KR101086674B1 - Piezoelectric ceramics composition - Google Patents
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Abstract
본 발명은 Fe2O3, Al2O3, Cr2O3 또는 Ga2O3 로부터 선택된 제1분말, Ta2O5 또는 Nb2O5로부터 선택된 제2분말 및 TiO2 분말을 분쇄하여 혼합 분말을 제조하고, 이 혼합 분말을 형틀에 넣어 프레스 경형 한 후, 고압하에서 가온 소성하여 제조된 압전 세라믹 조성물을 제공한다.The present invention Fe 2 O 3 , Al 2 O 3 , Cr 2 O 3 Or by pulverizing the first powder selected from Ga 2 O 3 , the second powder selected from Ta 2 O 5 or Nb 2 O 5 , and the TiO 2 powder to prepare a mixed powder, and putting the mixed powder into a mold to press harden it. It provides a piezoelectric ceramic composition prepared by heating and baking under high pressure.
세라믹, 압전, 무연 Ceramic, Piezo, Lead Free
Description
본 발명은 압전 세라믹 조성물에 관한 것이다.The present invention relates to piezoelectric ceramic compositions.
압전 세라믹이란 압전 효과를 발생시키는 세라믹을 의미한다. 압전 세라믹과 같은 압전체에 외부로부터 압력이나 진동과 같은 기계에너지를 가하면 판의 양면에 외력에 비례하는 양·음의 전하(電荷)가 나타난다. 또한 압전체에 전기를 흘려주면 전기에너지가 진동에너지로 전환되어 진동을 발생한다. 압전체가 갖는 이러한 효과를 압전효과라고 한다. Piezoelectric ceramic means a ceramic which produces a piezoelectric effect. When mechanical energy such as pressure or vibration is applied to a piezoelectric body such as a piezoelectric ceramic, positive and negative charges in proportion to the external force appear on both sides of the plate. In addition, when electricity is supplied to the piezoelectric body, electrical energy is converted into vibration energy to generate vibration. This effect of the piezoelectric body is called the piezoelectric effect.
이러한 압전효과의 예로 가스레인지의 점화과정을 들 수 있다. 가스레인지의손잡이를 통하여 압전체에 압력을 가하면, 전기를 생성시켜 불꽃이 생성되며 가스와 함께 불이 붙게 되는 효과를 가져오게 된다. An example of such a piezoelectric effect is the ignition process of a gas range. When pressure is applied to the piezoelectric body through the handle of the gas range, sparks are generated by generating electricity, and the fire is caused to ignite with the gas.
또한 초음파 경우는 위 예시와 반대로 압전체에 전기에너지를 가하여 진동에너지로 전환시키는 경우에 해당하며, 가습기나 세척기 등의 생활용품, 초음파 모터 등도 그러한 예이다. 이밖에도 두 가지 압전효과를 복합시킨 예로, 전기에너지를 기계에너지(초음파)로 변환해 내보내고 돌아온 기계에너지를 다시 전기에너지로 바꾼 어군탐지기 및 비파괴검사가 있다. In addition, the ultrasonic case corresponds to the case of converting the piezoelectric material into vibration energy by applying electric energy to the piezoelectric material, and household goods such as a humidifier or a washing machine, an ultrasonic motor, and the like. Another example of the combination of two piezoelectric effects is a fish finder and a nondestructive test that converts electrical energy into mechanical energy (ultrasound) and sends it back to electrical energy.
이와 같이 다양한 분야에서 압전효과를 이용한 제품들이 사용되므로 압전효과의 주매체인 압전체의 소재에 대한 연구가 활발하게 진행되고 있다.As products using the piezoelectric effect are used in various fields as described above, research on the material of the piezoelectric material, which is the main medium of the piezoelectric effect, is being actively conducted.
