技术领域technical field
本发明属于环境友好型材料领域，特别是提供一种铌酸钾钠基压电陶瓷材料及其制备方法。The invention belongs to the field of environment-friendly materials, and in particular provides a potassium-sodium niobate-based piezoelectric ceramic material and a preparation method thereof.
背景技术Background technique
压电陶瓷是一种能够实现机械能和电能相互转换的功能陶瓷材料，广泛应用于军事、汽车、商业和医疗技术等领域。由于含铅基压电陶瓷具有较大的压电常数，并且可以通过掺杂改性来调节器性能来满足不同的应用需求，所以在应用中含铅基压电陶瓷仍是主要的应用功能陶瓷，主要有Pb(Ti,Zr)O3(PZT)，PbTiO3-PbZrO3-ABO3(ABO3为复合钙钛矿型铁电体)及PbTiO3等。但是由于铅具有毒性对环境具有不友好型，由于人类和大自然和谐相处以及可持续发展的需要,国内外学者开始积极探索无铅化的压电陶瓷。Piezoelectric ceramics are functional ceramic materials capable of interconverting mechanical and electrical energy, and are widely used in military, automotive, commercial and medical technology fields. Since lead-based piezoelectric ceramics have a large piezoelectric constant and can be modified by doping to adjust performance to meet different application requirements, lead-based piezoelectric ceramics are still the main functional ceramics in applications. , mainly Pb(Ti,Zr)O3 (PZT), PbTiO3 -PbZrO3 -ABO3 (ABO3 is a composite perovskite ferroelectric) and PbTiO3 . However, because lead is toxic and unfriendly to the environment, due to the harmonious coexistence between human beings and nature and the need for sustainable development, scholars at home and abroad have begun to actively explore lead-free piezoelectric ceramics.
铌酸盐基（KNN）无铅压电陶瓷是在20世纪60年代左右首先发展研究。其化学通式为ABO3(A为K、Na；B为Nb、Ta、Sb等)。铌酸盐基无铅压电陶瓷具有较高的居里点，机械品质因数和介电常数都比较低，声传播速度较大。然而,KNN压电陶瓷的缺点,在高温时烧结由于K,Na元素的挥发，导致化学计量比的偏离，很难通过传统的烧结方法得到致密性很大的陶瓷体。为了克服纯KNN陶瓷的上述缺陷、优化它的压电性能,主要集中在以下两个方面:(1)组分掺杂改性;(2)制备工艺与织构改性来改进。Niobate-based (KNN) lead-free piezoelectric ceramics were first developed and researched around the 1960s. Its general chemical formula is ABO3 (A is K, Na; B is Nb, Ta, Sb, etc.). Niobate-based lead-free piezoelectric ceramics have a high Curie point, low mechanical quality factor and dielectric constant, and high sound propagation velocity. However, the disadvantage of KNN piezoelectric ceramics is that the sintering at high temperature is due to the volatilization of K and Na elements, which leads to the deviation of the stoichiometric ratio, and it is difficult to obtain a dense ceramic body by traditional sintering methods. In order to overcome the above-mentioned defects of pure KNN ceramics and optimize its piezoelectric properties, the following two aspects are mainly concentrated: (1) component doping modification; (2) preparation process and texture modification to improve.
目前制备铌酸钠钾基粉末的方法有水热法、溶胶-凝胶法、固相反应法、熔盐法、共沉淀法等方法。很多传统的方法在制备的过程中对条件的要求都比较苛刻，且生成的粉末颗粒直径也比较大，固相法容易造成粒子之间的烧结板结且粒度颗粒大不均匀，因而不能达到纳米级别的要求。水热法可以直接制备粉体，省掉了传统固相烧结工艺必须经过的预烧阶段，工艺简单。水热反应的温度比较低(200℃左右即可，溶胶-凝胶法通常在600℃以上)，所以更加环保节能。另外，水热法制备的粉体，颗粒均匀，纯度高，省时省力。At present, methods for preparing sodium-potassium niobate-based powder include hydrothermal method, sol-gel method, solid-phase reaction method, molten salt method, co-precipitation method and the like. Many traditional methods have strict requirements on the conditions during the preparation process, and the diameter of the generated powder particles is also relatively large. The solid-phase method is easy to cause sintering and compaction between the particles and the particle size is uneven, so it cannot reach the nanometer level. requirements. The hydrothermal method can directly prepare powder, which saves the pre-sintering stage that must be passed through the traditional solid-state sintering process, and the process is simple. The temperature of the hydrothermal reaction is relatively low (about 200°C, and the sol-gel method is usually above 600°C), so it is more environmentally friendly and energy-saving. In addition, the powder prepared by the hydrothermal method has uniform particles, high purity, and saves time and effort.
