Preparation method of lead-free piezoelectric ceramic component with low strain hysteresis
By introducing metal particles into lead-free BiFeO3-BaTiO3-based piezoelectric ceramics to construct 0-3 composite ceramics, the problem of high strain hysteresis is solved, the electrogenic strain performance and strain stability are improved, and the device has faster response speed, lower power consumption and heat generation are achieved.
Patent Information
- Application Number
- CN202411631366.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-15
- Publication Date
- 2025-04-22
- Estimated Expiration
- 2044-11-15
AI Technical Summary
The lead-free BiFeO3-BaTiO3-BaTiO3-Basic Piezoelectric Ceramic System has a high strain hysteresis, which leads to heat generated during actual use of the device, slow response speed, low insulation resistance, and difficult to use.
By introducing metal particles to construct 0-3 composite ceramics, specific process steps such as ball milling, prefixing, granulation, sintering and cooling are used to prepare lead-free piezoelectric ceramic components with low strain hysteresis.
It effectively reduces the strain hysteresis of lead-free piezoelectric ceramic components, improves electrostrain performance, reduces the power consumption and heat generation of the device, extends the life of the device, and maintains excellent strain stability over a wide temperature range.
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Figure CN119263810B_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of piezoelectric ceramics, and in particular relates to a method for preparing a lead-free piezoelectric ceramic component with low strain hysteresis. Background Art
[0002] Lead-based piezoelectric ceramics are widely used in military and civilian products due to their excellent electrostrain performance. However, with the widespread concern of society about environmental issues, the environmental protection problems caused by lead are becoming increasingly serious. Therefore, it is necessary to find a lead-free piezoelectric ceramic system to replace lead-based piezoelectric ceramics. BiFeO3-BaTiO3-based piezoelectric ceramics have attracted widespread attention due to their high Curie temperature and excellent electrostrain. However, this ceramic system has a high driving electric field and strain hysteresis. At the same time, due to Bi in the preparation process, 3+ Volatilization and Fe 3+ The valence change of ions leads to low insulation resistance, which makes it difficult to use in actual products. Reducing its strain hysteresis is an important part of its application in actual products. Strain hysteresis mainly causes the device to generate heat during actual use, and the device drive will be slower than the driving electric field.
[0003] In order to solve the problem of large strain hysteresis in the lead-free BiFeO3-BaTiO3-based piezoelectric ceramic system, researchers have shown their abilities. Some researchers have reduced strain hysteresis by adjusting the domain structure and morphology and constructing polar nano-micro-regions. The strain hysteresis has been improved, but the driving electric field is relatively high.
[0004] Some researchers have reduced the high hysteresis caused by the transformation of electric domains or phase structures by constructing macroscopic pseudo-cubic phases and coexisting microscopic multiphases, but the strain value is low under high electric fields; some have reduced the energy barrier of electric domain deflection by constructing defects, but the strain hysteresis remains high. Summary of the invention
[0005] The object of the present invention is to provide a method for preparing a lead-free piezoelectric ceramic component with low strain hysteresis in order to solve the above-mentioned problems.
