CN116768626B - PbNb (PbNb) material 2 O 6 Base piezoelectric ceramic material and preparation method thereof - Google Patents
PbNb (PbNb) material 2 O 6 Base piezoelectric ceramic material and preparation method thereof Download PDFInfo
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 58
- 239000000463 material Substances 0.000 title claims abstract description 17
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- 238000000034 method Methods 0.000 claims abstract description 30
- 230000008569 process Effects 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 50
- 239000000843 powder Substances 0.000 claims description 40
- 238000000498 ball milling Methods 0.000 claims description 35
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- 229910006404 SnO 2 Inorganic materials 0.000 claims description 12
- 239000011812 mixed powder Substances 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 12
- 238000007873 sieving Methods 0.000 claims description 12
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- 229910021193 La 2 O 3 Inorganic materials 0.000 claims 1
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Abstract
The invention belongs to the technical field of ceramic materials and electronic devices with electronic information functions, and provides a PbNb (PbNb-based ceramic) material 2 O 6 Base piezoelectric ceramic material and preparation method thereof for solving PbNb 2 O 6 The base piezoelectric ceramics are difficult to sinter. The piezoelectric ceramic material body of the invention is composed of PbNb 2 O 6 The phase composition has the molecular formula: pb 0.97 La 0.02 (Nb 0.936‑x Ti 0.08 Sn 1.25x ) 2 O 6 The value range of x is as follows: x is more than or equal to 0.00 and less than or equal to 0.10; the material is made of Pb 0.97 La 0.02 (Nb 0.936 Ti 0.08 ) 2 O 6 On the basis of (1) through Sn 4+ Ion doping modification to make PbNb 2 O 6 The base piezoelectric ceramic material has the characteristics of good compactness, high Curie temperature, low dielectric loss and the like, and provides an effective solution for the development of high temperature resistance and conversion efficiency improvement of piezoelectric components; at the same time, the PbNb 2 O 6 The preparation method of the base piezoelectric ceramic material has the advantages of simple process, low cost and the like, and industrial production is utilized.
Description
Technical Field
The invention belongs to the technical field of electronic information functional ceramic materials and electronic devices, and particularly provides a PbNb (PbNb-based ceramic) material 2 O 6 The base piezoelectric ceramic material and the preparation method thereof are used in the fields of piezoelectric transducers, piezoelectric stacks and the like.
Background
The piezoelectric ceramic refers to a multifunctional material capable of realizing the mutual conversion of mechanical energy and electric energy, is always a hot spot in the research field of materials at home and abroad, and has application fields in various industries, such as piezoelectric transformers, electroacoustic/ultrasonic/underwater acoustic transducers, standard signal sources, filters, accelerometers, amplifiers, surface waveguides, pressure gauges, angular accelerometers, displacement generators, storage and display, infrared detectors, nonlinear elements and the like. With rapid development of technology, piezoelectric ceramics applied in high temperature environments are particularly attractive, and have been widely used in many fields such as petrochemical industry, computers, nuclear energy and electrical appliances; however, many electronic devices place higher and higher demands on piezoelectric components, and in particular, piezoelectric devices operating in high-temperature environments are being challenged, so that it is still urgent to develop high-temperature piezoelectric devices with good performance.
In order to ensure that the piezoelectric device applied at high temperature works normally, the piezoelectric material must have two conditions; first, the material needs to have a high T when used at high temperature c (curie temperature), and below the curie temperature, the piezoelectric properties of the piezoelectric material are less affected by temperature; secondly, the material has a high d 33 (piezoelectric coefficient) and remain constant over a wide temperature range. In many high temperature piezoceramic systems, pbNb 2 O 6 The matrix-based piezoelectric ceramics are particularly attractive, which have a relatively high curie temperature (T c About 570 ℃ C.), lower mechanical quality factor (Q) m ) These characteristics are important for applications of sensors and detectors at high temperatures; however, pure phase PbNb 2 O 6 The base piezoelectric ceramics are difficult to sinter; accordingly, a PbNb of the invention 2 O 6 The base piezoelectric ceramic material and the preparation method thereof have the characteristics of higher Curie temperature, low dielectric loss and the like, and are beneficial to further enriching the requirements of the products.