发明内容Contents of the invention
面对现有技术存在的问题，本发明旨在提供一种同时具有制备工艺简单和较高压电性能的铌酸钾钠基压电陶瓷。Facing the problems existing in the prior art, the present invention aims to provide potassium sodium niobate-based piezoelectric ceramics with simple preparation process and high piezoelectric performance.
本发明提供的一种铌酸钾钠基压电陶瓷材料的化学组成为KaNabNbxSbyO3，其中0.2<a≤0.8，0.2<b≤0.8，0.6<x≤1，0<x≤0.4。The chemical composition of a potassium sodium niobate-based piezoelectric ceramic material provided by the present invention is Ka Nab Nbx Sby O3 , wherein 0.2<a≤0.8, 0.2<b≤0.8, 0.6<x≤1,0 <x≤0.4.
本发明按照化学组成，实验步骤如下：According to the chemical composition of the present invention, the experimental steps are as follows:
(1)按照化学组成，将原料按照摩尔百分比计算出各自所需质量，采用水热法，将原料放入聚四氟乙烯的反应釜内胆，搅拌均匀，在温度180-220℃，保温20-40小时，进行铌酸盐的合成；(1) According to the chemical composition, calculate the required mass of the raw materials according to the molar percentage, and use the hydrothermal method to put the raw materials into the polytetrafluoroethylene reactor liner, stir evenly, and keep the temperature at 180-220°C for 20 -40 hours, carry out the synthesis of niobate;
(2)抽滤、干燥后的粉末，加入适量5%的聚乙烯醇造粒陈化；(2) The powder after suction filtration and drying is added with an appropriate amount of 5% polyvinyl alcohol to granulate and age;
(3)将颗粒装入Φ10-20mm的模具中，压制成型；(3) Pack the granules into a mold of Φ10-20mm, and press to form;
(4)陶瓷片排胶温度为450-550℃，排胶时间1-8小时；(4) The degumming temperature of the ceramic sheet is 450-550°C, and the degumming time is 1-8 hours;
(5)将排胶后的陶瓷片放入高温炉，用刚玉粉埋烧，烧结温度为900-1100℃，保温时间1-4小时；(5) Put the degummed ceramic sheet into a high-temperature furnace, bury and burn it with corundum powder, the sintering temperature is 900-1100°C, and the holding time is 1-4 hours;
(6)将铌酸钾钠基压电陶瓷片被银，极化，极化温度为100-200℃，时间为10-30分钟，电压为1-8kv/mm，完成极化1至2天后，对陶瓷片进行性能测试。(6) Polarize the potassium sodium niobate-based piezoelectric ceramic sheet with silver, the polarization temperature is 100-200°C, the time is 10-30 minutes, the voltage is 1-8kv/mm, and the polarization is completed 1 to 2 days later , to test the performance of the ceramic sheet.
本发明提出的铌酸钾钠基压电陶瓷具有如下优点：The potassium sodium niobate base piezoelectric ceramics proposed by the present invention has the following advantages:
(1)环境友好型材料，不含铅等有害成分，环保；(1) Environmentally friendly materials, free of harmful components such as lead, and environmentally friendly;
(2)陶瓷粉体制备简单，不需要通过观察反应现象来判别反应程度，操作方便，省时省力；(2) The preparation of ceramic powder is simple, and there is no need to judge the degree of reaction by observing the reaction phenomenon, which is convenient to operate and saves time and effort;
(3)较好的压电性能，压电常数d33能达到73pC/N。(3) Good piezoelectric performance, the piezoelectric constant d33 can reach 73pC/N.
