WO2010137765A1 - Piezoelectric material and method of manufacturing the same - Google Patents

Piezoelectric material and method of manufacturing the same Download PDF

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Publication number
WO2010137765A1
WO2010137765A1 PCT/KR2009/003662 KR2009003662W WO2010137765A1 WO 2010137765 A1 WO2010137765 A1 WO 2010137765A1 KR 2009003662 W KR2009003662 W KR 2009003662W WO 2010137765 A1 WO2010137765 A1 WO 2010137765A1
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WO
WIPO (PCT)
Prior art keywords
piezoelectric material
synthesizing
agnbo
nanbo
manufacturing
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PCT/KR2009/003662
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English (en)
French (fr)
Inventor
Jeong Ho Cho
Byoung Ik Kim
Yong Hyun Lee
Kyu Serk Han
Joong Hee Nam
Myoung Pyo Chun
Yoo Jung Choi
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Korea Institute Of Ceramic Engineering And Technology
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Publication of WO2010137765A1 publication Critical patent/WO2010137765A1/en

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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N30/00—Piezoelectric or electrostrictive devices
    • H10N30/80—Constructional details
    • H10N30/85—Piezoelectric or electrostrictive active materials
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/495—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N30/00—Piezoelectric or electrostrictive devices
    • H10N30/01—Manufacture or treatment
    • H10N30/09—Forming piezoelectric or electrostrictive materials
    • H10N30/093—Forming inorganic materials
    • H10N30/097—Forming inorganic materials by sintering
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N30/00—Piezoelectric or electrostrictive devices
    • H10N30/80—Constructional details
    • H10N30/85—Piezoelectric or electrostrictive active materials
    • H10N30/853—Ceramic compositions
    • H10N30/8542—Alkali metal based oxides, e.g. lithium, sodium or potassium niobates