Disclosure of Invention
The invention aims at pure phase PbNb 2 O 6 The piezoelectric ceramic is difficult to sinter, and provides a high T which is relatively easy to sinter c PbNb value of 2 O 6 The base piezoelectric ceramic material and the preparation method thereof are used for meeting the requirements of piezoelectric components working at high temperature; the PbNb provided by the invention 2 O 6 The base piezoelectric ceramic material has the characteristics of higher Curie temperature, low dielectric loss and the like, and is piezoelectricThe components and parts provide an effective solution for the development of high temperature resistance and conversion efficiency.
In order to achieve the above purpose, the invention adopts the following technical scheme:
PbNb (PbNb) material 2 O 6 The piezoelectric ceramic material is characterized by mainly comprising PbNb 2 O 6 The phase composition has the molecular formula:
Pb 0.97 La 0.02 (Nb 0.936-x Ti 0.08 Sn 1.25x ) 2 O 6
wherein, the value range of x is: x is more than 0.00 and less than or equal to 0.10.
Further, the dielectric constant of the piezoelectric ceramic material is 226-328, the dielectric loss is 0.011-0.024, d 33 The value is 32-65 pC/N, T c The value is 550-646 ℃.
Further, the preparation method of the piezoelectric ceramic material comprises the following steps:
step 1, batching: by PbO, la 2 O 3 、Nb 2 O 5 、TiO 2 、SnO 2 As raw material according to the molecular formula Pb 0.97 La 0.02 (Nb 0.936-x Ti 0.08 Sn 1.25x ) 2 O 6 Preparing mixed powder A; then taking PbO according to 2wt% of the mixed powder A as powder B; mixing the mixed powder A and the powder B to obtain piezoelectric phase powder; wherein PbO, la 2 O 3 、Nb 2 O 5 、TiO 2 、SnO 2 The purity of (2) is 99.97%, 99.95%, 99.90%, 99.00% and 99.50%, respectively;
step 2, ball milling for the first time: the wet milling method is adopted to carry out ball milling mixing on the piezoelectric phase powder, and the specific process is as follows: pure water is used as a dispersing agent, zirconia balls are used as ball milling media, and raw materials are arranged: pure water: mixing zirconia balls for 12 hours by adopting a wet milling method, discharging, drying at 120 ℃ and sieving to obtain piezoelectric phase powder after ball milling, wherein the weight ratio of the zirconia balls is 1:2:1.5; wherein the diameter of the zirconia balls is 3-15 mm;
step 3, presintering: placing the piezoelectric phase powder into a muffle furnace, heating from room temperature to 900 ℃ at a heating rate of 3 ℃/min, and preserving heat for 4 hours to obtain presintered powder;
step 4, secondary ball milling: ball milling is carried out on presintered powder by adopting a wet milling method, and the specific process is as follows: pure water is used as a dispersing agent, zirconia balls are used as ball milling media, and raw materials are arranged: pure water: mixing zirconia balls for 8 hours by adopting a wet milling method according to the weight ratio of 1:2:1.5, discharging, drying at 120 ℃ and sieving to obtain presintered powder after ball milling; wherein the diameter of the zirconia balls is 3-15 mm;
step 5: granulating: adding 6-10wt% of organic binder into the presintered powder according to the weight ratio, granulating, sieving, and pressing into cylindrical plastic blanks with the diameter of 10-12 mm and the height of 1.1-1.2 mm;
step 6: sintering: and (3) placing the plastic blank into a muffle furnace, and sintering for 4 hours at 1210 ℃ in an air atmosphere to obtain the piezoelectric ceramic material, wherein the temperature rise and fall rate is 3 ℃/min.
Based on the technical scheme, the invention has the beneficial effects that:
the invention provides a PbNb 2 O 6 Base piezoelectric ceramic material, which is made of Pb 0.97 La 0.02 (Nb 0.936 Ti 0.08 ) 2 O 6 Based on (1), sn is introduced 4+ Doping with ions due to Sn 4+ With Nb 5+ The ionic radii are close, helping to form solid solutions; and SnO 2 The melting point is higher, which is helpful for improving the compactness of the sintered sample; finally, the invention obtains the high T easy to sinter c PbNb value of 2 O 6 Base piezoelectric ceramic material, T c The piezoelectric ceramic material can well meet the increasingly severe requirements of the current piezoelectric devices on the use environment, and is suitable for being used as a high-temperature piezoelectric transducer, an acoustic component and an ultrasonic defect detection transducer material.