현재 압전 세라믹으로 전세계적으로 가장 널리 사용되고 있는 대표적인 소재는 Pb(납), Zr(지르코늄), Ti(티탄) 등이다. 대한민국 특허 공보 제498886호, 제586952호 등에 다양한 압전 세라믹 조성물이 소개되어 있으며, 최근 환경 문제에 대한 규제[예를 들어, RoHS의 규정(Directive on Restricfon of the use of certain Hazardous Substances in EEE)]가 늘어남에 따라 환경 친화적이면서도 우수한 압전효과를 나타내는 압전 세라믹 재료의 개발 필요성이 높아지고 있다. Pb (lead), Zr (zirconium), Ti (titanium) and the like are the most widely used materials worldwide as piezoelectric ceramics. Various piezoelectric ceramic compositions have been introduced in Korean Patent Publication Nos. 498886 and 5586952. Recently, regulations on environmental issues [eg, the Directive on Restricfon of the use of certain Hazardous Substances in EEE] Increasingly, there is a growing need to develop piezoelectric ceramic materials that are environmentally friendly and exhibit excellent piezoelectric effects.
이에 본 발명에서는 큰 압전 상수를 가지고 Free Pb(납)의 소재로 친환경적인 압전 세라믹 조성물을 제공하고자 한다.Accordingly, the present invention provides a piezoelectric ceramic composition that is environmentally friendly with a material of free Pb (lead) having a large piezoelectric constant.
본 발명은 Fe2O3 , Al2O3, Cr2O3 또는 Ga2O3 로부터 선택된 제1분말, Ta2O5 또는 Nb2O5로부터 선택된 제2분말 및 TiO2 분말을 분쇄하여 혼합 분말을 제조하고, 이 혼합 분말을 형틀에 넣어 프레스(press) 경형한 후, 고압하에서 가온 소성하여 제조된 압전 세라믹 조성물을 제공한다.The present invention Fe 2 O 3 , Al 2 O 3 , Cr 2 O 3 Alternatively, the first powder selected from Ga 2 O 3 , the second powder selected from Ta 2 O 5 or Nb 2 O 5 , and TiO 2 powder are pulverized to prepare a mixed powder, and the mixed powder is put into a mold to press hard After that, a piezoelectric ceramic composition prepared by heating and baking under high pressure is provided.
본 발명의 압전 세라믹 조성물에서의 제1분말, 제2분말, TiO2 분말의 몰비는 다양하게 변화될 수 있다. 예를 들어, 제1분말: 제2분말: TiO2 분말의 몰비가 1: 1: 2로 혼합되어 제조된 압전 세라믹 조성물이 바람직하다. The molar ratio of the first powder, the second powder, and the TiO 2 powder in the piezoelectric ceramic composition of the present invention may be variously changed. For example, a piezoelectric ceramic composition prepared by mixing a molar ratio of first powder: second powder: TiO 2 powder in a 1: 1: 2 ratio is preferable.
본 발명의 압전 세라믹 조성물에서의 제1분말, 제2분말 및 TiO2 분말의 분쇄 및 혼합은 공지된 분쇄방법인 습식볼밀(Ball Mill), 비즈밀(Beads Mill), 초음파 파동에 의해 균일 혼합될 수 있다. 이때 분쇄된 분말의 입자크기는 다양하게 변화 할 수 있으나, 1마이크로미터 이하로 분쇄 혼합되어 제조된 압전 세라믹 조성물이 바람직하다.The grinding and mixing of the first powder, the second powder and the TiO 2 powder in the piezoelectric ceramic composition of the present invention may be uniformly mixed by a well-known grinding method such as a wet ball mill, beads mill, or ultrasonic wave. Can be. At this time, the particle size of the pulverized powder may vary, but the piezoelectric ceramic composition prepared by pulverizing and mixing to 1 micrometer or less is preferable.
본 발명의 압전 세라믹 조성물은 소성 단계에서 고압하에 제조된 것이 바람직하다. 예를들어, 1GPa 이상 10GPa 이하가 바람직하며, 3GPa 또는 5GPa 에서 가온 소성된 압전 세라믹 조성물이 보다 바람직하다.The piezoelectric ceramic composition of the present invention is preferably prepared under high pressure in the firing step. For example, 1 GPa or more and 10 GPa or less are preferable, and the piezoelectric ceramic composition heated and baked at 3 GPa or 5 GPa is more preferable.