Definitions

  • the present disclosure relates to a piezoelectric material and a method of manufacturing the piezoelectric material, and more particularly, to a lead-free piezoelectric material based on AgNbO 3 -KNbO 3 -NaNbO 3 and a method of manufacturing the lead-free piezoelectric material.
  • a piezoelectric material is a material capable of transforming mechanical energy applied thereto to electric energy, and vice versa.
  • the piezoelectric effect is expressed by electromechanical coupling coefficient, K p , which is defined as the ratio of mechanical energy generated in response to electric energy applied.
  • K p electromechanical coupling coefficient
  • a piezoelectric material of an excellent electromechanical coupling coefficient allows linear transformation between electric energy and mechanical energy. Accordingly, a mechanical transformation levelcan be controlled precisely, and an external vibration signal can be transformed precisely to a linear electric signal.
  • Such a piezoelectric material is used as a material for ultrasonic vibrators, electromechanical ultrasonic transducers, actuators, and the like, which are widely used in the fields of ultrasonic apparatuses, display devices, audio devices, communication devices, sensors, etc.
  • PZT Pb(Zr, Ti)O 3
  • the PZT powder is prepared through solid state synthesis which is performed by mixing principal compositions including PbO, ZrO 2 and TiO 2 , and impurities, such as MgO, Nb 2 O 5 , and the like, and sintering the mixture at high temperature.
  • PbO Pb(Zr, Ti)O 3
  • impurities such as MgO, Nb 2 O 5 , and the like
  • the present disclosure provides a piezoelectric material that can replace PZT, and a method of manufacturing the piezoelectric material.
  • the present disclosure also provides a piezoelectric material that forms xAgNbO 3 -yKNbO 3 -zNaNbO 3 having a single phase perovskite crystal structure so that it can be sintered in air, and a method of manufacturing the piezoelectric material.
  • a method of manufacturing a piezoelectric material including: preparing a raw material producing intermediate materials including AgNbO 3 , KNbO 3 , and NaNbO 3 from the raw material; and synthesizing the intermediate materials to produce a piezoelectric material powder.
  • the synthesizing of the intermediate materials may includesynthesizing two of the intermediate materials, and synthesizing the resultant material with the remaining intermediate material. That is, the synthesizing of the intermediate materials may include synthesizing AgNbO 3 and NaNbO 3 to produce AgNbO 3 -NaNbO 3 , and synthesizing AgNbO 3 -NaNbO 3 with KNbO 3 .
  • the synthesizing of the intermediate materials may be performed in air.
  • the method may further include adding an oxide additive to the piezoelectric material powder, after the synthesizing of the intermediate materials.
  • the oxide additive may be one or more selected from Li 2 O, Fe 2 O 3 , Bi 2 O 3 , V 2 O 5 , MnO 2 , ZnO, Sb 2 O 3 , Sb 2 O 5 , and Ta 2 O 5 .
  • the method may further include sintering the piezoelectric material powder in air.
  • a piezoelectric material having a composition of xAgNbO 3 -yKNbO 3 -zNaNbO 3 (where, 0 ⁇ x ⁇ 1.0, 0 ⁇ y ⁇ 1.0, and 0 ⁇ z ⁇ 1.0), and manufactured by the method in accordance with the exemplary embodiment.
  • the piezoelectric material may have a single phase perovskite crystal structure.
  • a piezoelectric material powder of xAgNbO 3 -yKNbO 3 -zNaNbO 3 is manufactured by preparing raw materials, producing intermediate materials (AgNbO 3 , KNbO 3 , and NaNbO 3 ), respectively, and then synthesizing the intermediate materials in sequence.
  • xAgNbO 3 -yKNbO 3 -zNaNbO 3 having a single phase perovskite crystal structure can be manufactured. Accordingly, sintering can be performed in air, and thus the manufacturing cost can be reduced and the productivitycan be improved in comparison to the typical method performed in an oxygen atmosphere.
  • oxide additives can be added during the production of the piezoelectric material powder, and thus the piezoelectric properties can be improved.
  • FIG. 1 is a flow diagram illustrating a method of manufacturing a piezoelectric material in accordance with an exemplary embodiment.
  • FIG. 2 is a flow diagram illustrating a method of manufacturing a piezoelectric material in accordance with another exemplary embodiment.
  • FIG. 3 is a diagram illustrating an X-ray diffraction pattern of a piezoelectric material powder manufactured through typical solid state synthesis.
  • FIG. 4 is a diagram illustrating an X-ray diffraction pattern of a piezoelectric material powder having a composition of 0.2AgNbO 3 -0.4KNbO 3 -0.4NaNbO 3 in accordance with still another exemplary embodiment.
  • FIG. 5 is a diagram illustrating an X-ray diffraction pattern of a piezoelectric materialpowder having a composition of 0.2AgNbO 3 -0.8[xKNbO 3 -(1-x)NaNbO 3 ] in accordance with yet another exemplary embodiment.
  • FIG. 6 is a diagram illustrating an X-ray diffraction pattern of a piezoelectric material powder containing an oxide additive in accordance with even another exemplary embodiment.
  • FIG. 1 is a flow diagram illustrating a method of manufacturing a piezoelectric material in accordance with an exemplary embodiment.
