Piezoelectric ceramic material with electrostrictive strain with low hysteresis and wide temperature range stability in low electric field and preparation method and application thereof

Abstract

The invention discloses a piezoelectric ceramic material with low hysteresis and wide temperature range stability electrostrictive strain in a low electric field and a preparation method and application thereof, and belongs to the technical field of functional ceramic materials. The piezoelectric ceramic material is prepared by combining a traditional solid-phase reaction method with a two-step method. The method mainly comprises the following steps: weighing raw materials, ball-milling, calcining, granulating, forming, degumming and sintering. The chemical composition of the piezoelectric ceramic material is xSm-yPbHfO3-zPb (Sc1 / 2Ta1 / 2) O3-(1-y-z) PbTiO3 (Sm-PH-PST-PT), x is larger than or equal to 0 and smaller than or equal to 0.03, y is larger than or equal to 0.25 and smaller than or equal to 0.5, and z is larger than or equal to 0.05 and smaller than or equal to 0.31. According to the piezoelectric ceramic material, through component optimization and microstructure regulation and control, the unipolar strain fluctuation rate in a wide temperature range (25 DEG C to 200 DEG C) under a low electric field of 2kV / mm is smaller than or equal to 4.4%, excellent temperature stability is shown, the application requirements of a piezoelectric actuator in a wide temperature range and at a high temperature can be met, and the piezoelectric ceramic material has remarkable application value.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of piezoelectric ceramic preparation, and particularly relates to a piezoelectric ceramic material with low hysteresis and wide temperature stability electric strain under low electric field and a preparation method and application thereof. BACKGROUND

[0002] Piezoelectric ceramic materials can realize the mutual conversion between mechanical energy and electric energy due to their unique effects, become an important functional material, and are widely used in the fields of sensors, transducers, actuators and the like. A piezoelectric actuator is an electromechanical converter based on the inverse piezoelectric effect, which can generate accurate displacement or force by applying an electric field, and its core advantage lies in high precision, fast response, miniaturization and electromagnetic compatibility. It is widely used in the fields of industrial manufacturing, medical health, energy environment and consumer electronics.

[0003] In lead-based piezoelectric ceramic materials, PZT-based piezoelectric ceramics become the most widely used piezoelectric material due to their excellent piezoelectric properties and relatively mature preparation process. For example, a PZT-based piezoelectric ceramic material with large electric strain under low electric field and high Curie temperature is disclosed in Chinese Patent Publication No. CN119912259A, which has a chemical composition of Pb1-2n-1.5xLaxSrnBan(ZryTi1-y)O3-zwt%Sn. Through the composite doping of La, Sr, Ba and the like, the performance characteristics of large electric strain under low electric field and high Curie temperature are realized. In recent years, lead scandium tantalate lead titanate (PST-PT) series piezoelectric ceramics have attracted widespread attention due to their excellent piezoelectric properties and electric strain characteristics. For example, a lanthanum-doped lead scandium tantalate lead titanate piezoelectric ceramic (CN115636667A) is disclosed in Chinese Patent Publication No. CN115636667A, which has a chemical composition of yLa-(1-x)Pb(Sc1 / 2Ta1 / 2)O3-xPbTiO3. Through the doping of La element, the performance indexes of high piezoelectric coefficient, high electromechanical coupling coefficient, large strain response, low strain hysteresis and high temperature stability are realized. In the aspect of lead-free piezoelectric ceramic materials, barium titanate-based piezoelectric ceramics also attract attention due to their environmental protection characteristics. For example, a doped barium titanate lead-free ceramic with high electric strain and low hysteresis is disclosed in Chinese Patent Publication No. CN115093216A, which has a chemical formula of BaTi1-xSnxO3. Through the doping of Sn 4+ , the performance characteristics of high electric strain and low hysteresis are realized, but the Curie temperature is relatively low, which limits its application in high temperature environments.

[0004] It can be seen that the strain performance of piezoelectric ceramic material for piezoelectric actuator mainly has three key indicators of strain value, hysteresis and temperature stability. Among them, the strain value determines the output capacity of the actuator, the hysteresis affects the precision, and the temperature stability guarantees the adaptability of working conditions. Usually, the electric field applied to the piezoelectric material often reaches the level of 4kV / mm or more, resulting in a high driving voltage of the piezoelectric actuator; due to the mechanism of microstructure transformation and phase change, the hysteresis of most piezoelectric materials is large, so that the response of the piezoelectric actuator is not timely; many piezoelectric materials also have poor stable temperature performance. On the one hand, the characteristics of piezoelectric materials are affected by the temperature change caused by the heat generated by dielectric loss and mechanical loss, so the reliability of the device in service depends largely on the strain temperature stability of the material, on the other hand, in special fields such as aerospace and oil and gas exploration, the upper limit of the working temperature of the device has reached 200 o C or more, therefore, it is of great significance to develop a piezoelectric ceramic material with low hysteresis and wide temperature stability of electric strain under low electric field, which meets the needs of modern high-performance piezoelectric devices. SUMMARY

[0005] In order to overcome the above-mentioned defects of the prior art, the purpose of the present application is to provide a piezoelectric ceramic material with low hysteresis and wide temperature stability of electric strain under low electric field and its preparation method, which has high strain response and low hysteresis, and lays a solid material foundation for the design of piezoelectric actuator with excellent stability in a wide temperature range.

[0006] In order to achieve the above-mentioned purpose, the present application adopts the following technical scheme: The present application discloses a piezoelectric ceramic material with low hysteresis and wide temperature stability of electric strain under low electric field, which is a rare earth Sm element doped PH-PST-PT ternary piezoelectric ceramic, and its chemical composition is xSm-yPbHfO3-zPb(Sc 1 / 2 Ta 1 / 2 )O3-(1-y-z)PbTiO3(Sm-PH-PST-PT), wherein 0≤x≤0.03, 0.25≤y≤0.5, 0.05≤z≤0.31.

[0007] Preferably, the piezoelectric coefficient of the piezoelectric ceramic is 155-614pC / N, the unipolar strain is 0.103%-0.186%, the strain hysteresis is 14.78%-21.83%, the Curie temperature is 225 o C-306 o C, the room temperature dielectric constant is 928-2849, the remanent polarization is 16.86-33.00μC / cm 2 , and the coercive field is 0.54-1.30kV / mm.