At the same time, the invention provides the PbNb 2 O 6 The preparation method of the base piezoelectric ceramic material has simple preparation process and low preparation cost, and compared with Pb is introduced in the process of proportioning 0.97 La 0.02 (Nb 0.936-x Ti 0.08 Sn 1.25x ) 2 O 6 Excessive "PbO", ensure PbNb 2 O 6 Base piezoelectric ceramic material: pb 0.97 La 0.02 (Nb 0.936-x Ti 0.08 Sn 1.25x ) 2 O 6 The successful preparation of (3) compensates for the PbO volatilized during the sintering process.
Drawings
FIG. 1 shows PbNb in examples 1 to 6 of the present invention 2 O 6 XRD patterns of the base piezoelectric ceramic materials, wherein x=0.00, 0.02, 0.04, 0.06, 0.08, 0.10 correspond to examples 1 to 6 in order.
FIG. 2 shows PbNb in examples 1 to 6 of the present invention 2 O 6 SEM photographs of the surface of the base piezoelectric ceramic material were obtained, wherein examples 1 to 6 correspond to (a) to (f) in this order.
Detailed Description
In order to make the objects, technical solutions and advantageous effects of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings and examples.
Example 1
The present embodiment provides a PbNb 2 O 6 Base piezoelectric ceramic material made of PbNb 2 O 6 The phase composition has the molecular formula: pb 0.97 La 0.02 (Nb 0.936-x Ti 0.08 Sn 1.25x ) 2 O 6 Wherein x=0.00; the piezoelectric ceramic material is prepared by the following steps:
step 1, batching: by PbO, la 2 O 3 、Nb 2 O 5 、TiO 2 、SnO 2 As raw material according to the molecular formula Pb 0.97 La 0.02 (Nb 0.936-x Ti 0.08 Sn 1.25x ) 2 O 6 Preparing mixed powder A; then taking PbO according to 2wt% of the mixed powder A as powder B; mixing the mixed powder A and the powder B to obtain piezoelectric phase powder; wherein PbO, la 2 O 3 、Nb 2 O 5 、TiO 2 、SnO 2 The purity of (2) is 99.97%, 99.95%, 99.90%, 99.00% and 99.50%, respectively;
step 2, ball milling for the first time: the wet milling method is adopted to carry out ball milling mixing on the piezoelectric phase powder, and the specific process is as follows: pure water is used as a dispersing agent, zirconia balls are used as ball milling media, and raw materials are arranged: pure water: mixing zirconia balls for 12 hours by adopting a wet milling method, discharging, drying at 120 ℃ and sieving with a 60-mesh sieve to obtain piezoelectric phase powder after ball milling; wherein the diameter of the zirconia balls is 3-15 mm;
step 3, presintering: placing the piezoelectric phase powder into a muffle furnace, heating from room temperature to 900 ℃ at a heating rate of 3 ℃/min, and preserving heat for 4 hours to obtain presintered powder;
step 4, secondary ball milling: ball milling is carried out on presintered powder by adopting a wet milling method, and the specific process is as follows: pure water is used as a dispersing agent, zirconia balls are used as ball milling media, and raw materials are arranged: pure water: mixing zirconia balls for 8 hours by adopting a wet milling method, discharging, drying at 120 ℃ and sieving with a 60-mesh sieve to obtain ball-milled presintered powder, wherein the weight ratio of the zirconia balls is 1:2:1.5; wherein the diameter of the zirconia balls is 3-15 mm;
step 5: granulating: adding 6-10wt% of organic binder into the presintered powder according to the weight ratio for granulating, sieving with a 40-mesh sieve, and pressing into cylindrical plastic blanks with the diameter of 10-12 mm and the height of 1.1-1.2 mm;
step 6: sintering: placing the plastic blank into a muffle furnace, and sintering for 4 hours at 1210 ℃ in air atmosphere to obtain a piezoelectric ceramic material, wherein the temperature rise and fall rate is 3 ℃/min; to sinter Pb 0.97 La 0.02 (Nb 0.936-x Ti 0.08 Sn 1.25x ) 2 O 6 And polishing the surface of the ceramic material to prepare a sample to be measured.
Aiming at the sample to be detected, obtaining phase structure information of the material by using a Miniflex X-ray diffractometer, and obtaining the apparent morphology of the material by using a JEOL JSM-6490 SEM; then based on the piezoelectric constant of Berlincourt method test material at 110Hz, dielectric measurement is carried out by an Agilent 4284A precise LCR table at room temperature to 700 ℃ and frequency of 100kHz to obtain T c Values.