  • a raw material is prepared for producing a compound having a perovskite crystal structure (S100). That is, Ag, Nb and O for AgNbO 3 are weighed and prepared according to their mole fractions, K, Nb and O for KNbO 3 are weighed and prepared according to their mole fractions, and Na, Nb and O for NaNbO 3 are weighed and prepared according to their mole fractions.
  • the prepared raw materials are mixed and calcined to produce intermediate materials including AgNbO 3 , KNbO 3 , and NaNbO 3 , respectively (S200). That is, to produce AgNbO 3 , a mixture of Ag, Nb and O is prepared by weighing and mixing Ag, Nb and O according to their mole fractions, and the mixture is added with a dispersion solvent, pulverized through a first ball mill, and subjected to calcination, for example, at approximately 850°C for approximately 5 hours.
  • KNbO 3 a mixture of K, Nb and O is prepared by weighing and mixing K, Nb and O according to their mole fractions, and the mixture is added with a dispersion solvent, pulverized through a first ball mill, and subjected to calcination, for example, at approximately 850°C for approximately 5 hours.
  • a mixture of Na, Nb and O is prepared by weighing and mixing Na, Nb and O according to their mole fractions, and the mixture is added with a dispersion solvent, pulverized through a first ball mill, and subjected to calcination, for example, at approximately 850°C for approximately 5 hours.
  • the produced intermediate materials are synthesized (S300).
  • any two intermediate materials selected from AgNbO 3 , KNbO 3 , and NaNbO 3 are synthesized first, and the resultant material is then synthesized with the remaining intermediate material.
  • AgNbO 3 and NaNbO 3 are synthesized to produce AgNbO 3 -NaNbO 3
  • AgNbO 3 -NaNbO 3 is synthesized with KNbO 3 to produce AgNbO 3 -NaNbO 3 -KNbO 3 .
  • AgNbO 3 and NaNbO 3 are mixed according to the desired mole fractions, and the mixture is calcined in air at a temperature ranging from approximately 800°C to approximately 1,100°C to produce AgNbO 3 -NaNbO 3 .
  • the synthesized AgNbO 3 -NaNbO 3 is very stable in air even at a high temperature.
  • the synthesized AgNbO 3 -NaNbO 3 is added with a desired mole fraction of KNbO 3 , and the mixture is calcined in air, for example, at a temperature ranging from approximately 800°C to approximately 1,100°C to produce a piezoelectric material powder of xAgNbO 3 -yKNbO 3 -zNaNbO 3 (where, 0 ⁇ x ⁇ 1.0, 0 ⁇ y ⁇ 1.0, and 0 ⁇ z ⁇ 1.0).
  • the piezoelectric materialpowder is added with a small amount of organic material, such as polyvinyl alcohol (PVA) and polyvinyl butyral (PVB), and then a final material is manufactured (S400).
  • organic material such as polyvinyl alcohol (PVA) and polyvinyl butyral (PVB)
  • the piezoelectric material powder is formed into an approximately 1 cm diameter disk-shape under a pressure of approximately 1 ton/cm2, to produce a specimen (S500).
  • Adsorbed water and adhesive water areremoved from the specimen, for example, at approximately 250°C by heating the specimen at a heating rate of approximately 1 °C/min, and combined water and binders are burned away, for example, at approximately 600°C for approximately 2 hours, respectively. Then, the specimen is heat-treated in airat approximately 900°C to approximately 1,100°C for approximately 2 hours, to produce a sintered specimen (S600).
  • the sintered specimen is subjected to polishing and washing. After screen-printing a silver paste on both side of the sintered specimen, the sintered specimen is baked at approximately 700°C for approximately 10 minutes to form a silver electrode, and applied with a voltage of approximately 3 kV/mm to approximately 5 kV/mm for approximately 30 minutes in silicon oil for polarization treatment (S700).
  • a piezoelectric material powder of xAgNbO 3 -yKNbO 3 -zNaNbO 3 is manufactured by synthesizing raw materials to produce intermediate materials including AgNbO 3 , KNbO 3 , and NaNbO 3 , respectively, and then synthesizing the intermediate materials in sequence.
  • oxide additives may be added thereto.
  • a method of manufacturing a piezoelectric material added with oxide additives will be described below with reference to FIG. 2. Descriptions of FIG. 2 similar to that of FIG. 1 will be made briefly.
  • FIG. 2 is a flow diagram illustrating a method of manufacturing a piezoelectric material in accordance with another exemplary embodiment.
  • a raw material is prepared for producing a compound having a perovskite crystal structure (S100).
  • the prepared raw materials are mixed and calcined to produce intermediate materials including AgNbO 3 , KNbO 3 , and NaNbO 3 , respectively (S200).
  • the produced intermediate materials are synthesized to produce a primary powder (S300).
  • a primary powder S300
  • any two intermediate materials selected from AgNbO 3 , KNbO 3 , and NaNbO 3 are synthesized first, and the resultant material is then synthesized with the remaining intermediate material to produce a primary powder of xAgNbO 3 -yKNbO 3 -zNaNbO 3 (where, 0 ⁇ x ⁇ 1.0, 0 ⁇ y ⁇ 1.0, and 0 ⁇ z ⁇ 1.0).
  • the primary powder is added with one or more oxide additives, such as Li 2 O, Fe 2 O 3 , Bi 2 O 3 , V 2 O 5 , MnO 2 , ZnO, Sb 2 O 3 , Sb 2 O 5 , Ta 2 O 5 and the like. Then, the mixture is subjected to second ball-mill, drying, pulverizing,and screening to produce a secondary powder (S350).
  • oxide additives such as Li 2 O, Fe 2 O 3 , Bi 2 O 3 , V 2 O 5 , MnO 2 , ZnO, Sb 2 O 3 , Sb 2 O 5 , Ta 2 O 5 and the like.