본 발명의 압전 세라믹 조성물은 다음과 같은 소성 단계를 거쳐 제조된 것이바람직하다:The piezoelectric ceramic composition of the present invention is preferably prepared through the following firing step:
0에서 900내지 1300℃로 천천히 가온하는 단계; 이후, 900 내지 1300℃로 일정시간 유지하는 단계: 및 900 내지 1300℃에서 0℃로 천천히 냉각하는 단계.Warming slowly from 0 to 900 to 1300 ° C .; Thereafter, the step of maintaining a constant time at 900 to 1300 ℃: and slowly cooling to 0 ℃ at 900 to 1300 ℃.
각 온도 범위의 단계에서의 가온, 온도 유지 및 냉각 시간은 다양하게 변할 수 있으나, 바람직한 가온 시간은 3시간 내지 10시간, 온도 유지 시간은 7시간 내지 72시간, 냉각 시간은 10시간 내지 24시간이다. The warming, temperature holding and cooling time at the stage of each temperature range may vary, but the preferred warming time is 3 to 10 hours, the temperature holding time is 7 to 72 hours, and the cooling time is 10 to 24 hours. .
또한, 본 발명의 압전 세라믹 조성물은 미반응 된 부분이 없게 하기 위해, 생성된 압전 세라믹 조성물을 다시 분쇄하고 이를 형틀에 넣어 프레스 경형하여 생성된 혼합물을 고압하에서 가온 소성하여 압전 세라믹 조성물을 제조할 수도 있다. In addition, in order that the piezoelectric ceramic composition of the present invention has no unreacted portion, the piezoelectric ceramic composition may be prepared by pulverizing the resultant piezoelectric ceramic composition and putting it in a mold to heat press the resulting mixture under high pressure. have.
또한, 본 발명은 초음파 용착기, 초음파 세척기, 초음파 가공기, 유니몰 프(Unimorph), 바이몰프(Bimorph), 부저(piezoelectric buzzer), 압전 액츄에이터, 초음파 모터, 압전 변압기와 수중센서, 공중초음파 센서, 비파괴 검사용 센서인 압전 액츄에이터용인 압전 세라믹 조성물을 제공한다. 본 발명의 압전 세라믹 조성물은 압전 액츄에이터에 사용하는 것이 바람직하다. In addition, the present invention is an ultrasonic welding machine, ultrasonic cleaner, ultrasonic processing machine, unimorph, bimorph, piezoelectric buzzer, piezoelectric actuator, ultrasonic motor, piezoelectric transformer and underwater sensor, air ultrasonic sensor, non-destructive A piezoelectric ceramic composition for piezoelectric actuators, which are inspection sensors, is provided. It is preferable to use the piezoelectric ceramic composition of this invention for a piezoelectric actuator.
또한, 압전 액츄에이터는 광학(optic)및 비젼(Vision)시스템에서 있어서, 거울(mirror)혹은 렌즈(Lenses)의 포지셔닝(positioning)장치, 마이크로 스캐닝(micro-scanning), 디더링(dithering), 초점(Focusing)장치, 공진조율기(Laser cavity tuning), 섬유 정렬 또는 변형기(Alignment or deformation of fibers), FBG 변형기(Deformation of FBG), 스캐너(Scanners), 초퍼(Choppers), 간섭계(Interferometers), 모듈레이터(Modulators), PDP 글래스 컷팅(PDP glass cutting); 기계적(Mechanics)인 시스템에 있어서, 전자잠금장치(electronic Locking system),도어락(door lock), 도어(sliding door),슬라이딩 커튼(sliding curtain), 슬라이딩 창(sliding window), 툴 포지셔닝(Positioning of tools), 픽앤플레이스(Pick & Place), 클램프(Clamps), 액티브웨지(Active Wedges), 댐핑(Damping), 능동조절기(Active control), 초음파 또는 음파진동 발생기(Generation of ultrasonic or sonic vibrations), NDT, 건강모니터 장치(Health monitoring device); 유체(Fluidics) 시스템에 있어서, 비례밸브(Proportional valves), 펌프(Pumps), 측정기(Measuring), 주입기(Injections), 