[0008] The application further discloses a preparation method of the piezoelectric ceramic material with low hysteresis and wide temperature range stability under low electric field. 1) ingredients are weighed according to the stoichiometric ratio of xSm-yPbHfO3-zPb(Sc 1 / 2 Ta 1 / 2 )O3-(1-x-y)PbTiO3(Sm-PH-PST-PT), wherein 0<=x<=0.03, 0.25<=y<=0.5, 0.05<=z<=0.31, and the raw materials of Sm2O3, HfO2, ScTaO4, TiO2 and PbO are ball-milled uniformly, to obtain a mixture, and then the mixture is dried and ground for standby use; 2) the mixture treated in step 1) is pre-fired to obtain Sm-PH-PST-PT pre-fired powder with pure perovskite phase, and then the pre-fired powder is secondarily ball-milled and dried to obtain pre-fired powder; 3) the pre-fired powder after secondary ball-milling is granulated, sieved and pressed into a green sheet, and the green sheet is degassed and sintered to obtain Sm-PH-PST-PT ternary piezoelectric ceramic.

[0009] Preferably, in step 1), the ScTaO4 precursor is prepared according to the following method: the raw materials of Sc2O3 and Ta2O5 are weighed according to the stoichiometric ratio of ScTaO4, ball-milled uniformly, dried and ground, and then calcined at 1300-1400 o C for 2-4 h to obtain the ScTaO4 precursor; Preferably, in step 1), the ball-milling speed is 250-280 rpm, the ball-milling time is 24 h, and the drying temperature is 70-90 o C.

[0010] Preferably, in step 2), the pre-firing temperature is 850-900 o C, the pre-firing time is 2-4 h, the secondary ball-milling speed is 250-280 rpm, the secondary ball-milling time is 12 h, and the drying temperature is 70-90 o C.

[0011] Preferably, in step 3), the pre-fired powder is granulated by using a polyvinyl alcohol aqueous solution with a mass fraction of 5%, the addition amount of the polyvinyl alcohol aqueous solution is 5%-10% of the mass of the pre-fired powder, and the mesh size of the sieve used for sieving is 80-100 mesh.

[0012] Preferably, in step 3), the degassing temperature is 550 o C, the degassing time is 2 h, and the heating rate during the degassing process is 1 o C / min.

[0013] Preferably, in step 3), the sintering treatment temperature is 1200-1300 o C, the heating rate during sintering is 3 o C / min, and the holding time is 2 h.

[0014] The application further discloses application of the piezoelectric ceramic material with low hysteresis and wide temperature range stability in preparation of high-performance electromechanical devices.

[0015] Compared with the prior art, the application has the following beneficial effects: The piezoelectric ceramic material with low hysteresis and wide temperature range stability disclosed by the application has the following advantages: First, by means of MPB component design and rare earth Sm element doping for microstructure regulation, a new ternary piezoelectric ceramic material system, i.e., Sm-PH-PST-PT ternary piezoelectric ceramic, is formed, and single-pole strain fluctuation rate ≤4.4% in a wide temperature range (25 o C to 200 o C) under low electric field (2 kV / mm) is realized, and excellent temperature stability is shown; Second, the piezoelectric ceramic material has excellent piezoelectric performance, the piezoelectric coefficient is 155-614 pC / N, the single-pole strain is 0.103%-0.186%, and the strain hysteresis is 14.78%-21.83%, which is obviously lower than that of traditional piezoelectric materials, and the problem of slow response caused by large hysteresis of the existing piezoelectric materials is solved; Third, the piezoelectric ceramic material has a Curie temperature of 225-306℃, a room temperature dielectric constant of 928-2849, a remanent polarization of 16.86-33.00 μC / cm², and a coercive field of 0.54-1.30 kV / mm, and has wide temperature range stability, which meets the demand of high-temperature application in special fields; Therefore, the piezoelectric ceramic material has the electric strain characteristics of low hysteresis and wide temperature range stability under low electric field, and is very suitable for application in high-performance piezoelectric devices such as actuators, sensors and transducers BRIEF DESCRIPTION OF DRAWINGS Figure 1 It is a ternary phase diagram of the piezoelectric ceramic material of the application; Figure 2 It is an X-ray crystal diffraction spectrum of the piezoelectric ceramic material prepared by the application; wherein a is a pure system along MPB 5 components; b is a system with PT changed; and c is different Sm doping contents; Figure 3 It is a curve of dielectric constant of the piezoelectric ceramic prepared in Example 10 changing with temperature at a frequency of 1 kHz; Figure 4Piezoelectric ceramic prepared in Example 10, room temperature polarization intensity as a function of electric field; Figure 5 Piezoelectric ceramic prepared in Example 10, room temperature monopolar strain as a function of electric field; Figure 6 Piezoelectric ceramic prepared in Example 10, monopolar strain as a function of temperature at 2kV / mm electric field. DETAILED DESCRIPTION

[0016] In order to make the person skilled in the art better understand the technical scheme of the present application, the technical scheme in the embodiments of the present application will be described clearly and completely below in conjunction with the drawings in the embodiments of the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by the person skilled in the art without creative labor should belong to the protection scope of the present application.

[0017] It should be noted that the terms "first", "second" and the like in the specification and claims of the present application and the above-described drawings are used to distinguish similar objects, and do not necessarily indicate a specific order or a chronological sequence. It should be understood that the data thus used can be interchanged under appropriate circumstances, so that the embodiments of the present application described herein can be implemented in an order other than that illustrated or described herein. In addition, the terms "include" and "have" and any variations thereof are intended to cover non-exclusive inclusion, for example, a process, method, system, product or device including a series of steps or units does not have to be limited to only those steps or units clearly listed, but can include other steps or units not clearly listed or inherent to these processes, methods, products or devices.

[0018] The present application discloses a piezoelectric ceramic material with low hysteresis and wide temperature stability of electric strain under low electric field, which has a chemical composition of xSm-yPbHfO3-zPb(Sc 1 / 2 Ta 1 / 2 )O3-(1-y-z)PbTiO3(Sm-PH-PST-PT), wherein 0≤x≤0.03, 0.25≤y≤0.5, 0.05≤z≤0.31.

[0019] The present application discloses a piezoelectric ceramic material with low hysteresis and wide temperature stability of electric strain under low electric field and a preparation method thereof, which comprises the following steps: 1) Sc2O3 and Ta2O5 raw materials are accurately weighed according to the stoichiometric ratio of ScTaO4, then mixed by ball milling, dried and ground, put into a corundum crucible, compacted and calcined to obtain a ScTaO4 precursor.