附图说明Description of drawings
图1为本发明的一个示例陶瓷材料的X射线衍射图谱。Fig. 1 is an X-ray diffraction pattern of an exemplary ceramic material of the present invention.
图2为本发明的一个示例陶瓷材料的扫描电子显微镜照片。Figure 2 is a scanning electron micrograph of an exemplary ceramic material of the present invention.
具体实施方式detailed description
本发明中的压电陶瓷样品，采取水热法制备陶瓷粉体，常压烧结工艺，其过程包括粉体制备、造粒陈化、压片、烧结、被银、极化等工艺流程。具体为：The piezoelectric ceramic sample in the present invention adopts hydrothermal method to prepare ceramic powder, and the normal pressure sintering process includes powder preparation, granulation and aging, tableting, sintering, silvering, polarization and other technological processes. Specifically:
(1)按照化学组成，将原料按照摩尔百分比计算出各自所需质量，采用水热法，将原料放入聚四氟乙烯的反应釜内胆，搅拌均匀，在温度180-220℃，保温20-40小时，进行铌酸盐的合成；(1) According to the chemical composition, calculate the required mass of the raw materials according to the molar percentage, and use the hydrothermal method to put the raw materials into the polytetrafluoroethylene reactor liner, stir evenly, and keep the temperature at 180-220°C for 20 -40 hours, carry out the synthesis of niobate;
(2)抽滤、干燥后的粉末，加入适量5%的聚乙烯醇造粒陈化；(2) The powder after suction filtration and drying is added with an appropriate amount of 5% polyvinyl alcohol to granulate and age;
(3)将颗粒装入Φ10-20mm的模具中，压制成型；(3) Pack the granules into a mold of Φ10-20mm, and press to form;
(4)陶瓷片排胶温度为450-550℃，排胶时间1-8小时；(4) The degumming temperature of the ceramic sheet is 450-550°C, and the degumming time is 1-8 hours;
(5)将排胶后的陶瓷片放入高温炉，用刚玉粉埋烧，烧结温度为900-1100℃，保温时间1-4小时；(5) Put the degummed ceramic sheet into a high-temperature furnace, bury and burn it with corundum powder, the sintering temperature is 900-1100°C, and the holding time is 1-4 hours;
(6)将铌酸钾钠基压电陶瓷片被银，极化，极化温度为100-200℃，时间为10-30分钟，电压为1-8kv/mm，完成极化1至2天后，对陶瓷片进行性能测试。(6) Polarize the potassium sodium niobate-based piezoelectric ceramic sheet with silver, the polarization temperature is 100-200°C, the time is 10-30 minutes, the voltage is 1-8kv/mm, and the polarization is completed 1 to 2 days later , to test the performance of the ceramic sheet.
下面结合具体实施例对本发明的内容作进一步详细说明，但本发明不限于以下列举的特定例子。The content of the present invention will be further described in detail below in conjunction with specific embodiments, but the present invention is not limited to the specific examples listed below.
实施例1Example 1
(1)按照通式KaNabNbxSbyO3取a=0.5，b=0.5，x=1，y=0，采用AR或4N级的KOH、NaOH、Nb2O3、Sb2O3为原料，按上式化学计量称量。采用水热法，将原料放入聚四氟乙烯的反应釜内胆，加入蒸馏水搅拌均匀，在温度180℃，保温24小时，进行铌酸盐的合成；(1) According to the general formula Ka Nab Nbx Sby O3 , take a=0.5, b=0.5, x=1, y=0, and use AR or 4N grade KOH, NaOH, Nb2 O3 , Sb2 O3 is the raw material, weighed stoichiometrically according to the above formula. Using the hydrothermal method, put the raw materials into the polytetrafluoroethylene reactor liner, add distilled water and stir evenly, and keep the temperature at 180°C for 24 hours to synthesize niobate;
(2)抽滤、干燥后的粉末，加入适量5%的聚乙烯醇造粒陈化；(2) The powder after suction filtration and drying is added with an appropriate amount of 5% polyvinyl alcohol to granulate and age;
(3)将颗粒装入Φ10mm的模具中，压制成型；(3) Pack the granules into a mold of Φ10mm and press them into shape;
(4)陶瓷片排胶温度为500℃，排胶时间1小时；(4) The debinding temperature of the ceramic sheet is 500°C, and the debinding time is 1 hour;
(5)将排胶后的陶瓷片放入高温炉，用刚玉粉埋烧，烧结温度为1060℃，保温时间2小时；(5) Put the degummed ceramic sheet into a high-temperature furnace, bury and burn it with corundum powder, the sintering temperature is 1060°C, and the holding time is 2 hours;
(6)将铌酸钾钠基压电陶瓷片被银，极化，极化温度为120℃，时间为15分钟，电压为3kv/mm，完成极化1天后，对陶瓷片进行性能测试。(6) The sodium potassium niobate-based piezoelectric ceramic sheet was silver-coated and polarized. The polarization temperature was 120° C. for 15 minutes and the voltage was 3 kv/mm. After the polarization was completed for 1 day, performance tests were performed on the ceramic sheet.
