纳米复合PZT压电陶瓷的制备及其力学性能研究
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摘要
纳米复合陶瓷是指纳米相颗粒均匀、弥散地分布在陶瓷基体中形成的复合材料。陶瓷结构纳米化可使其力学性能显著提高，突出表现在:断裂强度、断裂韧性和耐高温性能三个方面，同时还能提高材料的硬度、弹性模量、Weibull模数、并对热导率、热膨胀系数、抗热震性等产生有益的影响。
但是，压电陶瓷的结构纳米化对其性能的影响尚缺乏研究。本文利用Pb(NO_3)_2、Zr(NO_3)_4-5H_2O、Ti(OC4_H_9)_4作为原料，NaOH作为矿化剂，通过溶胶-凝胶法结合水热处理制备了组成近于准同型相界(MPB)的Pb(Zr_0.52Ti_0.48)O_3纳米晶(PZT)粉体并利用传统氧化物烧结法制备组成相同的PZT粉体。通过DSC/TGA、FT-IR、XRD和SEM对合成粉体进行了分析和表征。由此制备了均匀组成和结构的普通和纳米复合PZT陶瓷，并对其弹性模量、弯曲强度、硬度和断裂韧性等力学性能进行了测试分析;且利用SEM分析了PZT陶瓷的断口形貌及断裂方式；又通过Weibull统计评价了PZT陶瓷的弯曲强度的分散性；还通过R曲线模拟分析，研究了极化对PZT陶瓷强度的影响。
DSC/TGA、FT-IR、XRD和SEM结果表明：溶胶-凝胶法制备的PZT相在220℃开始出现，270℃水热处理2h合成了纯相纳米晶PZT粉体，粉体的晶粒大小为25nm左右。
纳米复合PZT压电性能测试结果表明其机电耦合系数，介电常数和压电系数等压电性能指标均不低于普通PZT陶瓷。力学性能测试结果表明：纳米复合PZT陶瓷的弹性模量较普通PZT陶瓷有明显提高，约提高36%；纳米复合PZT陶瓷的弯曲强度较普通PZT陶瓷有明显提高，约提高29%，纳米复合PZT强度的升高主要是晶界强化导致的结果；不同载荷下，纳米复合PZT陶瓷硬度均高于普通PZT陶瓷的硬度，并且两种材料都存在压痕尺寸效应；在压痕载荷5Kg条件下，纳米复合PZT陶瓷的断裂韧性较普通PZT陶瓷有明显提高，约提高50%左右；极化状态纳米复合PZT陶瓷的断裂韧性存在各向异性，平行于极化方向的断裂韧性值高于另外两个垂直于极化方向断裂韧性值，并认为这种断裂韧性的各向异性是由极化PZT陶瓷的电畴结构及力致畴变现象造成的。对弯曲强度的Weibull统计分析表明：在试验样品数为26的情况下，普通PZT陶瓷的Weibull模数为3.59，而纳米复合PZT陶瓷材料Weibull模数为8.167，说明纳米复合PZT陶瓷材料弯曲强度波动范围较小。断口的SEM与分形分析表明：普通PZT陶瓷在快速扩展区的断裂方式是沿晶断裂，纳米复相PZT陶瓷是穿晶断裂，穿晶断裂的断口分形维数高于沿晶断裂，分形维数与断裂韧性成正比例关系，这明显表明压电陶瓷微观结构纳米化对断裂韧性的有益影响。R曲线模拟分析表明：极化方向的裂纹扩展阻力随着裂纹深度的增加而增加，体现了畴致偏转对断裂的阻碍作用。
综上所述，本课题研究表明，PZT压电陶瓷结构的纳米化，可以实现其在压电性能不变或稍有提高的情况下，大幅度地提高力学性能。换言之，结构纳米化，可以在保证PZT压电陶瓷原有性能参数的条件下，显著地改善其力学性能。因此，可以预期，PZT压电陶瓷的结构纳米化将显著改善其力学性能，延长陶瓷制件的服役寿命。
Nano-phase composite ceramic is a composite material which contains nano-phase particles in homogeneous dispersion state. Nano-phase composite ceramic can enhance its mechanical properties which mainly express in three points: fracture strength, fracture toughness and high temperature resistance. And it can enhance hardness, elastic modulus, Weibull modulus of materials; also can produce higher heat conductivity, coefficient of thermal expansion and heat-shock resistance.
But now there is lacking in the researches of nanotechnology of piezoelectric ceramic structure effecting its properties. To prepare PZT nano-crystal powders with a composition of Pb(Zr_(0.52) Ti_(0.48))O_3,which is near the morphotropic phase boundary (MPB), the raw materials used were reagent grade lead nitrate [Pb(NO_3)_2],zirconium nitrate hydrate [Zr(NO_3)_4·5H_2O], tetra-butyl titanate [Ti(OC_4H_9)_4],using NaOH as the mineralizes, which use sol-gel method with hydro-thermal treating. And it use conventional oxide sintering method to prepare PZT powders with a identical composition. Powders are characterized by DSC/TGA, FT-IR, XRD, and SEM analysis. Common and nano-phase composite PZT ceramics were prepared which owe homogeneous composition and structure using powders, testing and analyzing elastic modulus, flexural strength, hardness and fracture toughness of PZT ceramics. SEM test of PZT ceramics fracture analyses its fracture mode. Weibull statistics evaluates flexural strength dispersibility of PZT ceramics. It also studies that polarization impacts strength in different direction with R curve analysis.