[0020] 2) According to the stoichiometric ratio of xSm-yPbHfO3-zPb(Sc 1 / 2 Ta 1 / 2 )O3-(1-y-z)PbTiO3(Sm-PH-PST-PT), wherein 0≤x≤0.03, 0.25≤y≤0.5, 0.05≤z≤0.31, Sm2O3, HfO2, ScTaO4, TiO2, PbO are weighed into a ball mill jar and anhydrous ethanol is added as a ball milling medium for primary ball milling.

[0021] 3) The mixture after ball milling in 2) is dried in an oven and then ground, and is put into a crucible for pre-sintering to obtain Sm-PH-PST-PT pre-sintered powder with a pure perovskite phase structure.

[0022] 4) The pre-sintered powder obtained in 3) is subjected to secondary ball milling and then dried in an oven.

[0023] 5) A certain amount of the pre-sintered powder after secondary ball milling is weighed, polyvinyl alcohol (PVA) aqueous solution is added for granulation and sieving, and a green sheet with a certain shape and size is pressed.

[0024] 6) The green sheet is subjected to degassing treatment, and then sintering densification is performed on the degassed green sheet to obtain a Sm-PH-PST-PT ceramic sheet.

[0025] The Sm-PH-PST-PT ceramic sheet after sintering is subjected to subsequent sample preparation and electrical property testing, including: The ceramic sheet is ground to a certain thickness, and the upper and lower surfaces are treated to make electrodes.

[0026] The ceramic sheet after electrode application is polished with sandpaper to remove the excess electrodes on the edges, and then is subjected to polarization treatment and aging for 24 h, and is subjected to electrical property testing, with polarization for 60 min at room temperature and a polarization electric field of 3 kV / mm.

[0027] The present application is described below in combination with the drawings and specific examples: Example 1 4.7604g of Sc2O3 (99.9%) and 15.2396g of Ta2O5 (99.99%) are weighed into a ball mill jar, and are ball milled on a planetary ball mill (Nanjing University Instrument Factory QM-3SP2) at a speed of 280 revolutions per minute for 24 h, and then are placed in an oven at 80 o C for drying treatment, and then are calcined in a muffle furnace at a temperature of 1300-1400 o C for 2-4 h to obtain a ScTaO4 precursor.

[0028] According to the stoichiometric ratio of 0.300PH-0.224PST-0.476PT, 2.6503g of HfO2(99.99%), 1.3764g of ScTaO4, 1.5973g of TiO2(99.99%) and 9.5635g of PbO(99.9%) were weighed into a ball mill jar and 20mL of anhydrous ethanol was added, and the mixed slurry was ball milled on a planetary ball mill at a speed of 280r / min for 24h, and then the ball-mixed slurry was dried in an oven at 80 o C.

[0029] The dried mixed powder was ground, and then placed in a corundum crucible and compacted, and the crucible was placed in a muffle furnace and heated to 900 o C at a heating rate of 3 o C / min, and 0.300PH-0.224PST-0.476PT pre-fired powder was obtained after holding for 2h, and then the pre-fired powder was crushed and ground again and placed in a ball mill jar for 12h, and finally dried in an oven.

[0030] 6g of 0.300PH-0.224PST-0.476PT ceramic powder was weighed into a mortar, and about 0.6g of PVA solution was added in multiple times for granulation, and the powder particles were repeatedly ground and sieved (80 mesh) to ensure that the powder particles were uniformly sized and fully granulated.

[0031] 0.75g of the granulated powder was weighed into a die with a diameter of 10mm for tabletting, and the green tablet obtained by pressing was placed in a muffle furnace and slowly heated to 550 o C at a heating rate of 1 o C / min, and degassing was performed for 2h.

[0032] After degassing, the green tablet was placed in a 30mL small crucible and buried with the same component of the second ball-milled powder, and placed in a high-temperature furnace and heated to 1200~1300 o C at a heating rate of 3 o C / min, and held for 2h to obtain dense 0.300PH-0.224PST-0.476PT ceramic tablets.

[0033] Then the dense 0.300PH-0.224PST-0.476PT ceramic tablets after sintering were ground to a thickness of 0.7mm, and an electrode was plated by treatment, and then the excess electrode on the edge was polished off, and finally the electrical performance test was performed after polarization for 60min at room temperature and aging for 24h.

[0034] The piezoelectric ceramic of 0.300PH-0.224PST-0.476PT prepared in the embodiment has the following characteristics: piezoelectric coefficient of 243pC / N, unipolar strain of 0.103%, strain hysteresis of 21.83%, Curie temperature of 270 o C, relative dielectric constant at room temperature of 1425, remanent polarization of 19.02μC / cm 2 , and coercive field of 0.56kV / mm.

[0035] Example 2 According to the stoichiometric ratio of 0.325PH-0.196PST-0.479PT, 2.8600g of HfO2(99.99%), 1.1996g of ScTaO4, 1.6011g of TiO2(99.89%) and 9.5261 of PbO(99.9%) were weighed into a ball mill jar and 20mL of anhydrous ethanol was added, and the mixture was ball milled on a planetary ball mill at a speed of 280r / min for 24h, and then the ball-mixed slurry was dried in an oven at 80 o C.

[0036] The dried mixed powder was ground, and then was placed in a corundum crucible and compacted, and the crucible was placed in a muffle furnace and heated to 900 o C at a heating rate of 3℃ / min, and after two hours of heat preservation, 0.325PH-0.196PST-0.479PT pre-sintered powder was obtained, and then the pre-sintered powder was crushed and ground and was again placed in a ball mill jar and ball milled for 12h, and finally was dried in an oven.

[0037] 6g of 0.325PH-0.196PST-0.479PT ceramic powder was weighed into a mortar, and about 0.6g of PVA solution was added in multiple times for granulation, and the powder particles were repeatedly ground and sieved (80 mesh) to ensure that the powder particles were uniform in size and fully granulated.

[0038] 0.75g of the granulated powder was weighed into a die with a diameter of 10mm for tabletting, and the green tablet obtained by tabletting was placed in a muffle furnace and slowly heated to 550 o C at a heating rate of 1 o C / min, and was heat preserved for 2h for degassing.

[0039] The green tablet after degassing was placed in a 30mL small crucible and was buried in a second ball-milled powder of the same composition, and was placed in a high-temperature furnace and heated to 1200~1300 o C at a heating rate of 3 o C / min, and was heat preserved for 2h to obtain dense 0.325PH-0.196PST-0.479PT ceramic tablets.

[0040] The sintered and densified 0.325PH-0.196PST-0.479PT ceramic sheet is then ground to a thickness of 0.7 mm, coated with electrodes by processing, and then the excess electrodes on the edges are polished off. Finally, the electrical performance test can be performed after the sheet is polarized at room temperature for 60 min and aged for 24 h.