实施例2Example 2
(1)按照通式KaNabNbxSbyO3取a=0.5，b=0.5，x=0.96，y=0.04，采用AR或4N级的KOH、NaOH、Nb2O3、Sb2O3为原料，按上式化学计量称量。采用水热法，将原料放入聚四氟乙烯的反应釜内胆，加入蒸馏水搅拌均匀，在温度200℃，保温24小时，进行铌酸盐的合成；(1) According to the general formula Ka Nab Nbx Sby O3 , take a=0.5, b=0.5, x=0.96, y=0.04, and use AR or 4N grade KOH, NaOH, Nb2 O3 , Sb2 O3 is the raw material, weighed stoichiometrically according to the above formula. Using the hydrothermal method, put the raw materials into the liner of the polytetrafluoroethylene reactor, add distilled water and stir evenly, and keep the temperature at 200 ° C for 24 hours to synthesize niobate;
(2)抽滤、干燥后的粉末，加入适量5%的聚乙烯醇造粒陈化；(2) The powder after suction filtration and drying is added with an appropriate amount of 5% polyvinyl alcohol to granulate and age;
(3)将颗粒装入Φ10mm的模具中，压制成型；(3) Pack the granules into a mold of Φ10mm and press them into shape;
(4)陶瓷片排胶温度为500℃，排胶时间1小时；(4) The debinding temperature of the ceramic sheet is 500°C, and the debinding time is 1 hour;
(5)将排胶后的陶瓷片放入高温炉，用刚玉粉埋烧，烧结温度为1040℃，保温时间2小时；(5) Put the degummed ceramic sheet into a high-temperature furnace, bury and burn it with corundum powder, the sintering temperature is 1040°C, and the holding time is 2 hours;
(6)将铌酸钾钠基压电陶瓷片被银，极化，极化温度为120℃，时间为15分钟，电压为3kv/mm，完成极化1天后，对陶瓷片进行性能测试。(6) The sodium potassium niobate-based piezoelectric ceramic sheet was silver-coated and polarized. The polarization temperature was 120° C. for 15 minutes and the voltage was 3 kv/mm. After the polarization was completed for 1 day, performance tests were performed on the ceramic sheet.