[0006] The technical solution adopted by the present invention is as follows: a method for preparing a lead-free piezoelectric ceramic component with low strain hysteresis, the preparation method comprising the following steps:
[0007] S1: Prepare raw materials. Weigh BaCO3, TiO2, La2O3, HfO2, Bi2O3, SrCO3, Fe2O3, and Fe3O4 raw materials according to the stoichiometric ratio. The general chemical formula of the materials is:
[0008] 0.97[Bi 1.05 Fe 0.07 +2 Fe 0.93+3 O3-0.3Ba(Hf 0.05 Ti 0.95 )O3)]-0.03(La 0.1 Sr 0.8 )TiO 3-δ -xPt;
[0009] Abbreviated as: xPt / BF-BHT-LST, (0.5≤x≤2vol.%), which is a 0-3 composite piezoelectric ceramic material;
[0010] S2: ball milling and mixing, the raw materials are wet ball milled for 12 hours to ensure that the raw materials are evenly mixed;
[0011] S3: pre-sintering, drying the ball-milled mixture, and then pre-sintering at a temperature of 800-850° C. for 4-6 hours to obtain a pre-sintered ceramic powder;
[0012] S4: Granulation: wet ball milling the pre-fired ceramic powder, drying it, and then adding a binder for granulation, wherein the mass fraction of the binder added is 5% to 10%, and the mass fraction is 7%;
[0013] S5: Sintering: Sintering the granulated mixture at a temperature of 1000-1080° C. for 1-3 hours;
[0014] S6: ball milling treatment, hand grinding the sintered ceramic material for 2 hours to achieve the desired particle size;
[0015] S7: adding metal particles, mixing the ground ceramic powder with Pt metal particles, and using a high-energy ball mill for 15 minutes to evenly disperse the metal particles in the ceramic powder;
[0016] S8: Granulation and sintering again: the mixed powder is dried, PVA is added to granulate, pressed into a disc with a thickness of 1.1 mm and a diameter of 12 mm, and then sintered at 1040-1080°C;
[0017] S9: Cooling: After sintering, cool to 800°C at a rate of 10°C / min, then take out and air-cool, and then package and store the obtained lead-free piezoelectric ceramic with low strain hysteresis, thus completing the preparation process of the entire lead-free piezoelectric ceramic component with low strain hysteresis.
[0018] In a preferred embodiment, in step S2, ZrO2 balls and SiC balls are selected as ball milling media to avoid contamination of ceramic materials; the ball milling time should be controlled at about 12 hours to ensure that the raw materials are mixed evenly to form uniform ceramic powder; the ball milling speed should be adjusted according to the type and diameter of the ball milling media to ensure the ball milling efficiency.
[0019] In a preferred embodiment, in step S3, the pre-firing temperature should be controlled within the range of 800-850°C to ensure that the reaction between the raw materials is fully carried out to form a stable ceramic phase; the pre-firing time should be controlled within 4-6 hours to ensure that the reaction is fully carried out and to avoid excessive sintering; the pre-firing atmosphere should be adjusted according to the properties of the ceramic material, such as pre-firing in air or passing inert gas protection.
[0020] In a preferred embodiment, in step S4, the amount of binder added should be controlled within the range of 5% to 10% to ensure the strength and fluidity of the ceramic particles.
[0021] In a preferred embodiment, in step S5, the sintering temperature should be controlled within the range of 1000-1080°C to ensure the densification and grain growth of the ceramic material; the sintering time should be controlled within 1-3 hours to ensure that the reaction is fully carried out and to avoid over-sintering; the sintering atmosphere should be adjusted according to the properties of the ceramic material, such as sintering in air or passing inert gas protection.
[0022] In a preferred embodiment, in step S6, the ball milling time should be controlled at about 2 hours to ensure that the ceramic powder reaches the required particle size; the ball milling speed should be adjusted according to the type and diameter of the ball milling medium to ensure the ball milling efficiency.
[0023] In a preferred embodiment, in step S7, the amount of metal particles added should be controlled within the range of 0.5% to 2% by volume to ensure that the metal particles are evenly dispersed and play their role; the ball milling time should be controlled within about 15 minutes to ensure that the metal particles are evenly dispersed in the ceramic powder.
[0024] In a preferred embodiment, in step S8, the sintering temperature should be controlled within the range of 1000-1040° C. to ensure the densification and grain growth of the ceramic material; the sintering time should be controlled within 1-3 hours to ensure that the reaction is fully carried out and to avoid over-sintering;
[0025] Sintering atmosphere: The sintering atmosphere should be adjusted according to the properties of the ceramic material, such as sintering in air or passing inert gas protection.
[0026] In a preferred embodiment, in step S9, the cooling rate should be controlled at 10°C / min to ensure uniform cooling of the ceramic material and avoid internal stress. Air cooling or water cooling can be used and adjusted according to the properties of the ceramic material.