[0041] The 0.325PH-0.196PST-0.479PT piezoelectric ceramic prepared in this example has the following characteristics: a piezoelectric coefficient of 287 pC / N, a unipolar strain of 0.113%, a strain hysteresis of 18.49%, a Curie temperature of 281 o C, a relative dielectric constant at room temperature of 1441, a remanent polarization of 19.17 μC / cm 2 , and a coercive field of 0.60 kV / mm.

[0042] Example 3 According to the stoichiometric ratio of 0.350PH-0.168PST-0.482PT, 3.0680 g of HfO2 (99.99%), 1.0242 g of ScTaO4, 1.6049 g of TiO2 (99.89%), and 9.4890 g of PbO (99.9%) are weighed into a ball mill jar and 20 mL of anhydrous ethanol is added. The mixture is ball milled on a planetary ball mill at a speed of 280 revolutions per minute for 24 h, and then the ball-mixed slurry is dried in an oven at 80 o C.

[0043] The dried mixed powder is ground, and then placed in a corundum crucible and compacted. The crucible is placed in a muffle furnace and heated to 900 o C at a heating rate of 3 o C / min, and held for 2 h to obtain 0.350PH-0.168PST-0.482PT pre-sintered powder. The pre-sintered powder is then crushed and ground and placed in a ball mill jar for 12 h, and finally dried in an oven.

[0044] 6 g of 0.350PH-0.168PST-0.482PT ceramic powder is weighed into a mortar, and about 0.6 g of PVA solution is added in multiple portions for granulation. The powder particles are repeatedly ground and sieved (80 mesh) to ensure that the powder particles are uniformly sized and fully granulated.

[0045] 0.75 g of the granulated powder is weighed into a die with a diameter of 10 mm to form a green sheet. The green sheet is placed in a muffle furnace and slowly heated to 550 o C at a heating rate of 1 o C / min, and held for 2 h to remove the binder.

[0046] After the glue is removed, the green sheet is placed in a 30 mL small crucible and buried with the same group of secondary ball-milled powder, placed in a high-temperature furnace at a rate of 3 o C / min to 1200~1300 o C, and heat treated for 2 h to obtain a dense 0.350PH-0.168PST-0.482PT ceramic sheet.

[0047] Then the sintered dense 0.350PH-0.168PST-0.482PT ceramic sheet is ground to a thickness of 0.7 mm, coated with an electrode by processing, and then the excess electrode on the edge is polished off. Finally, after polarization for 60 min at room temperature and aging for 24 h, the electrical performance test can be performed.

[0048] The 0.350PH-0.168PST-0.482PT piezoelectric ceramic prepared in this example has the following characteristics: piezoelectric coefficient of 377 pC / N, unipolar strain of 0.131%, strain hysteresis of 15.75%, Curie temperature of 285 o C, relative dielectric constant at room temperature of 1739, remanent polarization of 25.55 μC / cm 2 , and coercive field of 0.65 kV / mm.

[0049] Example 4 According to the stoichiometric ratio of 0.375PH-0.140PST-0.485PT, 3.2744 g of HfO2 (99.99%), 0.8502 g of ScTaO4, 1.6086 g of TiO2 (99.89%), and 9.4522 g of PbO (99.9%) are weighed into a ball mill jar and 20 mL of anhydrous ethanol is added. The mixture is ball-milled on a planetary ball mill at a speed of 280 revolutions / min for 24 h, and then the ball-milled slurry is dried in an oven at 80 o C.

[0050] The dried mixed powder is ground, then placed in a corundum crucible and compacted, and the crucible is placed in a muffle furnace at a rate of 3 o C / min to 900 o C, and heat treated for 2 h to obtain 0.375PH-0.140PST-0.485PT pre-sintered powder, which is then crushed and ground and placed in a ball mill jar for ball milling for 12 h, and finally dried in an oven.

[0051] 6 g of 0.375PH-0.140PST-0.485PT ceramic powder is weighed into a mortar, and about 0.6 g of PVA solution is added in multiple portions for granulation. The powder particles are repeatedly ground and sieved (80 mesh) to ensure uniform size and sufficient granulation.

[0052] 0.75g of the granulated powder was weighed into a 10mm diameter die for tabletting, and the green tablet obtained was placed in a muffle furnace at 1 o C / min to 550 o C for 2h to remove the binder.

[0053] The green tablet after binder removal was placed in a 30mL small crucible and buried with the same component of the second ball-milled powder, and placed in a high-temperature furnace at 3 o C / min to 1200~1300 o C for 2h to obtain dense 0.375PH-0.140PST-0.485PT ceramic tablets.

[0054] The sintered dense 0.375PH-0.140PST-0.485PT ceramic tablets were then ground to a thickness of 0.7mm, and an electrode was plated by treatment, after which the excess electrode on the edge was polished off, and finally the electrical performance test was carried out after polarization for 60min at room temperature and aging for 24h.

[0055] The 0.375PH-0.140PST-0.485PT piezoelectric ceramic prepared in this example has the following characteristics: piezoelectric coefficient of 342pC / N, unipolar strain of 0.114%, strain hysteresis of 15.47%, Curie temperature of 295 o C, room temperature relative dielectric constant of 1357, remanent polarization of 26.85μC / cm 2 , and coercive field of 0.66kV / mm.

[0056] Example 5 According to the stoichiometric ratio of 0.400PH-0.112PST-0.488PT, 3.4792g of HfO2(99.99%), 0.6776g of ScTaO4, 1.6123g of TiO2(99.89%) and 9.4156g of PbO(99.9%) were weighed into a ball mill jar and 20mL of anhydrous ethanol was added, and the mixture was ball-milled on a planetary ball mill at a speed of 280rpm for 24h, after which the ball-milled slurry was dried in an oven at 80 o C.

[0057] The mixed powder after drying was ground, and then placed in a corundum crucible and compacted, and the crucible was placed in a muffle furnace at 3 o C / min to 900 o C for 2h to obtain 0.400PH-0.112PST-0.488PT pre-sintered powder, which was then crushed and ground and placed in a ball mill jar for ball-milling for 12h, and finally dried in an oven.

[0058] Take 6g of 0.400PH-0.112PST-0.488PT ceramic powder into a mortar, add about 0.6g of PVA solution in multiple times for granulation, repeat multiple times of grinding and sieving (80 mesh) to ensure obtaining uniformly sized and fully granulated powder particles.