잉크젯(Ink jet), 작은물방울 발생기(Droplet generators), 질량유량계(Mass flow meter); 전 자(Electronics) 시스템에 있어서, 마스크 포지셔닝(Positioning of masks), 웨이퍼 또는 마그네틱 헤드(wafers or magnetic heads), 비자기적 발동기(Non-magnetic actuation), 서킷브레이커(Circuit breakers), 칩테스팅(Chip testing); 우주항공(Air & Space) 시스템에 있어서, 액티브플랩(Active flaps), 세이프 컨트롤(Shape control), 액티브윙(Active wing); 및 전기에너지(Electric energy) 시스템에 있어서, 압전 발생기(Piezoelectric generator), 에너지하베스팅(Energy harvesting), 전기스위치(Electric switch)인 것을 포함한다.Piezoelectric actuators are also used in optical and vision systems, such as positioning of mirrors or lenses, micro-scanning, dithering, and focusing. Devices, laser cavity tuning, alignment or deformation of fibers, deformation of FBG, scanners, choppers, interferometers, modulators PDP glass cutting; In mechanical systems, electronic locking systems, door locks, sliding doors, sliding curtains, sliding windows, and positioning of tools Pick & Place, Clamps, Active Wedges, Damping, Active Control, Generation of ultrasonic or sonic vibrations, NDT, Health monitoring device; In fluidics systems, proportional valves, pumps, measuring instruments, injectors, ink jets, droplet generators, and mass flow meters ); In electronics systems, positioning of masks, wafers or magnetic heads, non-magnetic actuation, circuit breakers, chip testing ); An air & space system, comprising: active flaps, shape controls, active wings; And in the electric energy (Electric energy) system, it includes a piezoelectric generator (Piezoelectric generator), energy harvesting (Energy harvesting), an electric switch (Electric switch).
본 발명의 고압력하에서 소성된 무연 압전 세라믹 조성물은 무연이라 친환경 소재이면서, 큰 압전 상수를 가진다. 따라서, 본 발명의 압전 세라믹 조성물은 다양한 액츄에이터, 초음파 모터, 초음파 가공기, 압전 변압기, 공중초음파 센서, 비파괴검사용 센서 등에 이용할 수 있다. The lead-free piezoelectric ceramic composition fired under the high pressure of the present invention is lead-free and is an environmentally friendly material, and has a large piezoelectric constant. Therefore, the piezoelectric ceramic composition of the present invention can be used in various actuators, ultrasonic motors, ultrasonic processors, piezoelectric transformers, aerial ultrasonic sensors, nondestructive inspection sensors and the like.
이하 본 발명의 내용을 실시예를 통해 보다 상세하게 설명하기로 한다. 다만 이들 실시예는 본 발명의 내용을 이해하기 위해 제시되는 것일 뿐 본 발명의 권리 범위가 이들 실시예로 한정되는 것은 아니다.Hereinafter, the contents of the present invention will be described in more detail with reference to Examples. However, these examples are only presented to understand the content of the present invention, but the scope of the present invention is not limited to these examples.
이하 실시예에서 사용된 재료는 고순도화학, 삼전화학 또는 Aldrich 사에서 구입하여 사용하였다.The materials used in the following examples were purchased from high purity chemistry, trielectric chemistry or Aldrich.