[0027] In summary, due to the adoption of the above technical solution, the beneficial effects of the present invention are:
[0028] 1. In the present invention, by introducing metal particles to construct 0-3 composite ceramics, the strain hysteresis of the lead-free piezoelectric ceramic components is effectively reduced, and the electro-strain performance is improved. The reduction of strain hysteresis means that the device responds faster under the same electric field, thereby reducing the power consumption and heat generation of the device and extending the life of the device. The improvement of electro-strain means that the device has a larger deformation under the same electric field, and can be applied to occasions requiring larger displacement, such as micro-displacement motors, fuel injection valve controllers, inkjet printing, etc. The reduction of residual strain means that the device can return to its initial state faster after the electric field disappears, which improves the stability of the device.
[0029] 2. In the present invention, the component has excellent strain stability in a wide temperature range and can be used in occasions with large temperature changes, such as high-temperature micro-displacement occasions, such as fire-fighting robots, inkjet printing, and Mars surface exploration robots. The lead-free formula meets environmental protection requirements and is conducive to reducing environmental pollution. The preparation process of 0-3 composite ceramics is simple, low-cost, and easy to mass produce. The low strain hysteresis lead-free piezoelectric ceramic component prepared by this preparation method has excellent performance and has broad application prospects in many application fields, and is expected to promote the further development of lead-free piezoelectric ceramic materials. BRIEF DESCRIPTION OF THE DRAWINGS
[0030] Figure 1 It is a schematic diagram of the electrostrain loop of the piezoelectric ceramic of the present invention;
[0031] Figure 2 (ab) is the XRD pattern of the xPt / BF-BHT-LST component in the present invention;
[0032] Figure 2 (cf) is the SEM morphology of the x Pt / BF-BHT-LST component in the present invention;
[0033] Figure 2 (gh) is the XRD pattern of the EDS morphology 1 vol% Pt / BF-BHT-LST component in the present invention;
[0034] Figure 3 (a) is the electrostrain loop of the xPt / BF-BHT-LST component of the present invention;
[0035] Figure 3 (b) is the strain hysteresis of the x Pt / BF-BHT-LST component under different electric fields in the present invention;
[0036] Figure 3 (c) is the residual strain of the xPt / BF-BHT-LST component under different electric fields in the present invention;
[0037] Figure 3(d) is the strain loop of 1 vol% Pt / BF-BHT-LST component at 25-175°C in the present invention;
[0038] Figure 4 It is a schematic diagram of the excellent electrostrain performance of the 0-3 composite ceramic in the present invention. DETAILED DESCRIPTION
[0039] In order to make the purpose, technical solution and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.
[0040] Reference Figure 1-4 ,
[0041] Embodiment 1:
[0042] A method for preparing a lead-free piezoelectric ceramic component with low strain hysteresis, the preparation method comprising the following steps:
[0043] S1: Prepare raw materials. Weigh BaCO3, TiO2, La2O3, HfO2, Bi2O3, SrCO3, Fe2O3, and Fe3O4 raw materials according to the stoichiometric ratio. The general chemical formula of the materials is:
[0044] 0.97[Bi 1.05 Fe 0.07 +2 Fe 0.93 +3 O3-0.3Ba(Hf 0.05 Ti 0.95 )O3)]-0.03(La 0.1 Sr 0.8 )TiO 3-δ -xPt, abbreviated as: xPt / BF-BHT-LST, (0.5≤x≤2vol.%), is a 0-3 composite piezoelectric ceramic material;
[0045] S2: ball milling and mixing, the raw materials are wet ball milled for 12 hours to ensure that the raw materials are evenly mixed;
[0046] S3: pre-sintering, drying the ball-milled mixture, and then pre-sintering at a temperature of 800-850° C. for 4-6 hours to obtain a pre-sintered ceramic powder;
[0047] S4: Granulation: wet ball milling the pre-fired ceramic powder, drying it, and then adding a binder (PVA or paraffin wax) for granulation, wherein the binder is added at a mass fraction of 5% to 10%, preferably PVA, with a mass fraction of 7%;
[0048] S5: Sintering: Sintering the granulated mixture at a temperature of 1000-1080° C. for 1 hour;
[0049] S6: ball milling treatment, hand grinding the sintered ceramic material for 2 hours to achieve the desired particle size;
[0050] S7: adding metal particles, mixing the ground ceramic powder with Pt metal particles, and using a high-energy ball mill for 15 minutes to evenly disperse the metal particles in the ceramic powder;
[0051] S8: Granulation and sintering again: the mixed powder is dried, PVA is added to granulate, pressed into a disc with a thickness of 1.1 mm and a diameter of 12 mm, and then sintered at 1040-1080°C;
[0052] S9: Cooling: After sintering, cool to 800°C at a rate of 10°C / min, then take out and air-cool, and then package and store the obtained lead-free piezoelectric ceramic with low strain hysteresis, thus completing the preparation process of the entire lead-free piezoelectric ceramic component with low strain hysteresis.
