KR960006244B1 - Piezo electric composition - Google Patents
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- KR960006244B1 KR960006244B1 KR1019880014645A KR880014645A KR960006244B1 KR 960006244 B1 KR960006244 B1 KR 960006244B1 KR 1019880014645 A KR1019880014645 A KR 1019880014645A KR 880014645 A KR880014645 A KR 880014645A KR 960006244 B1 KR960006244 B1 KR 960006244B1
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- 239000000203 mixture Substances 0.000 title claims abstract description 18
- 239000000919 ceramic Substances 0.000 abstract description 4
- 239000000843 powder Substances 0.000 description 8
- 238000006467 substitution reaction Methods 0.000 description 4
- 239000007787 solid Substances 0.000 description 3
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000004677 Nylon Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- 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
- C04B35/48—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 zirconium or hafnium oxides, zirconates, zircon or hafnates
- C04B35/49—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 zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates
- C04B35/491—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 zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates based on lead zirconates and lead titanates, e.g. PZT
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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
- H10N30/01—Manufacture or treatment
- H10N30/09—Forming piezoelectric or electrostrictive materials
- H10N30/093—Forming inorganic materials
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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
- H10N30/853—Ceramic compositions
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Abstract
Description
제1도는 본 발명의 조성범위를 나타내는 삼각도.1 is a triangular diagram showing the composition range of the present invention.
제2도는 WO3첨가에 따른 압전상수(d33)와 압축 파괴강도를 나타낸 그래프.2 is a graph showing the piezoelectric constant (d 33 ) and the compressive fracture strength according to the addition of WO 3 .
제3도는 Sr치환에 따른 압전상수(d33)와 압축파괴강도의 변화를 나타낸 그래프.·3 is a graph showing changes in piezoelectric constant (d 33 ) and compressive fracture strength according to Sr substitution.
* 도면의 주요 부분에 대한 부호의 설명* Explanation of symbols for the main parts of the drawings
X : 압축파괴강도 O : 압전상수X: Compressive fracture strength O: Piezoelectric constant
본 발명은 고주파용 압전진동사 및 고체 초음파 지연선에 사용되는 압전세라믹 조성물에 관한 것으로써,Pb(Co1/3Sb2/3)O3, PbTiO3및 PbZrO3를 주성분으로 하고, 여기에 Pb의 일부를 Sr로 치환함과 동시에 소량의 WO3를 첨가하여 압전상수와 압축파괴강도가 동시에 높고 PbO 분위기 분말을 사용하지 않아도 안정성이 있는 특성을 나타내며, 낮은 온도에서 소결가능한 조성물에 관한 것이다.The present invention relates to a piezoceramic composition used in high-frequency piezoelectric vibrators and solid ultrasonic delay lines, comprising Pb (Co 1/3 Sb 2/3 ) O 3 , PbTiO 3 and PbZrO 3 as main components. Substituting a portion of Pb with Sr and adding a small amount of WO 3 at the same time high piezoelectric constant and compressive fracture strength and exhibits a stable characteristic even without using a PbO atmosphere powder, and relates to a composition sinterable at low temperatures.
종래, 압전세라믹 조성물로서는 BaTiO3, PbTiO3, PZT계를 주성분으로 하고, 여기에 Mn등의 첨가물을 소량 첨가한 것 또는 PMN, PCN등을 첨가한 것이 널리 사용되어 왔으나, 이들은 1300℃ 이상의 고온에서 소결되고 PbO증발을 막기 위해 PbO분위기 분말을 사용하는 번거로움이 있으며, 압전상수는 높으나 압축파괴강도가 낮아 고주파용의 얇은 제품이나 고체 초음파 지연선등의 사용에는 부적합 하였다.Conventionally, as piezoceramic compositions, those containing BaTiO 3 , PbTiO 3 , and PZT system as main components, and those containing small amounts of additives such as Mn or PMN, PCN, etc. have been widely used. PbO atmosphere powders are sintered to prevent PbO evaporation, and the piezoelectric constant is high, but the compressive fracture strength is low, making it unsuitable for use in thin products for high frequency or solid ultrasonic delay lines.
따라서, 본 발명의 목적은 전술함 문제점을 해결하기 위해서 Pb(Co1/3Sb2/3)O3, PbTiO3PbZrO3를 주성분으로 하고, 여기에 Pb의 일부를 Sr로 치환하고, 소량의 WO3를 첨가하여 압전상수와 압축파괴강도가 모두 높으며,1200℃의 낮은 온도에서도 소결되여 PbO분위기 분말을 사용하지 않고도 안정된 특성을 나타내는 압전 세라믹 조성물을 제공하는데 있다.Accordingly, an object of the present invention is to solve the above-mentioned problems, Pb (Co 1/3 Sb 2/3 ) O 3 , PbTiO 3 PbZrO 3 as a main component, a portion of Pb is replaced with Sr, and a small amount of WO 3 is added to provide a piezoelectric ceramic composition having both high piezoelectric constant and compressive fracture strength, and sintered even at a low temperature of 1200 ° C. to exhibit stable characteristics without using PbO atmosphere powder.