고압력에서 제조된 세라믹 Ceramics manufactured at high pressure 엑츄에이터용Actuator 압전 세라믹 조성물 제조 Piezoelectric Ceramic Composition Preparation
< 실시예 1> 3 GPa 압력하에서 소성된 FeTiTaO6 압전 세라믹 제조 <Example 1> The fired under pressure 3 GPa FeTiTaO 6 Piezoelectric ceramic manufacturing
원료 분말 Fe2O3 분말 (1.049 g), TiO2 분말(1.049 g), Ta2O5 분말(2.902 g) 를 혼합한 후에, 혼합분말을 분쇄 평균입경이 1 마이크로미터 이하가 되도록 분쇄하였다. 이후, 분쇄된 혼합분말을 형틀에 넣은 후 Press (2 GPa) (2인치 두께 5mm의 치수로 프레스 경형)한 후에, 프레스 경형된 물질을 다음과 같은 조건하에서 전기로에서 1차 소성하였다.Raw material powder Fe 2 O 3 powder (1.049 g), TiO 2 powder (1.049 g), and Ta 2 O 5 powder (2.902 g) were mixed, and the mixed powder was pulverized so that the average particle diameter was 1 micrometer or less. Thereafter, the pulverized mixed powder was put in a mold and then Press (2 GPa) (press hardening to a dimension of 2 inches thick 5 mm), and then the press hardened material was first calcined in an electric furnace under the following conditions.
1. 전기로에서 3GPa압력하 0 ℃ 에서 1200℃ 5 h 시간 동안 서서히 가열하였다. 1. The furnace was slowly heated at 0 ° C. and 1200 ° C. for 5 h under 3GPa pressure.
2. 전기로에서 3GPa 압력하 1200℃도 에서 10 시간 동안 가열 하였다. 2. The electric furnace was heated at 1200 ° C. for 10 hours under 3GPa pressure.
3. 전기로에서 3GPa압력하에서 1200℃ 도 에서 0℃로 5시간 동안 냉각시켰다. 3. In an electric furnace, it cooled for 5 hours from 1200 degreeC to 0 degreeC under 3 GPa pressure.
이후, 1차 소성물을 상기 원료 혼합 분쇄 방법과 동일하게 분쇄 평균입경이 1 마이크로미터 이하가 되도록 혼합 분쇄하고, 형틀에 넣은 후 Press (2 GPa로 2인치 두께 5mm의 치수로 프레스)경형한 후, 1차 소성과 동일한 방법으로 2차 소성하였다. Thereafter, the primary calcined product was mixed and ground to have a grinding average particle diameter of 1 micrometer or less in the same manner as the above-mentioned raw material mixing and grinding method, and put into a mold and press (2 GPa to 2 mm thick 5 mm in size) and then hardened. And secondary firing in the same manner as the primary firing.
이후, 2차 소성물을 1차 소성물과 동일한 방법 및 조건으로, 혼합 분쇄, 프 레스 경형 및 소성하여, 표제의 압전 세라믹 조성물을 제조하였다. Thereafter, the secondary calcined product was mixed pulverized, press hardened and calcined in the same manner and conditions as the primary calcined product to prepare the title piezoelectric ceramic composition.
<실시예2>3GPa 압력하에서 소성된 AlTiTaO6 압전 세라믹 조성물 제조Example 2 AlTiTaO 6 calcined under 3 GPa pressure Piezoelectric Ceramic Composition Preparation
실시예1에서 사용한 원료 분말 대신 Al2O3 분말 (0.725 g), TiO2 분말(1.135 g), Ta2O5 분말(3.140 g) 을 사용한 것 및 소성을 1200℃ 대신 1300℃ 온도로 한 것을 제외하고는 실시예1과 동일한 방법으로 표제의 압전 세라믹 조성물을 제조하였다. Al 2 O 3 powder (0.725 g), TiO 2 powder (1.135 g), Ta 2 O 5 powder (3.140 g) was used instead of the raw material powder used in Example 1, and the firing was performed at 1300 ° C. instead of 1200 ° C. Except for the same piezoelectric ceramic composition was prepared in the same manner as in Example 1.
<실시예3> 3GPa 압력하에서 소성된 CrTiTaO6 압전 세라믹 조성물 제조Example 3 CrTiTaO 6 calcined under 3 GPa pressure Piezoelectric Ceramic Composition Preparation
실시예1에서 사용한 원료 분말 대신 Cr2O3 분말 (1.008 g), TiO2 분말(1.060 g), Ta2O5 분말(2.932 g) 을 사용한 것 및 소성을 1200℃ 대신 1300℃ 온도로 한 것을 제외하고는 실시예1과 동일한 방법으로 표제의 압전 세라믹 조성물을 제조하였다. Cr 2 O 3 powder (1.008 g), TiO 2 powder (1.060 g), Ta 2 O 5 powder (2.932 g) was used instead of the raw material powder used in Example 1, and the firing was performed at a temperature of 1300 ° C. instead of 1200 ° C. Except for the same piezoelectric ceramic composition was prepared in the same manner as in Example 1.