[0059] Take 0.75g of the granulated powder into a 10mm diameter die for tabletting, put the obtained green tablet into a muffle furnace at 1 o C / min to 550 o C for 2h for degassing.

[0060] After degassing, the green tablet is put into a 30mL small crucible and buried with the second ball-milled powder of the same composition, and placed in a high-temperature furnace at 3 o C / min to 1200~1300 o C for 2h to obtain dense 0.400PH-0.112PST-0.488PT ceramic tablets.

[0061] Then the sintered dense 0.400PH-0.112PST-0.488PT ceramic tablets are ground to a thickness of 0.7mm, coated with electrodes by processing, then the excess electrodes on the edges are polished off, and finally the electrical performance test can be carried out after polarization for 60min at room temperature and aging for 24h.

[0062] The 0.400PH-0.112PST-0.488PT piezoelectric ceramic prepared in this example has the following characteristics: piezoelectric coefficient of 317pC / N, unipolar strain of 0.107%, strain hysteresis of 17.26%, Curie temperature of 306 o C, room temperature relative dielectric constant of 1240, remanent polarization of 26.03μC / cm 2 , and coercive field of 0.68kV / mm.

[0063] Example 6 According to the stoichiometric ratio of 0.350PH-0.188PST-0.462PT, take 3.057g of HfO2(99.99%), 1.1420g of ScTaO4, 1.5326g of TiO2(99.89%) and 9.4541 of PbO(99.9%) into a ball mill jar and add 20mL of anhydrous ethanol, and ball mill the mixture on a planetary ball mill at a speed of 280r / min for 24h, then dry the ball-milled slurry in an oven at 80 o C.

[0064] Grind the dried mixed powder, then put it into a corundum crucible and compact it, put the crucible into a muffle furnace at 3o C / min to 900 o C for 2h to obtain 0.350PH-0.188PST-0.462PT pre-fired powder, then the pre-fired powder was crushed and ground again and placed in a ball mill for 12h, and finally dried in an oven.

[0065] 6g of 0.350PH-0.188PST-0.462PT ceramic powder was weighed into a mortar, and about 0.6g of PVA solution was added in multiple times for granulation, and repeatedly ground and sieved (80 mesh) to ensure that uniform and fully granulated powder particles were obtained.

[0066] 0.75g of the granulated powder was weighed into a die with a diameter of 10mm for tabletting, and the green tablet obtained was placed in a muffle furnace at 1 o C / min to 550 o C for 2h for degassing.

[0067] The degassed green tablet was placed in a 30mL small crucible and buried with the second ball-milled powder of the same composition, and placed in a high-temperature furnace at 3 o C / min to 1200~1300 o C for 2h to obtain dense 0.350PH-0.188PST-0.462PT ceramic tablets.

[0068] The sintered dense 0.350PH-0.188PST-0.462PT ceramic tablets were then ground to a thickness of 0.7mm, coated with electrodes by processing, and then the excess electrodes on the edges were polished off, and finally the electrical performance test was carried out after polarization for 60min at room temperature and aging for 24h.

[0069] The 0.350PH-0.188PST-0.462PT piezoelectric ceramic prepared in this example has the following characteristics: piezoelectric coefficient of 155pC / N, unipolar strain of 0.104%, strain hysteresis of 19.84%, Curie temperature of 275 o C, room temperature relative dielectric constant of 928, remanent polarization of 20.02μC / cm 2 , and coercive field of 0.54kV / mm.

[0070] Example 7 According to the stoichiometric ratio of 0.350PH-0.178PST-0.472PT, 3.0623g of HfO2(99.99%), 1.0832g of ScTaO4, 1.5687g of TiO2(99.89%) and 9.4715 of PbO(99.9%) were weighed into a ball mill jar and 20mL of anhydrous ethanol was added, and the mixed slurry was ball milled on a planetary ball mill at a speed of 280r / min for 24h, and then the ball-mixed slurry was placed in a 80 o C oven to dry.

[0071] The dried mixed powder was ground, and then placed in a corundum crucible and compacted, and the crucible was placed in a muffle furnace at a heating rate of 3 o C / min to 900 o C, and 0.350PH-0.178PST-0.472PT pre-fired powder was obtained after holding for 2h, and then the pre-fired powder was crushed and ground and placed in a ball mill jar for 12h, and finally dried in an oven.

[0072] 6g of 0.350PH-0.178PST-0.472PT ceramic powder was weighed into a mortar, and about 0.6g of PVA solution was added in multiple times for granulation, and the powder particles were repeatedly ground and sieved (80 mesh) to ensure uniform size and sufficient granulation.

[0073] 0.75g of the granulated powder was weighed into a die with a diameter of 10mm for tabletting, and the green tablet obtained by pressing was placed in a muffle furnace at a heating rate of 1 o C / min to 550 o C for 2h for degassing.

[0074] The green tablet after degassing was placed in a 30mL small crucible and buried with the same component of the second ball-milled powder, and placed in a high-temperature furnace at a heating rate of 3 o C / min to 1200~1300 o C for 2h to obtain dense 0.350PH-0.178PST-0.472PT ceramic tablets.

[0075] Then the dense 0.350PH-0.178PST-0.472PT ceramic tablets after sintering were ground to a thickness of 0.7mm, and an electrode was plated by processing, and then the excess electrode on the edge was polished off, and finally the electrical performance test was carried out after polarization for 60min at room temperature and aging for 24h.

[0076] The piezoelectric ceramic 0.350PH-0.178PST-0.472PT prepared in the embodiment has the following characteristics: piezoelectric coefficient of 178 pC / N, unipolar strain of 0.106%, strain hysteresis of 19.55%, Curie temperature of 280 o C, relative dielectric constant at room temperature of 1016, remanent polarization of 19.29 μC / cm 2 , and coercive field of 0.54 kV / mm.

[0077] Example 8 According to the stoichiometric ratio of 0.350PH-0.158PST-0.492PT, 3.0737 g of HfO2 (99.99%), 0.9651 g of ScTaO4, 1.6412 g of TiO2 (99.89%) and 9.5065 g of PbO (99.9%) were weighed into a ball mill jar and 20 mL of anhydrous ethanol was added, and the mixture was ball milled on a planetary ball mill at a speed of 280 revolutions per minute for 24 h, and then the ball-mixed slurry was dried in an oven at 80 o C.