[0053] In step S1, the purity of the raw material should reach above 99.9% to ensure the performance of the ceramic material. The particle size of the raw material should be controlled at 5 μm-10 μm to facilitate ball milling and subsequent processes.
[0054] In step S2, ZrO2 balls and SiC balls are selected as ball milling media to avoid contamination of ceramic materials. The ball milling time should be controlled to about 12 hours to ensure that the raw materials are evenly mixed to form uniform ceramic powder. The ball milling speed should be adjusted according to the type and diameter of the ball milling media to ensure ball milling efficiency.
[0055] In step S3, the pre-firing temperature should be controlled within the range of 800-850°C to ensure that the reaction between the raw materials is fully carried out to form a stable ceramic phase. The pre-firing time should be controlled within 4-6 hours to ensure that the reaction is fully carried out and to avoid over-sintering. The pre-firing atmosphere should be adjusted according to the properties of the ceramic material, such as pre-firing in air or passing inert gas protection.
[0056] In step S4, the amount of binder added should be controlled within the range of 5% to 10% to ensure the strength and fluidity of the ceramic particles.
[0057] In step S5, the sintering temperature should be controlled within the range of 1000-1080°C to ensure the densification and grain growth of the ceramic material. The sintering time should be controlled within 1-3 hours to ensure that the reaction is fully carried out and to avoid over-sintering. The sintering atmosphere should be adjusted according to the properties of the ceramic material, such as sintering in air or passing inert gas protection.
[0058] In step S6, the ball milling time should be controlled to about 2 hours to ensure that the ceramic powder reaches the required particle size. The ball milling speed should be adjusted according to the type and diameter of the ball milling medium to ensure the ball milling efficiency.
[0059] In step S7, the amount of metal particles added should be controlled within the range of 0.5% to 2% (volume fraction) to ensure that the metal particles are evenly dispersed and play their role. The ball milling time should be controlled within about 15 minutes to ensure that the metal particles are evenly dispersed in the ceramic powder.
[0060] In step S8, the sintering temperature should be controlled within the range of 1000-1040°C to ensure the densification and grain growth of the ceramic material. The sintering time should be controlled within 1-3 hours to ensure that the reaction proceeds fully and to avoid over-sintering.
[0061] Sintering atmosphere: The sintering atmosphere should be adjusted according to the properties of the ceramic material, such as sintering in air or passing inert gas protection.
[0062] In step S9, the cooling rate should be controlled at 10°C / min to ensure uniform cooling of the ceramic material and avoid internal stress. Air cooling or water cooling can be used, and the cooling rate can be adjusted according to the properties of the ceramic material.
[0063] In the present invention, by introducing metal particles to construct 0-3 composite ceramics, the strain hysteresis of the lead-free piezoelectric ceramic components is effectively reduced, and the electro-strain performance is improved. The reduction of strain hysteresis means that the device responds faster under the same electric field, and the driving electric field can be reduced, thereby reducing the power consumption and heat generation of the device and extending the life of the device. The improvement of electro-strain means that the deformation of the device under the same electric field is greater, and it can be applied to occasions requiring greater displacement or force, such as micro-displacement drives, ultrasonic transducers, etc. The reduction of residual strain means that the device can return to its initial state faster after the electric field disappears, which improves the response speed and stability of the device.