DSC/TGA, FT-IR, XRD, and SEM results indicate: PZT nano-phase started to form at as low as 220℃,while phase-pure PZT powders were obtained at 270℃for 2h, its grain size is about 25nm.
The piezoelectric testing results of nano-phase composite PZT ceramics indicate that performance date of electromechanical coupling coefficient, dielectric constant and piezoelectric coefficient is not below that of common PZT ceramics. The test results of mechanical properties indicate: elastic modulus is much higher than that of common PZT ceramics, with increasing about 36%. Flexural strength of nano-phase composite PZT ceramics is much higher than that of common PZT ceramics, with increasing about 29%, as the result of grain boundary strengthening. Hardness of nano-phase composite PZT ceramics is much higher than that of common PZT ceramics at different indentation loading, with indentation size effect. Fracture strength of nano-phase composite PZT ceramics is much higher than that of common PZT ceramics at 5Kg indentation loading, with increasing about 50%. Fracture toughness of nano-phase composite PZT ceramics in polarization state has anisotropy, with that of parallel polarization direction higher than the vertical, owing to its ferroelectric domain structure and mechano-domain transformation. Weibull statistics analysis of flexural strength indicates: common PZT ceramic has a Weibull modulus m=3.59, while nano-phase composite PZT ceramic with a Weibull modulus m=8.167, it also expresses flexural strength of nano-phase composite PZT ceramic fluctuates in a narrower range. SEM test and fractal analysis of PZT ceramics fracture morphology indicate that common PZT ceramic fracture mode is intercrystalline cracking, while nano-phase composite PZT ceramic is intergranular cracking and its fractal dimensionality is higher than that of the intercrystalline,its fractal dimensionality is direct proportional to fracture toughness. It obviously indicates nanotechnology of piezoelectric ceramic structure produces good affecting on its fracture toughness. R curve analysis indicates that resisting force of crack growth in polarization direction increases with crack size increasing, owing to ferroelectric domain deflection.
To summarize, this study revealed that nanotechnology of piezoelectric ceramic structure can enhance its mechanical properties greatly on the condition of piezoelectric property is unchanged or slightly enhanced.
In brief, nanotechnology of ceramic structure can enhance its mechanical properties greatly, ensuring intrinsic property parameters of piezoelectric ceramic. Therefore we can anticipate that nanotechnology of piezoelectric ceramic structure can enhance its mechanical properties greatly and can prolong service life of its products.
但是，压电陶瓷的结构纳米化对其性能的影响尚缺乏研究。本文利用Pb(NO_3)_2、Zr(NO_3)_4-5H_2O、Ti(OC4_H_9)_4作为原料，NaOH作为矿化剂，通过溶胶-凝胶法结合水热处理制备了组成近于准同型相界(MPB)的Pb(Zr_0.52Ti_0.48)O_3纳米晶(PZT)粉体并利用传统氧化物烧结法制备组成相同的PZT粉体。通过DSC/TGA、FT-IR、XRD和SEM对合成粉体进行了分析和表征。由此制备了均匀组成和结构的普通和纳米复合PZT陶瓷，并对其弹性模量、弯曲强度、硬度和断裂韧性等力学性能进行了测试分析;且利用SEM分析了PZT陶瓷的断口形貌及断裂方式；又通过Weibull统计评价了PZT陶瓷的弯曲强度的分散性；还通过R曲线模拟分析，研究了极化对PZT陶瓷强度的影响。
DSC/TGA、FT-IR、XRD和SEM结果表明：溶胶-凝胶法制备的PZT相在220℃开始出现，270℃水热处理2h合成了纯相纳米晶PZT粉体，粉体的晶粒大小为25nm左右。
纳米复合PZT压电性能测试结果表明其机电耦合系数，介电常数和压电系数等压电性能指标均不低于普通PZT陶瓷。力学性能测试结果表明：纳米复合PZT陶瓷的弹性模量较普通PZT陶瓷有明显提高，约提高36%；纳米复合PZT陶瓷的弯曲强度较普通PZT陶瓷有明显提高，约提高29%，纳米复合PZT强度的升高主要是晶界强化导致的结果；不同载荷下，纳米复合PZT陶瓷硬度均高于普通PZT陶瓷的硬度，并且两种材料都存在压痕尺寸效应；在压痕载荷5Kg条件下，纳米复合PZT陶瓷的断裂韧性较普通PZT陶瓷有明显提高，约提高50%左右；极化状态纳米复合PZT陶瓷的断裂韧性存在各向异性，平行于极化方向的断裂韧性值高于另外两个垂直于极化方向断裂韧性值，并认为这种断裂韧性的各向异性是由极化PZT陶瓷的电畴结构及力致畴变现象造成的。对弯曲强度的Weibull统计分析表明：在试验样品数为26的情况下，普通PZT陶瓷的Weibull模数为3.59，而纳米复合PZT陶瓷材料Weibull模数为8.167，说明纳米复合PZT陶瓷材料弯曲强度波动范围较小。断口的SEM与分形分析表明：普通PZT陶瓷在快速扩展区的断裂方式是沿晶断裂，纳米复相PZT陶瓷是穿晶断裂，穿晶断裂的断口分形维数高于沿晶断裂，分形维数与断裂韧性成正比例关系，这明显表明压电陶瓷微观结构纳米化对断裂韧性的有益影响。R曲线模拟分析表明：极化方向的裂纹扩展阻力随着裂纹深度的增加而增加，体现了畴致偏转对断裂的阻碍作用。
综上所述，本课题研究表明，PZT压电陶瓷结构的纳米化，可以实现其在压电性能不变或稍有提高的情况下，大幅度地提高力学性能。换言之，结构纳米化，可以在保证PZT压电陶瓷原有性能参数的条件下，显著地改善其力学性能。因此，可以预期，PZT压电陶瓷的结构纳米化将显著改善其力学性能，延长陶瓷制件的服役寿命。