  • the secondary powder is added with a small amount of organic material, such as polyvinyl alcohol (PVA) and polyvinyl butyral (PVB), and then a final material is manufactured (S400).
  • organic material such as polyvinyl alcohol (PVA) and polyvinyl butyral (PVB)
  • the secondary powder is formed to produce a specimen (S500).
  • Adsorbed water and adhesive water are removed from the specimen, and combined water and binders are burned away. Then, the specimen is heat-treated in airto produce a sintered specimen (S600).
  • the sintered specimen is subjected to polishing and washing. After screen-printing silver paste on both side of the sintered specimen, and forming a silver electrode, the specimen is applied with a voltage in silicon oil for polarization treatment (S700).
  • FIG. 3 is a diagram illustrating an X-ray diffraction pattern of a piezoelectric material powder manufactured through typical solid state synthesis in air, the diagram being taken after calcination.
  • the typical solid state synthesis indicates the method of manufacturing a piezoelectric material powder by mixing Ag 2 O, K 2 CO 3 , Na 2 CO 3 , and Nb 2 O 5 according to a predetermined mole ratio and performing a typical manufacturing method. From FIG. 3, it can be seen that, in the piezoelectric material powder manufactured by such typical solid state synthesis, a large amount of second phases formed though the calcination was performed at approximately 900°C. In the piezoelectric material powder manufactured by the typical sold state synthesis, the formation of the second phase increases with temperature. Accordingly, the process is preferably performed in an oxygen atmosphere to prevent the formation of second phases.
  • FIG. 4 is a diagram illustrating an X-ray diffraction pattern of a piezoelectric material powder of 0.2AgNbO 3 -0.4KNbO 3 -0.4NaNbO 3 in accordance with an exemplary embodiment, the diagram being taken after calcination at 1,000°C. That is, the X-ray diffraction pattern was taken after calcining the piezoelectric material powder of xAgNbO 3 -yKNbO 3 -zNaNbO 3 , which was manufactured by producing raw material powders including AgNbO 3 , KNbO 3 , and NaNbO 3 , respectively, and then synthesizing the raw material powders in sequence according to an exemplary embodiment. From FIG. 4, it can be seen that second phases did not form and a single phase perovskite compound was synthesized well. This compound is stable up to its melting temperature.
  • FIG. 5 is a diagram illustrating an X-ray diffraction pattern of a piezoelectric material powder of xAgNbO 3 -yKNbO 3 -zNaNbO 3 in accordance with an exemplary embodiment.
  • FIG. 6 is a diagram illustrating an X-ray diffraction pattern of a piezoelectric material powder of 0.2AgNbO 3 -0.8[0.5KNbO 3 -0.5NaNbO 3 ] containing 0.5wt% ZnO as an oxide additive in accordance with an exemplary embodiment, the diagram being taken after calcination in air. From FIG. 6, it can be seen that a compound having a structure of a complete single phase perovskite wassynthesized even when an oxide additive was added thereto.
  • Properties of the piezoelectric material of KNbO 3 -NaNbO 3 manufactured by the typical solid state synthesis, and the piezoelectric material of xAgNbO 3 -yKNbO 3 -zNaNbO 3 manufactured by exemplary embodiments are given in Table 1.
  • Properties shown in Table 1 include measured values of permittivity, electromechanical coupling coefficient (K p ), and mechanical quality factor (Q m ).
  • the measured values of the electromechanical coupling coefficient show examples of a planar mode of a piezoelectricceramic vibrator in a disk-shape.
  • the effect of the present invention is not limited to the planar mode of a piezoelectric ceramic vibrator in a disk-shape, and the present invention is also available in other vibration modes, such as thickness-longitudinal vibration and thickness sliding vibration, used in other piezoelectric ceramic vibrators, particularly, for example, a resonator.
  • the piezoelectric material manufactured in accordance with the exemplary embodiment was measured to have a permittivity of 402 and an electromechanical coupling coefficient, K p of 29.5%
  • the piezoelectric material manufactured in accordance with the exemplary embodiment was measured to have a permittivity of 549 to 575 and an electrochemical coupling coefficient, K p of 38.7% to 39.0%.
  • the piezoelectric materialmanufactured in accordance with the exemplary embodiment was measured to have a mechanical quality factor, Q m of 97 to 99.
  • the piezoelectric materialin accordance with the exemplary embodiment is improved in all of permittivity, electromechanical coupling coefficient (Kp), and mechanical quality factor (Qm) in comparison with the piezoelectric material of pure (K,Na)NbO 3 manufactured by the typical solid state synthesis, and thus has very excellent properties.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Compositions Of Oxide Ceramics (AREA)
PCT/KR2009/003662 2009-05-25 2009-07-06 Piezoelectric material and method of manufacturing the same WO2010137765A1 (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109650884A (zh) * 2018-09-09 2019-04-19 中南大学 一种铌酸银基陶瓷及其制备方法和应用
CN113529059A (zh) * 2021-07-15 2021-10-22 清华大学 铌酸银基无铅反铁电膜及其制备方法和应用
CN114914088A (zh) * 2022-05-25 2022-08-16 南京邮电大学 一种高储能铌酸银陶瓷电容器及其制备方法
CN114956817A (zh) * 2022-06-17 2022-08-30 陕西科技大学 一种高储能密度的铌酸银钠基无铅反铁电陶瓷材料及其制备方法