[0078] The dried mixed powder was ground, and then was placed in a corundum crucible and compacted, and the crucible was placed in a muffle furnace and heated to 900 o C at a heating rate of 3 o C / min, and 0.350PH-0.158PST-0.492PT pre-sintered powder was obtained after holding for 2 h, and then the pre-sintered powder was crushed and ground and was again placed in a ball mill jar and ball milled for 12 h, and finally was dried in an oven.

[0079] 6 g of 0.350PH-0.158PST-0.492PT ceramic powder was weighed into a mortar, and about 0.6 g of PVA solution was added in multiple times for granulation, and the powder particles were repeatedly ground and sieved (80 mesh) to ensure that the powder particles were uniform in size and fully granulated.

[0080] 0.75 g of the granulated powder was weighed into a die with a diameter of 10 mm to press a green sheet, and the green sheet was placed in a muffle furnace and slowly heated to 550 o C at a heating rate of 1 o C / min, and degassing was performed for 2 h.

[0081] The degassed green sheet was placed in a 30 mL small crucible and was buried in a second ball-milled powder of the same composition, and was placed in a high-temperature furnace and heated to 1200-1300 o C at a heating rate of 3 o C / min, and was held for 2 h to obtain a dense 0.350PH-0.158PST-0.492PT ceramic sheet.

[0082] Then, the sintered and dense 0.350PH-0.158PST-0.492PT ceramic sheet is ground to a thickness of 0.7mm, and electrodes are plated on it. After that, the excess electrodes on the edges are ground off. Finally, it is polarized at room temperature for 60 minutes and aged for 24 hours before electrical performance testing can be performed.

[0083] The 0.350PH-0.158PST-0.492PT piezoelectric ceramic prepared in this embodiment has the following characteristics: a piezoelectric coefficient of 302 pC / N, a unipolar strain of 0.126%, a strain hysteresis of 20.07%, and a Curie temperature of 293°C. o C, with a relative permittivity of 1757 at room temperature and a remanent polarization of 20.19 μC / cm. 2 The coercive field is 0.99 kV / mm.

[0084] Example 9 According to the stoichiometric ratio of 0.350PH-0.148PST-0.502PT, 3.0793g of HfO2 (99.99%), 0.9057g of ScTaO4, 1.6776g of TiO2 (99.89%), and 9.5241g of PbO (99.9%) were weighed and placed into a ball mill jar, and 20mL of anhydrous ethanol was added. The mixture was ball-milled at 280 rpm for 24 hours in a planetary ball mill. The ball-milled slurry was then placed in an 80°C container. o Dry in an oven at temperature C.

[0085] The dried mixed powder is ground, then placed in a corundum crucible and compacted. The crucible is then placed in a muffle furnace at 3... o The heating rate increased to 900 °C / min. o C, after heat preservation for 2 hours, 0.350PH-0.148PST-0.502PT pre-calcined powder was obtained. Then, the pre-calcined powder was crushed and ground, and then placed in a ball mill jar for ball milling for 12 hours. Finally, it was dried in an oven.

[0086] Weigh 6g of 0.350PH-0.148PST-0.502PT ceramic powder and place it in a mortar. Add about 0.6g of PVA solution in several batches for granulation. Grind and sieve (80 mesh) repeatedly to ensure that the powder particles are uniform in size and fully granulated.

[0087] Weigh 0.75g of granulated powder and pour it into a 10mm diameter mold for pressing. Place the pressed green sheet into a muffle furnace at 1... o The heating rate was slowly increased to 550 °C / min. o Keep warm for 2 hours and then remove the glue.

[0088] After the glue is removed, the green sheet is placed in a 30 mL small crucible and buried with the same group of secondary ball-milled powder, placed in a high-temperature furnace at a rate of 3 o C / min to 1200~1300 o C, and heat treated for 2 h to obtain dense 0.350PH-0.148PST-0.502PT ceramic sheets.

[0089] Then the sintered dense 0.350PH-0.148PST-0.502PT ceramic sheet is ground to a thickness of 0.7 mm, coated with an electrode by processing, then the excess electrode on the edge is polished off, and finally the electrical performance test can be carried out after polarization at room temperature for 60 min and aging for 24 h.

[0090] The 0.350PH-0.148PST-0.502PT piezoelectric ceramic prepared in this example has the following characteristics: piezoelectric coefficient of 247 pC / N, unipolar strain of 0.101%, strain hysteresis of 20.29%, Curie temperature of 296 o C, room temperature relative dielectric constant of 1528, remanent polarization of 16.86 μC / cm 2 , and coercive field of 1.12 kV / mm.

[0091] Example 10 According to the stoichiometric ratio of 0.01Sm-0.350PH-0.168PST-0.482PT, 0.0727 g of Sm2O3 (99.9%), 3.0680 g of HfO2 (99.99%), 1.0242 g of ScTaO4, 1.6049 g of TiO2 (99.89%), and 9.4890 g of PbO (99.9%) are weighed into a ball mill jar and 20 mL of anhydrous ethanol is added, and the mixture is ball-milled on a planetary ball mill at a speed of 280 revolutions / min for 24 h, and then the ball-milled slurry is placed in an oven at 80 o C to dry.

[0092] The dried mixed powder is ground, then placed in a corundum crucible and compacted, and the crucible is placed in a muffle furnace at a rate of 3 o C / min to 900 o C, and heat treated for 2 h to obtain 0.01Sm-0.350PH-0.168PST-0.482PT pre-sintered powder, then the pre-sintered powder is crushed and ground and placed in a ball mill jar for ball milling for 12 h, and finally dried in an oven.

[0093] Take 6g of 0.01Sm-0.350PH-0.168PST-0.482PT ceramic powder into a mortar, add about 0.6g of PVA solution in multiple times for granulation, and repeatedly grind and sieve (80 mesh) to ensure that the powder particles are uniform in size and fully granulated.

[0094] Take 0.75g of the granulated powder into a 10mm diameter die for tabletting, and put the green tablet obtained into a muffle furnace at 1 o C / min to 550 o C for 2h for degassing.

[0095] After degassing, the green tablet is placed in a 30mL small crucible and buried with the second ball-milled powder of the same composition, and is placed in a high-temperature furnace at 3 o C / min to 1200~1300 o C for 2h to obtain dense 0.01Sm-0.350PH-0.168PST-0.482PT ceramic tablets.

[0096] Then the sintered dense 0.01Sm-0.350PH-0.168PST-0.482PT ceramic tablets are ground to a thickness of 0.7mm, coated with electrodes by processing, and then the excess electrodes on the edges are polished off. Finally, the electrical performance test can be carried out after polarization for 60min at room temperature and aging for 24h.