Nano-phase composite ceramic is a composite material which contains nano-phase particles in homogeneous dispersion state. Nano-phase composite ceramic can enhance its mechanical properties which mainly express in three points: fracture strength, fracture toughness and high temperature resistance. And it can enhance hardness, elastic modulus, Weibull modulus of materials; also can produce higher heat conductivity, coefficient of thermal expansion and heat-shock resistance.
But now there is lacking in the researches of nanotechnology of piezoelectric ceramic structure effecting its properties. To prepare PZT nano-crystal powders with a composition of Pb(Zr_(0.52) Ti_(0.48))O_3,which is near the morphotropic phase boundary (MPB), the raw materials used were reagent grade lead nitrate [Pb(NO_3)_2],zirconium nitrate hydrate [Zr(NO_3)_4·5H_2O], tetra-butyl titanate [Ti(OC_4H_9)_4],using NaOH as the mineralizes, which use sol-gel method with hydro-thermal treating. And it use conventional oxide sintering method to prepare PZT powders with a identical composition. Powders are characterized by DSC/TGA, FT-IR, XRD, and SEM analysis. Common and nano-phase composite PZT ceramics were prepared which owe homogeneous composition and structure using powders, testing and analyzing elastic modulus, flexural strength, hardness and fracture toughness of PZT ceramics. SEM test of PZT ceramics fracture analyses its fracture mode. Weibull statistics evaluates flexural strength dispersibility of PZT ceramics. It also studies that polarization impacts strength in different direction with R curve analysis.
DSC/TGA, FT-IR, XRD, and SEM results indicate: PZT nano-phase started to form at as low as 220℃,while phase-pure PZT powders were obtained at 270℃for 2h, its grain size is about 25nm.
The piezoelectric testing results of nano-phase composite PZT ceramics indicate that performance date of electromechanical coupling coefficient, dielectric constant and piezoelectric coefficient is not below that of common PZT ceramics. The test results of mechanical properties indicate: elastic modulus is much higher than that of common PZT ceramics, with increasing about 36%. Flexural strength of nano-phase composite PZT ceramics is much higher than that of common PZT ceramics, with increasing about 29%, as the result of grain boundary strengthening. Hardness of nano-phase composite PZT ceramics is much higher than that of common PZT ceramics at different indentation loading, with indentation size effect. Fracture strength of nano-phase composite PZT ceramics is much higher than that of common PZT ceramics at 5Kg indentation loading, with increasing about 50%. Fracture toughness of nano-phase composite PZT ceramics in polarization state has anisotropy, with that of parallel polarization direction higher than the vertical, owing to its ferroelectric domain structure and mechano-domain transformation. Weibull statistics analysis of flexural strength indicates: common PZT ceramic has a Weibull modulus m=3.59, while nano-phase composite PZT ceramic with a Weibull modulus m=8.167, it also expresses flexural strength of nano-phase composite PZT ceramic fluctuates in a narrower range. SEM test and fractal analysis of PZT ceramics fracture morphology indicate that common PZT ceramic fracture mode is intercrystalline cracking, while nano-phase composite PZT ceramic is intergranular cracking and its fractal dimensionality is higher than that of the intercrystalline,its fractal dimensionality is direct proportional to fracture toughness. It obviously indicates nanotechnology of piezoelectric ceramic structure produces good affecting on its fracture toughness. R curve analysis indicates that resisting force of crack growth in polarization direction increases with crack size increasing, owing to ferroelectric domain deflection.
To summarize, this study revealed that nanotechnology of piezoelectric ceramic structure can enhance its mechanical properties greatly on the condition of piezoelectric property is unchanged or slightly enhanced.
In brief, nanotechnology of ceramic structure can enhance its mechanical properties greatly, ensuring intrinsic property parameters of piezoelectric ceramic. Therefore we can anticipate that nanotechnology of piezoelectric ceramic structure can enhance its mechanical properties greatly and can prolong service life of its products.
引文
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