Finally, pbNb of the present example 2 O 6 XRD patterns of the base piezoelectric ceramic material are shown in FIG. 1, surface SEM pictures are shown in FIG. 2, and crystal grains can be seen from the figuresThe size is large and the rod-shaped growth is realized; pbNb of the present embodiment 2 O 6 The piezoelectric dielectric property test result of the base piezoelectric ceramic material is as follows: the dielectric constant was 328, the dielectric loss was 0.019, the piezoelectric constant was 58pC/N, the Curie temperature was 634℃and the specific results are shown in Table 1.
Example 2
The present embodiment provides a PbNb 2 O 6 Base piezoelectric ceramic material made of PbNb 2 O 6 The phase composition has the molecular formula: pb 0.97 La 0.02 (Nb 0.936-x Ti 0.08 Sn 1.25x ) 2 O 6 Wherein x=0.02; the piezoelectric ceramic material was prepared and tested in the same manner as in example 1.
Finally, pbNb of the present example 2 O 6 The XRD pattern of the base piezoelectric ceramic material is shown in figure 1, the surface SEM picture is shown in figure 2, and the graph shows that crystal grains are fully grown and tightly stacked, and no obvious air holes are found; pbNb of the present embodiment 2 O 6 The piezoelectric dielectric property test result of the base piezoelectric ceramic material is as follows: the dielectric constant was 259, the dielectric loss was 0.021, the piezoelectric constant was 65pC/N, the Curie temperature was 629℃and the specific results are shown in Table 1.
Example 3
The present embodiment provides a PbNb 2 O 6 Base piezoelectric ceramic material made of PbNb 2 O 6 Phase and SnO 2 The phases are formed together, and the molecular formula is as follows: pb 0.97 La 0.02 (Nb 0.936-x Ti 0.08 Sn 1.25x ) 2 O 6 Wherein x=0.04; the piezoelectric ceramic material was prepared and tested in the same manner as in example 1.
Finally, pbNb of the present example 2 O 6 The XRD pattern of the base piezoelectric ceramic material is shown in figure 1, the surface SEM picture is shown in figure 2, and the crystal grains are fully grown and tightly stacked, and the crystal boundary is clearly visible; pbNb of the present embodiment 2 O 6 The piezoelectric dielectric property test result of the base piezoelectric ceramic material is as follows: dielectric constant 258, dielectric loss 0.024, piezoelectric constant 52pC/N, curie temperature 612 ℃, specific junctionThe results are shown in Table 1.
Example 4
The present embodiment provides a PbNb 2 O 6 Base piezoelectric ceramic material made of PbNb 2 O 6 Phase and SnO 2 The phases are formed together, and the molecular formula is as follows: pb 0.97 La 0.02 (Nb 0.936-x Ti 0.08 Sn 1.25x ) 2 O 6 Wherein x=0.06; the piezoelectric ceramic material was prepared and tested in the same manner as in example 1.
Finally, pbNb of the present example 2 O 6 The XRD pattern of the base piezoelectric ceramic material is shown in figure 1, the surface SEM picture is shown in figure 2, and the graph shows that crystal grains are fully grown and closely stacked, but a small amount of cracks appear; pbNb of the present embodiment 2 O 6 The piezoelectric dielectric property test result of the base piezoelectric ceramic material is as follows: the dielectric constant was 237, the dielectric loss was 0.017, the piezoelectric constant was 42pC/N, the Curie temperature was 646℃and the specific results are shown in Table 1.
Example 5
The present embodiment provides a PbNb 2 O 6 Base piezoelectric ceramic material made of PbNb 2 O 6 Phase and SnO 2 The phases are formed together, and the molecular formula is as follows: pb 0.97 La 0.02 (Nb 0.936-x Ti 0.08 Sn 1.25x ) 2 O 6 Wherein x=0.08; the piezoelectric ceramic material was prepared and tested in the same manner as in example 1.
Finally, pbNb of the present example 2 O 6 The XRD pattern of the base piezoelectric ceramic material is shown in FIG. 1, the surface SEM photograph is shown in FIG. 2, and as can be seen from the figure, the grain boundary is not clearly seen and the occurrence of air holes is started; pbNb of the present embodiment 2 O 6 The piezoelectric dielectric property test result of the base piezoelectric ceramic material is as follows: the dielectric constant was 250, the dielectric loss was 0.014, the piezoelectric constant was 39pC/N, the Curie temperature was 550℃and the specific results are shown in Table 1.