实施例3Example 3
(1)按照通式KaNabNbxSbyO3取a=0.5，b=0.5，x=0.96，y=0.04，采用AR或4N级的KOH、NaOH、Nb2O3、Sb2O3为原料，按上式化学计量称量。采用水热法，将原料放入聚四氟乙烯的反应釜内胆，加入蒸馏水搅拌均匀，在温度200℃，保温24小时，进行铌酸盐的合成；(1) According to the general formula Ka Nab Nbx Sby O3 , take a=0.5, b=0.5, x=0.96, y=0.04, and use AR or 4N grade KOH, NaOH, Nb2 O3 , Sb2 O3 is the raw material, weighed stoichiometrically according to the above formula. Using the hydrothermal method, put the raw materials into the liner of the polytetrafluoroethylene reactor, add distilled water and stir evenly, and keep the temperature at 200 ° C for 24 hours to synthesize niobate;
(2)抽滤、干燥后的粉末，加入适量5%的聚乙烯醇造粒陈化；(2) The powder after suction filtration and drying is added with an appropriate amount of 5% polyvinyl alcohol to granulate and age;
(3)将颗粒装入Φ10mm的模具中，压制成型；(3) Pack the granules into a mold of Φ10mm and press them into shape;
(4)陶瓷片排胶温度为500℃，排胶时间1小时；(4) The debinding temperature of the ceramic sheet is 500°C, and the debinding time is 1 hour;
(5)将排胶后的陶瓷片放入高温炉，用刚玉粉埋烧，烧结温度为1080℃，保温时间4小时；(5) Put the degummed ceramic sheet into a high-temperature furnace, bury and burn it with corundum powder, the sintering temperature is 1080°C, and the holding time is 4 hours;
(6)将铌酸钾钠基压电陶瓷片被银，极化，极化温度为120℃，时间为15分钟，电压为3kv/mm，完成极化1天后，对陶瓷片进行性能测试。(6) The sodium potassium niobate-based piezoelectric ceramic sheet was silver-coated and polarized. The polarization temperature was 120° C. for 15 minutes and the voltage was 3 kv/mm. After the polarization was completed for 1 day, performance tests were performed on the ceramic sheet.
实施例4Example 4
(1)按照通式KaNabNbxSbyO3取a=0.46，b=0.54，x=0.93，y=0.07，采用AR或4N级的KOH、NaOH、Nb2O3、Sb2O3为原料，按上式化学计量称量。采用水热法，将原料放入聚四氟乙烯的反应釜内胆，加入蒸馏水搅拌均匀，在温度200℃，保温24小时，进行铌酸盐的合成；(1) Take a=0.46, b=0.54, x=0.93, y=0.07 according to the general formula Ka Nab Nbx Sby O3 , and use AR or 4N grade KOH, NaOH, Nb2 O3 , Sb2 O3 is the raw material, weighed stoichiometrically according to the above formula. Using the hydrothermal method, put the raw materials into the liner of the polytetrafluoroethylene reactor, add distilled water and stir evenly, and keep the temperature at 200 ° C for 24 hours to synthesize niobate;
(2)抽滤、干燥后的粉末，加入适量5%的聚乙烯醇造粒陈化；(2) The powder after suction filtration and drying is added with an appropriate amount of 5% polyvinyl alcohol to granulate and age;
(3)将颗粒装入Φ10mm的模具中，压制成型；(3) Pack the granules into a mold of Φ10mm and press them into shape;
(4)陶瓷片排胶温度为500℃，排胶时间1小时；(4) The debinding temperature of the ceramic sheet is 500°C, and the debinding time is 1 hour;
(5)将排胶后的陶瓷片放入高温炉，用刚玉粉埋烧，烧结温度为1060℃，保温时间2小时；(5) Put the degummed ceramic sheet into a high-temperature furnace, bury and burn it with corundum powder, the sintering temperature is 1060°C, and the holding time is 2 hours;
(6)将铌酸钾钠基压电陶瓷片被银，极化，极化温度为120℃，时间为15分钟，电压为3kv/mm，完成极化1天后，对陶瓷片进行性能测试；(6) The sodium potassium niobate-based piezoelectric ceramic sheet was silver-coated, polarized, the polarization temperature was 120°C, the time was 15 minutes, and the voltage was 3kv/mm. After the polarization was completed for 1 day, the performance test was performed on the ceramic sheet;
图1是其X射线衍射图谱，图2是其扫描电镜照片。Fig. 1 is its X-ray diffraction pattern, and Fig. 2 is its scanning electron micrograph.
在烧结温度1060℃，保温时间2小时，按照通式KaNabNbxSbyO3取a=0.46，b=0.54，x=0.96，y=0.04，制备的陶瓷性能最优d33达到73pC/N，密度为4.39g/cm2。At a sintering temperature of 1060°C and a holding time of 2 hours, a = 0.46, b = 0.54, x = 0.96, y = 0.04 according to the general formula Ka Nab Nbx Sby O3 , the optimal performance of the prepared ceramics d33 reaches 73pC/N, the density is 4.39g/cm2 .
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