[0064] In the present invention, the component has excellent strain stability in a wide temperature range and can be used in occasions with large temperature changes, such as high-temperature sensors. The lead-free formula meets environmental protection requirements and is conducive to reducing environmental pollution. The preparation process of 0-3 composite ceramics is simple, low-cost, and easy to mass produce. The low strain hysteresis lead-free piezoelectric ceramic component prepared by this preparation method has excellent performance and has broad application prospects in many application fields, and is expected to promote the further development of lead-free piezoelectric ceramic materials.
[0065] Embodiment 2:
[0066] A method for preparing a lead-free piezoelectric ceramic component with low strain hysteresis, the preparation method comprising the following steps:
[0067] S1: Prepare raw materials. Weigh BaCO3, TiO2, La2O3, HfO2, Bi2O3, SrCO3, Fe2O3, and Fe3O4 raw materials according to the stoichiometric ratio. The general chemical formula of the materials is:
[0068] 0.97[Bi 1.05 Fe 0.07 +2 Fe 0.93 +3 O3-0.3Ba(Hf 0.05 Ti 0.95 )O3)]-0.03(La 0.1 Sr 0.8 )TiO 3-δ -xPt, abbreviated as: xPt / BF-BHT-LST, (0.5≤x≤2vol.%), is a 0-3 composite piezoelectric ceramic material;
[0069] S2: ball milling and mixing, the raw materials are wet ball milled for 12 hours to ensure that the raw materials are evenly mixed;
[0070] S3: pre-sintering, drying the ball-milled mixture, and then pre-sintering at a temperature of 800-850° C. for 4-6 hours to obtain a pre-sintered ceramic powder;
[0071] S4: Granulation: wet ball milling the pre-fired ceramic powder, drying it, and then adding a binder (PVA or paraffin wax) for granulation, wherein the binder is added at a mass fraction of 5% to 10%, preferably PVA, with a mass fraction of 7%;
[0072] S5: Sintering: Sintering the granulated mixture at a temperature of 1000-1080° C. for 3 hours;
[0073] S6: ball milling treatment, hand grinding the sintered ceramic material for 2 hours to achieve the desired particle size;
[0074] S7: adding metal particles, mixing the ground ceramic powder with Pt metal particles, and using a high-energy ball mill for 15 minutes to evenly disperse the metal particles in the ceramic powder;
[0075] S8: Granulation and sintering again: the mixed powder is dried, PVA is added to granulate, pressed into a disc with a thickness of 1.1 mm and a diameter of 12 mm, and then sintered at 1040-1080°C;
[0076] S9: Cooling: After sintering, cool to 800°C at a rate of 10°C / min, then take out and air-cool, and then package and store the obtained lead-free piezoelectric ceramic with low strain hysteresis, thus completing the preparation process of the entire lead-free piezoelectric ceramic component with low strain hysteresis.
[0077] In step S1, the purity of the raw material should reach above 99.9% to ensure the performance of the ceramic material. The particle size of the raw material should be controlled at 5 μm-10 μm to facilitate ball milling and subsequent processes.
[0078] In step S2, ZrO2 balls and SiC balls are selected as ball milling media to avoid contamination of ceramic materials. The ball milling time should be controlled to about 12 hours to ensure that the raw materials are evenly mixed to form uniform ceramic powder. The ball milling speed should be adjusted according to the type and diameter of the ball milling media to ensure ball milling efficiency.
[0079] In step S3, the pre-firing temperature should be controlled within the range of 800-850°C to ensure that the reaction between the raw materials is fully carried out to form a stable ceramic phase. The pre-firing time should be controlled within 4-6 hours to ensure that the reaction is fully carried out and to avoid over-sintering. The pre-firing atmosphere should be adjusted according to the properties of the ceramic material, such as pre-firing in air or passing inert gas protection.