Example 6
The present embodiment provides a PbNb 2 O 6 Base piezoelectric ceramic material made of PbNb 2 O 6 Phase and SnO 2 The phases are formed together, and the molecular formula is as follows: pb 0.97 La 0.02 (Nb 0.936-x Ti 0.08 Sn 1.25x ) 2 O 6 Wherein x=0.10; the piezoelectric ceramic material was prepared and tested in the same manner as in example 1.
Finally, pbNb of the present example 2 O 6 The XRD pattern of the base piezoelectric ceramic material is shown in figure 1, the surface SEM picture is shown in figure 2, and the grain boundary cannot be clearly seen, so that the number of air holes is increased; pbNb of the present embodiment 2 O 6 The piezoelectric dielectric property test result of the base piezoelectric ceramic material is as follows: the dielectric constant was 226, the dielectric loss was 0.011, the piezoelectric constant was 32pC/N, the Curie temperature was 550℃and the specific results are shown in Table 1.
TABLE 1
x=0.00 | x=0.02 | x=0.04 | x=0.06 | x=0.08 | x=0.10 | |
εr(100Hz) | 328 | 259 | 258 | 237 | 250 | 226 |
tanδ(100Hz) | 0.019 | 0.021 | 0.024 | 0.017 | 0.014 | 0.011 |
d33(pC/N) | 58 | 65 | 52 | 42 | 39 | 32 |
Tc(℃) | 634 | 629 | 612 | 646 | 550 | 550 |
Of the 6 examples described above, pb prepared in example 2 0.97 La 0.02 (Nb 0.916 Ti 0.08 Sn 0.025 ) 2 O 6 Ceramic d 33 Maximum value: 65pC/N, a dielectric constant of 259, a dielectric loss of 0.021 and a Curie temperature of 629 ℃; with a maximum d 33 Value and higher T c The comprehensive performance is optimal.
In summary, the present invention provides a high T c Value PbNb 2 O 6 Base pressureElectroceramic material and method for producing same, using Sn 4+ For PbNb 2 O 6 The modification of the base ceramic obtains the high-temperature piezoelectric ceramic material with the characteristics of high Curie temperature, low dielectric loss and the like, and provides an effective solution for piezoelectric sensors, detectors and high-temperature transducer elements at high temperature.
While the invention has been described in terms of specific embodiments, any feature disclosed in this specification may be replaced by alternative features serving the equivalent or similar purpose, unless expressly stated otherwise; all of the features disclosed, or all of the steps in a method or process, except for mutually exclusive features and/or steps, may be combined in any manner.
Claims (4)
1. PbNb (PbNb) material 2 O 6 The piezoelectric ceramic material is characterized by mainly comprising PbNb 2 O 6 The phase composition has the molecular formula:
Pb 0.97 La 0.02 (Nb 0.936-x Ti 0.08 Sn 1.25x ) 2 O 6
wherein x=0.02;
the piezoelectric ceramic materialT c The value is 629 ℃, the dielectric constant is 259, the dielectric loss is 0.021,d 33 a value of 65pC/N;
the piezoelectric ceramic material is prepared by the following steps:
step 1, batching: by PbO, la 2 O 3 、Nb 2 O 5 、TiO 2 、SnO 2 As raw material according to the molecular formula Pb 0.97 La 0.02 (Nb 0.936- x Ti 0.08 Sn 1.25x ) 2 O 6 X=0.02 to obtain mixed powder a; then taking PbO according to 2wt% of the mixed powder A as powder B; mixing the mixed powder A and the powder B to obtain piezoelectric phase powder;
step 2, ball milling for the first time: the wet milling method is adopted to carry out ball milling mixing on the piezoelectric phase powder, and the specific process is as follows: pure water is used as a dispersing agent, zirconia balls are used as ball milling media, and raw materials are arranged: pure water: mixing zirconia balls for 12 hours by adopting a wet milling method, discharging, drying at 120 ℃ and sieving to obtain piezoelectric phase powder after ball milling, wherein the weight ratio of the zirconia balls is 1:2:1.5;
step 3, presintering: placing the piezoelectric phase powder after ball milling into a muffle furnace, heating from room temperature to 900 ℃ at a heating rate of 3 ℃/min, and preserving heat for 4 hours to obtain presintered powder;
step 4, secondary ball milling: ball milling is carried out on presintered powder by adopting a wet milling method, and the specific process is as follows: pure water is used as a dispersing agent, zirconia balls are used as ball milling media, and raw materials are arranged: pure water: mixing zirconia balls for 8 hours by adopting a wet milling method according to the weight ratio of 1:2:1.5, discharging, drying at 120 ℃ and sieving to obtain presintered powder after ball milling;
step 5: granulating: adding 6-10wt% of organic binder into the presintered powder after ball milling for granulating, sieving, and pressing into cylindrical plastic blanks with the diameter of 10-12 mm and the height of 1.1-1.2 mm;
step 6: sintering: and (3) placing the plastic blank into a muffle furnace, and sintering for 4 hours at 1210 ℃ in an air atmosphere to obtain the piezoelectric ceramic material, wherein the temperature rise and fall rate is 3 ℃/min.