<실시예4>3GPa 압력하에서 소성된 GaTiTaO6 압전 세라믹 조성물 제조Example 4 GaTiTaO 6 calcined under 3 GPa pressure Piezoelectric Ceramic Composition Preparation
실시예1에서 사용한 원료 분말 대신 Ga2O3 분말 (1.188 g), TiO2 분말(1.012 g), Ta2O5 분말(2.800 g) 을 사용한 것 및 소성을 1200℃ 대신 1250℃ 온도로 한 것 을 제외하고는 실시예1과 동일한 방법으로 표제의 압전 세라믹 조성물을 제조하였다. Using Ga 2 O 3 powder (1.188 g), TiO 2 powder (1.012 g), Ta 2 O 5 powder (2.800 g) instead of the raw material powder used in Example 1, and firing at 1250 ° C. instead of 1200 ° C. Except for producing the title piezoelectric ceramic composition in the same manner as in Example 1.
<실시예5>3GPa 압력하에서 소성된 FeTiNbO6 압전 세라믹 조성물 제조Example 5 FeTiNbO 6 calcined under 3 GPa pressure Piezoelectric Ceramic Composition Preparation
실시예1에서 사용한 원료 분말 대신 Fe2O3 분말 (1.364 g), TiO2 분말(1.365 g), Nb2O5 분말(2.271 g) 을 사용한 것 및 소성을 1200℃ 대신 1250℃ 온도로 한 것을 제외하고는 실시예1과 동일한 방법으로 표제의 압전 세라믹 조성물을 제조하였다. Fe 2 O 3 powder (1.364 g), TiO 2 powder (1.365 g), Nb 2 O 5 powder (2.271 g) was used instead of the raw material powder used in Example 1, and the calcining was performed at a temperature of 1250 ° C. instead of 1200 ° C. Except for the same piezoelectric ceramic composition was prepared in the same manner as in Example 1.
<실시예6>3GPa 압력하에서 소성된 AlTiNbO6 압전 세라믹 조성물 제조Example 6 AlTiNbO 6 calcined at 3 GPa pressure Piezoelectric Ceramic Composition Preparation
실시예1에서 사용한 원료 분말 대신 원료 분말 Al2O3 분말 (0.966 g), TiO2 분말(1.514 g), Nb2O5 분말(2.520 g)을 사용한 것 및 소성을 1200℃ 대신 1300℃ 온도로 한 것을 제외하고는 실시예1과 동일한 방법으로 표제의 압전 세라믹 조성물을 제조하였다. Raw material powder Al 2 O 3 powder (0.966 g), TiO 2 powder (1.514 g), Nb 2 O 5 powder (2.520 g) instead of the raw material powder used in Example 1 and firing at a temperature of 1300 ° C. instead of 1200 ° C. Except one, the title piezoelectric ceramic composition was prepared in the same manner as in Example 1.
<실시예7> 3GPa 압력하에서 소성된 CrTiNbO6 압전 세라믹 조성물 제조Example 7 CrTiNbO 6 calcined at 3 GPa pressure Piezoelectric Ceramic Composition Preparation
실시예1에서 사용한 원료 분말 대신 Cr2O3 분말 (1.316 g), TiO2 분말(1.383 g), Nb2O5 분말(2.301 g) 을 사용한 것 및 소성을 1200℃ 대신 1250℃ 온도로 한 것을 제외하고는 실시예1과 동일한 방법으로 표제의 압전 세라믹 조성물을 제조하였다. Cr 2 O 3 powder (1.316 g), TiO 2 powder (1.383 g), Nb 2 O 5 powder (2.301 g) in place of the raw material powder used in Example 1, and the firing at 1250 ° C. instead of 1200 ° C. Except for the same piezoelectric ceramic composition was prepared in the same manner as in Example 1.