Families Citing this family (2)

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KR20120065774A (ko) 2010-12-13 2012-06-21 삼성전자주식회사 오디오 처리장치, 오디오 리시버 및 이에 적용되는 오디오 제공방법
CN114940617A (zh) * 2022-06-17 2022-08-26 陕西科技大学 一种稀土掺杂的铌酸银钠基陶瓷材料及其制备方法

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US20040127344A1 (en) * 2002-09-24 2004-07-01 Noritake Co., Limited Lead-free piezoelectric ceramic composition wherein Cu is contained in (KxA1-x)y(Nb1-zBz)O3 perovskite compound, and process of preparing the same
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109650884A (zh) * 2018-09-09 2019-04-19 中南大学 一种铌酸银基陶瓷及其制备方法和应用
CN109650884B (zh) * 2018-09-09 2021-10-15 中南大学 一种铌酸银基陶瓷及其制备方法和应用
CN113529059A (zh) * 2021-07-15 2021-10-22 清华大学 铌酸银基无铅反铁电膜及其制备方法和应用
CN114914088A (zh) * 2022-05-25 2022-08-16 南京邮电大学 一种高储能铌酸银陶瓷电容器及其制备方法
CN114914088B (zh) * 2022-05-25 2023-12-19 南京邮电大学 一种高储能铌酸银陶瓷电容器及其制备方法
CN114956817A (zh) * 2022-06-17 2022-08-30 陕西科技大学 一种高储能密度的铌酸银钠基无铅反铁电陶瓷材料及其制备方法

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