnitude of voltage V now;
The effective electrode area A of the sample, the capacitance C of the integrating capacitor and the magnitude of voltage V are substituted into formula Pr=C × V/A, the remanent polarization of ceramics is calculated.
5. method according to claim 4, the presser unit includes accommodating the hydrostatic pressing pressure testing machine of transmission medium, hydrostatic pressing pressurization scope of the step of the making the presser unit be pressurizeed including the setting hydrostatic pressing pressure testing machine, starts hydrostatic pressing pressurization protocols.
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