[0080] In step S4, the amount of binder added should be controlled within the range of 5% to 10% to ensure the strength and fluidity of the ceramic particles.
[0081] In step S5, the sintering temperature should be controlled within the range of 1000-1080°C to ensure the densification and grain growth of the ceramic material. The sintering time should be controlled within 1-3 hours to ensure that the reaction is fully carried out and to avoid over-sintering. The sintering atmosphere should be adjusted according to the properties of the ceramic material, such as sintering in air or passing inert gas protection.
[0082] In step S6, the ball milling time should be controlled to about 2 hours to ensure that the ceramic powder reaches the required particle size. The ball milling speed should be adjusted according to the type and diameter of the ball milling medium to ensure the ball milling efficiency.
[0083] In step S7, the amount of metal particles added should be controlled within the range of 0.5% to 2% (volume fraction) to ensure that the metal particles are evenly dispersed and play their role. The ball milling time should be controlled within about 15 minutes to ensure that the metal particles are evenly dispersed in the ceramic powder.
[0084] In step S8, the sintering temperature should be controlled within the range of 1000-1040°C to ensure the densification and grain growth of the ceramic material. The sintering time should be controlled within 1-3 hours to ensure that the reaction proceeds fully and to avoid over-sintering.
[0085] Sintering atmosphere: The sintering atmosphere should be adjusted according to the properties of the ceramic material, such as sintering in air or passing inert gas protection.
[0086] In step S9, the cooling rate should be controlled at 10°C / min to ensure uniform cooling of the ceramic material and avoid internal stress. Air cooling or water cooling can be used, and the cooling rate can be adjusted according to the properties of the ceramic material.
[0087] In the present invention, by introducing metal particles to construct 0-3 composite ceramics, the strain hysteresis of the lead-free piezoelectric ceramic components is effectively reduced, and the electro-strain performance is improved. The reduction of strain hysteresis means that the device responds faster under the same electric field, and the driving electric field can be reduced, thereby reducing the power consumption and heat generation of the device and extending the life of the device. The improvement of electro-strain means that the deformation of the device under the same electric field is greater, and it can be applied to occasions requiring greater displacement or force, such as micro-displacement drives, ultrasonic transducers, etc. The reduction of residual strain means that the device can return to its initial state faster after the electric field disappears, which improves the response speed and stability of the device.
[0088] In the present invention, the component has excellent strain stability in a wide temperature range and can be used in occasions with large temperature changes, such as high-temperature sensors. The lead-free formula meets environmental protection requirements and is conducive to reducing environmental pollution. The preparation process of 0-3 composite ceramics is simple, low-cost, and easy to mass produce. The low strain hysteresis lead-free piezoelectric ceramic component prepared by this preparation method has excellent performance and has broad application prospects in many application fields, and is expected to promote the further development of lead-free piezoelectric ceramic materials.
[0089] It should be noted that, in this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device. In the absence of further restrictions, the elements defined by the sentence "comprise a ..." do not exclude the existence of other identical elements in the process, method, article or device including the elements.