<실시예8> 3GPa 압력하에서 소성된 GaTiNbO6 압전 세라믹 조성물 제조Example 8 GaTiNbO 6 calcined at 3 GPa pressure Piezoelectric Ceramic Composition Preparation
실시예1에서 사용한 원료 분말 대신 Ga2O3 분말 (1.529 g), TiO2 분말(1.303 g), Nb2O5 분말(2.168 g) 을 사용한 것 및 소성을 1200℃ 대신 1100℃ 온도로 한 것을 제외하고는 실시예1과 동일한 방법으로 표제의 압전 세라믹 조성물을 제조하였다. Ga 2 O 3 powder (1.529 g), TiO 2 powder (1.303 g), Nb 2 O 5 powder (2.168 g) instead of the raw material powder used in Example 1, and the firing at 1100 ° C. instead of 1200 ° C. Except for the same piezoelectric ceramic composition was prepared in the same manner as in Example 1.
<실시예 9 > 5GPa 압력하에서 소성된 FeTiTaO6 압전 세라믹 조성물 제조Example 9 FeTiTaO 6 calcined at 5 GPa pressure Piezoelectric Ceramic Composition Preparation
실시예1에서 소성압력을 3GPa 대신 5GPa로 한 것을 제외하고는 실시예1과 동일한 방법으로 하여 표제의 세라믹 조성물을 제조하였다. The title ceramic composition was prepared in the same manner as in Example 1 except that the baking pressure in Example 1 was set to 5 GPa instead of 3 GPa.
<실시예10>5GPa 압력하에서 소성된 AlTiTaO6 압전 세라믹 조성물 제조Example 10 AlTiTaO 6 calcined under 5 GPa pressure Piezoelectric Ceramic Composition Preparation
실시예2에서 소성압력을 3GPa 대신 5GPa로 한 것을 제외하고는 실시예2과 동일한 방법으로 하여 표제의 세라믹 조성물을 제조하였다. The title ceramic composition was prepared in the same manner as in Example 2 except that the baking pressure in Example 2 was set to 5 GPa instead of 3 GPa.
<실시예11> 5GPa 압력하에서 소성된 CrTiTaO6 압전 세라믹 조성물 제조Example 11 CrTiTaO 6 calcined at 5 GPa pressure Piezoelectric Ceramic Composition Preparation
실시예3에서 소성압력을 3GPa 대신 5GPa로 한 것을 제외하고는 실시예3과 동일한 방법으로 하여 표제의 세라믹 조성물을 제조하였다. The title ceramic composition was prepared in the same manner as in Example 3 except that the baking pressure in Example 3 was set to 5 GPa instead of 3 GPa.
<실시예12>5GPa 압력하에서 소성된 GaTiTaO6 압전 세라믹 조성물 제조Example 12 GaTiTaO 6 calcined at 5 GPa pressure Piezoelectric Ceramic Composition Preparation
실시예4에서 소성압력을 3GPa 대신 5GPa로 한 것을 제외하고는 실시예4와 동일한 방법으로 하여 표제의 세라믹 조성물을 제조하였다. The title ceramic composition was prepared in the same manner as in Example 4 except that the baking pressure in Example 4 was set to 5 GPa instead of 3 GPa.
<실시예13>5GPa 압력하에서 소성된 FeTiNbO6 압전 세라믹 조성물 제조Example 13 FeTiNbO 6 calcined at 5 GPa pressure Piezoelectric Ceramic Composition Preparation
실시예5에서 소성압력을 3GPa 대신 5GPa로 한 것을 제외하고는 실시예5와 동일한 방법으로 하여 표제의 세라믹 조성물을 제조하였다. The title ceramic composition was prepared in the same manner as in Example 5 except that the baking pressure in Example 5 was set to 5 GPa instead of 3 GPa.