[0097] The 0.01Sm-0.350PH-0.168PST-0.482PT piezoelectric ceramic prepared in this example has the following characteristics: piezoelectric coefficient of 614pC / N, unipolar strain of 0.186%, strain hysteresis of 14.78%, Curie temperature of 261 o C, room temperature relative dielectric constant of 2849, remanent polarization of 33.00μC / cm 2 , and coercive field of 0.99kV / mm.

[0098] Example 11 According to the stoichiometric ratio of 0.02Sm-0.350PH-0.168PST-0.482PT, 0.1454g of Sm2O3 (99.9%), 3.0680g of HfO2 (99.99%), 1.0242g of ScTaO4, 1.6049g of TiO2 (99.89%), and 9.4890g of PbO (99.9%) are weighed into a ball mill jar and 20mL of anhydrous ethanol is added, and the mixture is ball-milled on a planetary ball mill at a speed of 280rpm for 24h, and then the ball-milled slurry is dried in an oven at 80 o C.

[0099] The mixed powder after drying is ground, and then is put into a corundum crucible and compacted, the crucible is put into a muffle furnace at a heating rate of 3 o C / min to 900 o C, and then is kept for 2h to obtain 0.02Sm-0.350PH-0.168PST-0.482PT pre-sintered powder. Then the pre-sintered powder is crushed and ground, and is put into a ball mill tank for ball milling for 12h, and finally is dried in an oven.

[0100] 6g of 0.02Sm-0.350PH-0.168PST-0.482PT ceramic powder is weighed into a mortar, and about 0.6g of PVA solution is added for granulation in multiple times. The powder is repeatedly ground and sieved (80 mesh) to ensure that the powder particles are uniform in size and fully granulated.

[0101] 0.75g of the granulated powder is weighed into a die with a diameter of 10mm for tabletting. The green tablet obtained by tabletting is put into a muffle furnace at a heating rate of 1 o C / min to 550 o C for 2h for degassing.

[0102] The green tablet after degassing is put into a 30mL small crucible, and is buried with the second ball-milled powder of the same composition, and is put into a high-temperature furnace at a heating rate of 3 o C / min to 1200~1300 o C for 2h to obtain dense 0.02Sm-0.350PH-0.168PST-0.482PT ceramic tablets.

[0103] Then the dense 0.02Sm-0.350PH-0.168PST-0.482PT ceramic tablets after sintering are ground to a thickness of 0.7mm, are plated with electrodes by processing, and then the excess electrodes on the edges are polished off. Finally, the electrical performance test can be carried out after polarization for 60min at room temperature and aging for 24h.

[0104] The 0.02Sm-0.350PH-0.168PST-0.482PT piezoelectric ceramic prepared in this example has the following characteristics: piezoelectric coefficient of 437pC / N, unipolar strain of 0.136%, strain hysteresis of 16.17%, Curie temperature of 252 o C, relative dielectric constant at room temperature of 2169, remanent polarization of 28.09μC / cm 2 , and coercive field of 1.27kV / mm.

[0105] Example 12 According to the stoichiometric ratio of 0.03Sm-0.350PH-0.168PST-0.482PT, 0.2180g of Sm2O3 (99.9%), 3.0680g of HfO2 (99.99%), 1.0242g of ScTaO4, 1.6049g of TiO2 (99.89%), and 9.4890g of PbO (99.9%) were weighed and placed into a ball mill jar, and 20mL of anhydrous ethanol was added. The mixture was ball-milled at 280 rpm for 24 hours in a planetary ball mill. The ball-milled slurry was then placed in an 80°C container. o Dry in an oven at temperature C.

[0106] The dried mixed powder is ground, then placed in a corundum crucible and compacted. The crucible is then placed in a muffle furnace at 3... o The heating rate increased to 900 °C / min. o After heating at C for 2 hours, 0.03Sm-0.350PH-0.168PST-0.482PT pre-calcined powder was obtained. The pre-calcined powder was then crushed, ground, and placed in a ball mill jar for ball milling for 12 hours. Finally, it was dried in an oven.

[0107] Weigh 6g of 0.03Sm-0.350PH-0.168PST-0.482PT ceramic powder and place it in a mortar. Add about 0.6g of PVA solution in several batches to granulate the powder. Grind and sieve (80 mesh) repeatedly to ensure that the powder particles are uniform in size and fully granulated.

[0108] Weigh 0.75g of granulated powder and pour it into a 10mm diameter mold for pressing. Place the pressed green sheet into a muffle furnace at 1... o The heating rate was slowly increased to 550 °C / min. o Keep warm for 2 hours and then remove the glue.

[0109] After debinding, the green sheet is placed in a 30mL crucible and calcined with a secondary ball-milled powder of the same composition. It is then placed in a high-temperature furnace at 3... o The heating rate was increased to 1200~1300 °C / min. o C, heat treatment for 2 hours to obtain dense ceramic sheets of 0.03Sm-0.350PH-0.168PST-0.482PT.

[0110] Then, the sintered and dense 0.03Sm-0.350PH-0.168PST-0.482PT ceramic sheet is ground to a thickness of 0.7mm, and electrodes are plated on it. After that, the excess electrodes on the edges are ground off. Finally, it is polarized at room temperature for 60 minutes and aged for 24 hours before electrical performance testing can be performed.

[0111] The piezoelectric ceramic prepared in the embodiment has the following characteristics: piezoelectric coefficient of 390 pC / N, unipolar strain of 0.120%, strain hysteresis of 15.99%, Curie temperature of 225 o C, relative dielectric constant at room temperature of 2110, remanent polarization of 27.35 μC / cm 2 , and coercive field of 1.30 kV / mm.

[0112] The application will be described in further detail below with reference to the drawings: The phase structure of the prepared ceramic powder is measured by X-ray diffraction as shown in the figure Figure 1 . According to the analysis of the PH-PST-PT ternary phase diagram, the MPB component is constructed by selecting nine different components, and then different Sm contents are doped on the basis of the optimized component. They are respectively: example 1: 0.300PH-0.224PST-0.476PT (A), example 2: 0.325PH-0.196PST-0.479PT (B), example 3: 0.350PH-0.168PST-0.482PT (C), example 4: 0.375PH-0.140PST-0.485PT (D), example 5: 0.400PH-0.112PST-0.488PT (E), example 6: 0.350PH-0.188PST-0.462PT (C1), example 7: 0.350PH-0.178PST-0.472PT (C2), example 8: 0.350PH-0.158PST-0.492PT (C3), example 9: 0.350PH-0.148PST-0.502PT (C4), example 10: 0.01Sm-0.350PH-0.168PST-0.482PT (0.01Sm-C), example 11: 0.02Sm-0.350PH-0.168PST-0.482PT (0.02Sm-C), and example 12: 0.03Sm-0.350PH-0.168PST-0.482PT (0.03Sm-C). As can be seen from the figure, the piezoelectric ceramic prepared in the examples 1-12 of the application has pure perovskite structure.