[0090] The above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit the same. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that the technical solutions described in the aforementioned embodiments may still be modified, or some of the technical features may be replaced by equivalents. However, these modifications or replacements do not deviate the essence of the corresponding technical solutions from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims
1. A method for preparing a lead-free piezoelectric ceramic component with low strain hysteresis, characterized in that: The preparation method comprises the following steps: S1: Prepare the raw materials. Weigh BaCO3, TiO2, La2O3, HfO2, Bi2O3, SrCO3, Fe2O3, and Fe3O4 according to the stoichiometric ratio. The general chemical formula of the materials is: 0.97[Bi 1.05 Fe 0.07 +2 Fe 0.93 +3 O3-0.3Ba(Hf 0.05 Ti 0.95 )O3)]-0.03(La 0.1 Sr 0.8 )TiO 3-δ - x Pt, (0.5≤ x ≤2 vol.%), 0-3 composite piezoelectric ceramic material; S2: ball milling and mixing, the raw materials are wet ball milled for 12 hours to ensure that the raw materials are evenly mixed; S3: pre-sintering, drying the ball-milled mixture, and then pre-sintering at a temperature of 800-850° C. for 4-6 hours to obtain a pre-sintered ceramic powder; S4: Granulation: wet ball milling the pre-fired ceramic powder, drying it, adding a binder to granulate it, and the mass fraction of the binder added is 5% to 10%; S5: Sintering: Sintering the granulated mixture at a temperature of 1000-1080° C. for 1-3 hours; S6: ball milling treatment, hand grinding the sintered ceramic material for 2 hours to achieve the desired particle size; S7: adding metal particles, mixing the ground ceramic powder with Pt metal particles, and using a high-energy ball mill for 15 minutes to evenly disperse the metal particles in the ceramic powder; S8: Granulation and sintering again: the mixed powder is dried, PVA is added to granulate, pressed into a disc with a thickness of 1.1 mm and a diameter of 12 mm, and then sintered at 1040-1080°C; S9: Cooling: After sintering, cool to 800°C at a rate of 10°C / min, then take out and air-cool, and then package and store the obtained lead-free piezoelectric ceramic with low strain hysteresis, thus completing the preparation process of the entire lead-free piezoelectric ceramic component with low strain hysteresis.
2. The method for preparing a lead-free piezoelectric ceramic component with low strain hysteresis according to claim 1, characterized in that: In the step S1, the purity of the raw material should reach above 99.9% to ensure the performance of the ceramic material; the particle size of the raw material should be controlled at 5 μm-10 μm to facilitate ball milling mixing and subsequent processes.
3. The method for preparing the lead-free piezoelectric ceramic component with low strain hysteresis according to claim 1, characterized in that: In step S2, ZrO2 balls and SiC balls are selected as ball milling media to avoid contamination of ceramic materials; the ball milling time is controlled within 12 hours to ensure that the raw materials are mixed evenly to form uniform ceramic powder; the ball milling speed should be adjusted according to the type and diameter of the ball milling media to ensure the ball milling efficiency.
4. The method for preparing a lead-free piezoelectric ceramic component with low strain hysteresis according to claim 1, characterized in that: In step S3, the pre-firing temperature should be controlled within the range of 800-850°C to ensure that the reaction between the raw materials is fully carried out to form a stable ceramic phase; the pre-firing time should be controlled within 4-6 hours to ensure that the reaction is fully carried out and to avoid over-sintering; the pre-firing atmosphere should be adjusted according to the properties of the ceramic material.
5. The method for preparing a lead-free piezoelectric ceramic component with low strain hysteresis according to claim 1, characterized in that: In step S5, the sintering temperature should be controlled within the range of 1000-1080°C to ensure the densification and grain growth of the ceramic material; the sintering time should be controlled within 1-3 hours to ensure sufficient reaction and avoid over-sintering; and the sintering atmosphere should be adjusted according to the properties of the ceramic material.
6. The method for preparing a lead-free piezoelectric ceramic component with low strain hysteresis according to claim 1, characterized in that: In step S6, the ball milling time is controlled within 2 hours to ensure that the ceramic powder reaches the required particle size; the ball milling speed should be adjusted according to the type and diameter of the ball milling medium to ensure the ball milling efficiency.
7. The method for preparing a lead-free piezoelectric ceramic component with low strain hysteresis according to claim 1, characterized in that: In the step S8, the sintering temperature should be controlled at 1040°C to ensure the densification and grain growth of the ceramic material; the sintering time should be controlled at 1-3 hours to ensure that the reaction is fully carried out and to avoid over-sintering; Sintering atmosphere: The sintering atmosphere should be adjusted according to the properties of the ceramic material.
Citation Information
Patent Citations
Multi-layer piezoelectric device and manufacture thereof
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NEW PROCESSING METHOD FOR GRAIN-ORIENTED LEAD-FREE PIEZOELECTRIC Na0.5Bi0.5TiO3-BaTiO3 CERAMICS EXHIBITING GIANT PERFORMANCE
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