<실시예14>5GPa 압력하에서 소성된 AlTiNbO6 압전 세라믹 조성물 제조Example 14 AlTiNbO 6 calcined at 5 GPa pressure Piezoelectric Ceramic Composition Preparation
실시예6에서 소성압력을 3GPa 대신 5GPa로 한 것을 제외하고는 실시예6과 동일한 방법으로 하여 표제의 세라믹 조성물을 제조하였다. The title ceramic composition was prepared in the same manner as in Example 6 except that the baking pressure in Example 6 was 5GPa instead of 3GPa.
<실시예15> 5GPa 압력하에서 소성된 CrTiNbO6 압전 세라믹 조성물 제조Example 15 CrTiNbO 6 calcined at 5 GPa pressure Piezoelectric Ceramic Composition Preparation
실시예7에서 소성압력을 3GPa 대신 5GPa로 한 것을 제외하고는 실시예7과 동 일한 방법으로 하여 표제의 세라믹 조성물을 제조하였다. The title ceramic composition was prepared in the same manner as in Example 7, except that the baking pressure in Example 7 was set to 5 GPa instead of 3 GPa.
<실시예16> 5GPa 압력하에서 소성된 GaTiNbO6 압전 세라믹 조성물 제조Example 16 GaTiNbO 6 Calcined at 5 GPa Pressure Piezoelectric Ceramic Composition Preparation
실시예8에서 소성압력을 3GPa 대신 5GPa로 한 것을 제외하고는 실시예8과 동일한 방법으로 하여 표제의 세라믹 조성물을 제조하였다. The title ceramic composition was prepared in the same manner as in Example 8 except that the baking pressure in Example 8 was 5GPa instead of 3GPa.
<실시예17 내지 32> <Examples 17 to 32>
실시예 1 내지 실시예16의 소성단계에서, 진공 전기로를 사용하여 Ti금속을 넣어 산소를 제거하여, 실시예 1 내지 실시예 16에서 "M'TiN'O6"대신 각 실시예 1 내지 16에 대응되는 "M'TiN'O2"를(여기서, M'은 Fe, Al, Cr 또는 Ga이며, N'은 Ti 또는 Ta이다) 실시예 17 내지 실시예 32로 제조하였다. In the firing steps of Examples 1 to 16, a Ti metal was added to remove oxygen by using a vacuum electric furnace, and in Examples 1 to 16, instead of "M'TiN'O 6 " in Examples 1 to 16, The corresponding "M'TiN'O 2 ", where M 'is Fe, Al, Cr or Ga and N' is Ti or Ta, was prepared in Examples 17-32.
<실험예> 압전성 확인Experimental Example Confirmation of Piezoelectricity
상기 실시예에서 제조한 압전 세라믹 조성물의 single crystal [001]에 대하여, 실온 300K에서, , 임피던스분석기(Agilent 4294A)로 주파수를 측정하고 Berlincourt d33 meter를 이용하여 압전상수(d33)를 측정하였다(진공유전율 8.854x 10ⁿ F/m ; n = -12). 그 결과는 하기 표1 및 표2와 같다.For a single crystal [001] of the piezoelectric ceramic composition prepared in the above example, at room temperature 300K, the frequency was measured with an impedance analyzer (Agilent 4294A) and the piezoelectric constant (d33) was measured using a Berlincourt d33 meter (vacuum). Dielectric constant 8.854 × 10 μs F / m; n = -12). The results are shown in Tables 1 and 2 below.
<표1> 3GPa 압력에서 소성된 압전 세라믹 조성물의 압전 상수TABLE 1 Piezoelectric constants of piezoelectric ceramic compositions fired at 3GPa pressure
<표2> 5GPa압력에서 소성된 압전 세라믹 조성물의 압전 상수Table 2: Piezoelectric constants of piezoelectric ceramic composition fired at 5GPa pressure
상기 표에서 나타낸 바와 같이, 고 압력하에서 소성한 압전 세라믹 조성물은 유전율(d33) 이 더욱 향상됨을 알 수 있다.As shown in the table, it can be seen that the dielectric constant d33 of the piezoelectric ceramic composition fired under high pressure is further improved.
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