2. PbNb as claimed in claim 1 2 O 6 The preparation method of the base piezoelectric ceramic material is characterized by comprising the following steps of:
step 1, batching: by PbO, la 2 O 3 、Nb 2 O 5 、TiO 2 、SnO 2 As raw material according to the molecular formula Pb 0.97 La 0.02 (Nb 0.936- x Ti 0.08 Sn 1.25x ) 2 O 6 X=0.02 to obtain mixed powder a; then taking PbO according to 2wt% of the mixed powder A as powder B; mixing the mixed powder A and the powder B to obtain piezoelectric phase powder;
step 2, ball milling for the first time: the wet milling method is adopted to carry out ball milling mixing on the piezoelectric phase powder, and the specific process is as follows: pure water is used as a dispersing agent, zirconia balls are used as ball milling media, and raw materials are arranged: pure water: mixing zirconia balls for 12 hours by adopting a wet milling method, discharging, drying at 120 ℃ and sieving to obtain piezoelectric phase powder after ball milling, wherein the weight ratio of the zirconia balls is 1:2:1.5;
step 3, presintering: placing the piezoelectric phase powder after ball milling into a muffle furnace, heating from room temperature to 900 ℃ at a heating rate of 3 ℃/min, and preserving heat for 4 hours to obtain presintered powder;
step 4, secondary ball milling: ball milling is carried out on presintered powder by adopting a wet milling method, and the specific process is as follows: pure water is used as a dispersing agent, zirconia balls are used as ball milling media, and raw materials are arranged: pure water: mixing zirconia balls for 8 hours by adopting a wet milling method according to the weight ratio of 1:2:1.5, discharging, drying at 120 ℃ and sieving to obtain presintered powder after ball milling;
step 5: granulating: adding 6-10wt% of organic binder into the presintered powder after ball milling for granulating, sieving, and pressing into cylindrical plastic blanks with the diameter of 10-12 mm and the height of 1.1-1.2 mm;
step 6: sintering: and (3) placing the plastic blank into a muffle furnace, and sintering for 4 hours at 1210 ℃ in an air atmosphere to obtain the piezoelectric ceramic material, wherein the temperature rise and fall rate is 3 ℃/min.
3. PbNb as claimed in claim 2 2 O 6 The preparation method of the base piezoelectric ceramic material is characterized in that in the step 1, pbO and La 2 O 3 、Nb 2 O 5 、TiO 2 、SnO 2 The purity of (3) was 99.97%, 99.95%, 99.90%, 99.00% and 99.50%, respectively.
4. PbNb as claimed in claim 2 2 O 6 The preparation method of the base piezoelectric ceramic material is characterized in that in the step 2 and the step 4, the diameter of the zirconia balls is 3-15 mm.
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CN111170736A (en) * | 2020-02-26 | 2020-05-19 | 中国科学院上海硅酸盐研究所 | Lead-based perovskite structure high-temperature piezoelectric ceramic and preparation method thereof |
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CN101265093A (en) * | 2008-04-30 | 2008-09-17 | 陕西师范大学 | Tungsten bronze structure lead lanthanum niobate titanate high-temperature piezoelectric ceramic and preparation method thereof |
CN111205066A (en) * | 2020-01-15 | 2020-05-29 | 三桥惠(佛山)新材料有限公司 | Preparation method of microwave dielectric ceramic |
CN111170736A (en) * | 2020-02-26 | 2020-05-19 | 中国科学院上海硅酸盐研究所 | Lead-based perovskite structure high-temperature piezoelectric ceramic and preparation method thereof |
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