[0113] Taking example 10 as an example, the related performance test is carried out, and the results are as follows: From Figure 2 the dielectric temperature spectrum, it can be seen that the Curie temperature of the piezoelectric ceramic prepared in example 10 of the application is 261 o C. From Figure 3 the polarization intensity-electric field curve, it can be seen that the remanent polarization of the piezoelectric ceramic prepared in example 10 of the application is 33.00 μC / cm2 The coercive field is 0.99 kV / mm respectively. Figure 4 It can be seen from the monopolar strain-electric field curve that the monopolar strain value of the piezoelectric ceramic prepared in the embodiment 10 of the present application is 0.186% under the electric field of 2 kV / mm. Figure 5 It can be seen from the monopolar strain-electric field curve under the electric field of 2 kV / mm at different temperatures that the monopolar strain value of the piezoelectric ceramic prepared in the embodiment 10 of the present application fluctuates by ≤4.4% under the electric field of 2 kV / mm at 25-200 o C.

[0114] In summary, the Sm-doped PH-PST-PT ternary piezoelectric ceramic prepared in the present application can effectively solve the key technical problems in the preparation of high-performance piezoelectric devices, i.e., can meet the performance requirements of low hysteresis, wide temperature range, high stability and strain response under low electric field.

[0115] The above content only illustrates the technical idea of the present application, and cannot limit the protection scope of the present application. Any modification made according to the technical idea of the present application on the basis of the technical scheme falls within the protection scope of the claims of the present application.

Claims

1. A piezoelectric ceramic material exhibiting both low hysteresis and wide-temperature-range stable electrostrain under low electric field conditions, characterized in that, This piezoelectric ceramic material is a rare-earth Sm-doped PH-PST-PT ternary piezoelectric ceramic material with the chemical composition xSm-yPbHfO3-zPb(Sc 1 / 2 Ta 1 / 2 )O3-(1-yz)PbTiO3(Sm-PH-PST-PT), where 0≤x≤0.03, 0.25≤y≤0.5, 0.05≤z≤0.

31.

2. The piezoelectric ceramic material with low hysteresis and wide temperature range stability under low electric field as described in claim 1, characterized in that, The piezoelectric ceramic exhibits a piezoelectric coefficient of 155-614 pC / N, a unipolar strain of 0.103%-0.186%, a strain hysteresis of 14.78%-21.83%, and a Curie temperature of 225°C. o C-306 o C, with a room temperature dielectric constant of 928-2849 and a remanent polarization of 16.86-33.00 μC / cm. 2 The coercive field is 0.54-1.30 kV / mm.

3. A method for preparing a piezoelectric ceramic material exhibiting both low hysteresis and wide-temperature-range stability under low electric field, characterized in that, Includes the following steps: 1) According to xSm-yPbHfO3-zPb(Sc 1 / 2 Ta 1 / 2 The stoichiometric ratio of Sm2O3-(1-yz)PbTiO3(Sm-PH-PST-PT) is used to prepare the mixture, where 0≤x≤0.03, 0.25≤y≤0.5, and 0.05≤z≤0.

31. The raw materials Sm2O3, HfO2, ScTaO4, TiO2 and PbO are weighed, ball-milled until uniform, and then dried and ground for later use. 2) The mixture is pre-calcined to obtain pure perovskite phase Sm-PH-PST-PT pre-calcined powder. Then, the Sm-PH-PST-PT pre-calcined powder is ball-milled and dried to obtain pre-calcined powder. 3) The pre-fired powder is granulated, then sieved and pressed into green sheets. After the green sheets are debinded, they are sintered to obtain Sm-PH-PST-PT piezoelectric ceramic material with low hysteresis and wide temperature range stability under low electric field.

4. The method for preparing a piezoelectric ceramic material with low hysteresis and wide temperature range stability under low electric field as described in claim 3, characterized in that, In step 1), the preparation method of the raw material ScTaO4 is as follows: Weigh the raw materials Sc2O3 and Ta2O5 according to the stoichiometric ratio of ScTaO4, ball mill them at 250-280 rpm for 24 hours, then dry them, crush and grind them, and finally grind them at 1300-1400 rpm. o Calcination at C for 2-4 h yields raw material ScTaO4.

5. A method for preparing a piezoelectric ceramic material with low hysteresis and wide temperature range stability under low electric field, as described in claim 3, characterized in that, In step 1), the ball milling speed is 250-280 rpm, the ball milling time is 24 hours, and the drying temperature is 70-90°C. o C.

6. A method for preparing a piezoelectric ceramic material with low hysteresis and wide temperature range stability under low electric field, as described in claim 3, characterized in that, In step 2), the pre-firing temperature is 850°C. - 900 o C. The pre-calcination time is 2-4 hours, the secondary ball milling speed is 250-280 rpm, the secondary ball milling time is 12 hours, and the drying temperature is 70-90°C. o C.

7. The method for preparing a piezoelectric ceramic material with low hysteresis and wide temperature range stability under low electric field as described in claim 3, characterized in that, In step 3), a 5% polyvinyl alcohol aqueous solution is used to granulate the pre-calcined powder. The amount of polyvinyl alcohol aqueous solution added is 5%-10% of the mass of the pre-calcined powder, and the sieve used for sieving has a mesh size of 80-100 mesh.

8. A method for preparing a piezoelectric ceramic material with low hysteresis and wide temperature range stability under low electric field, as described in claim 3, characterized in that, In step 3), the glue removal temperature is 550°C. o C, the glue removal treatment time is 2 hours, and the heating rate is 1. o C / min.

9. A method for preparing a piezoelectric ceramic material with low hysteresis and wide temperature range stability under low electric field, as described in claim 3, characterized in that, The sintering temperature is 1200-1300 °C, the heating rate is 3 °C / min, and the holding time is 2-4 h.

10. The piezoelectric ceramic material with low hysteresis and wide temperature range stability electrostrain under low electric field as described in claim 1 or 2, or the piezoelectric ceramic material with low hysteresis and wide temperature range stability electrostrain obtained by the preparation method described in any one of claims 3-9, is used in the preparation of piezoelectric devices.

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