상기 목적을 달성하고자 본 발명의 조성물은 xPb(Co1/3Sb2/3)O3-yPbTiO3- zPbZrO3(o≤x≤40,37≤y≤53,x+y+z=100)의 3성분계를 기본으로 하여 이중 Pb의 일부를 Sr로 치환하고, 여기에 WO3를 소량 첨가한 것으로, 좀더 상세하게로는 본 발명의 조성물은 상기 3성분계의 기본성분에 Pb의 일부를 Sr로 2∼5몰% 치환하고, 여기에 WO3를 0.2∼1.2wt% 첨가한 것이다. 제1도는 본 발명의 조성범위를 나타내는 삼각도로서 빗급친 부분이 바로 본 발명의 조성범위이다.The composition of the present invention to achieve the above object is xPb (Co 1/3 Sb 2/3 ) O 3 -yPbTiO 3 -zPbZrO 3 (o≤x≤40,37≤y≤53, x + y + z = 100) On the basis of the three-component system of, a part of the double Pb is substituted with Sr, and a small amount of WO 3 is added thereto. More specifically, the composition of the present invention is based on the three-component system. 2 to 5 mol% is a substituted, added 0.2~1.2wt% of WO 3 herein. 1 is a triangular diagram showing the composition range of the present invention, and the hatched portion is the composition range of the present invention.
Sr치환량이 상기 2몰% 미만일 경우에는 소결온도가 높아지고 재현성이 저하되어 분위기 분말(PbO)을 사용해야 하여, 상기 5몰% 를 초과할 경우에는 압전상수 및 압축파괴강도가 낮아지고 밀도 및 수축율등이 낮아져 균등성이 저하된다.When the Sr substitution amount is less than 2 mol%, the sintering temperature is increased and the reproducibility is lowered. Therefore, the atmosphere powder (PbO) must be used. When the Sr substitution amount is higher than 5 mol%, the piezoelectric constant and the compressive fracture strength are lowered, and the density and shrinkage rate are increased. It lowers and uniformity falls.
또한, WO3의 첨가 wt% 가 1.2를 초과하면 낱알(grain)크기가 너무 작아져 기공이 과다하게 생기므로 강도가 적어지고 밀도가 작아지게 되며, 상기 0.2미만일 경우 본 발명에 따른 만족할만한 효과를 얻을 수 없게 된다.In addition, when the addition wt% of WO 3 exceeds 1.2, the grain size is too small, so that pores are excessively generated, so that the strength is decreased and the density is decreased. When the amount is less than 0.2, the satisfactory effect of the present invention is achieved. You won't get it.
본 발명의 압전세라믹 조성물은 압전상수와 압축파괴강도가 동시에 높아서 앎은 소자를 사용하는 고주파용 초음파 진동자 및 고체 초음파 지연선의 제조에 사용될 수 있고, 또한 PbO분위기 조절용 분말 없이도 제반 특성을 일정하게 나타내며,1200℃ 의 저온에서 소결할 수 있다.The piezoceramic composition of the present invention can be used in the manufacture of high frequency ultrasonic vibrator and solid ultrasonic delay line using thin element due to high piezoelectric constant and compressive fracture strength at the same time, and also exhibits constant characteristics without PbO atmosphere control powder. It can sinter at low temperature of 1200 degreeC.
다음의 실시예에서 본 발명의 조성물의 제조방법 및 그 효과에 대하여 구체적으로 설명한다. 그러나, 다음의 실시예가 본 발명의 범위를 한정하는 것은 아니다.In the following examples, the preparation method of the composition of the present invention and the effects thereof will be described in detail. However, the following examples do not limit the scope of the present invention.
(실시예 1∼실시예 16)(Examples 1 to 16)
본 발명의 압전세라믹을 얻는 출발원료는 99% 순도 이상의 PbO, TiO2, ZrO2, CoO, Sb2O5, SrCO3, WO3분말을 사용하였다.As starting materials for obtaining the piezoelectric ceramics of the present invention, PbO, TiO 2 , ZrO 2 , CoO, Sb 2 O 5 , SrCO 3 , and WO 3 powder having 99% purity or higher were used.
이를 표 1의 조성에 맞게 평량한후 플래니터리밀(Planetary mill)로 나일론 Jar와 YTZ볼을 사용하여 4시간 혼합하였다. 혼합분말을 건조후 전기로를 사용하여 800∼850℃ 에서 하소한 후 플래니터리밀로 4시간분쇄하였다. 본쇄후 분말에 3wt%의 순수를 가하여 150kg/㎠ 의 압력으로 성형하여 두꼐 2mm,Ø25mm의 디스크를 제작하였다.This was weighed according to the composition of Table 1 and mixed for 4 hours using a nylon jar and a YTZ ball as a planetary mill. The mixed powder was dried and calcined at 800 to 850 ° C. using an electric furnace, and then ground in a planetary mill for 4 hours. After crushing, 3 wt% of pure water was added to the powder and molded at a pressure of 150 kg / cm 2 to prepare a disk having a thickness of 2 mm and Ø 25 mm.
이 디스크를 1200∼1230℃에서 2시간 소결하였으여, 이매 PbO분위기 조절용 분말을 사용하지 않았다. 소결시편에 Ag페이스트를 소부한 후 100℃의 실리콘 오일 속에서 직류전기 3kv/mm를 10분간 인가하여 분극처리하여 압전세라믹을 얻었다.The disc was sintered at 1200 to 1230 ° C. for 2 hours, so that no powder for controlling the bimetallic PbO atmosphere was used. Ag paste was sintered to the sintered specimen, and then a piezoelectric ceramic was obtained by applying a 3 kV / mm DC electric current for 10 minutes in silicon oil at 100 ° C.
이렇게 제작된 압전세라믹을 24시간 방치한 후 d33piezo meter를 이용하여 압전상수를 측정하였으며,UTM(Universal Testing Machine, ZWIC사 제품)을 이용하여 압축파괴강도를 측정하여 그 결과를 표1에 기재하였다.After the piezoceramic was left for 24 hours, the piezoelectric constant was measured using a d 33 piezo meter, and the compressive fracture strength was measured using a universal testing machine (UTM). The results are shown in Table 1. It was.
아울러, 이를 기초로 제2도 및 제3도에 WO3첨가량에 따른 d33및 압축파괴강도 변화와 Sr치환량에 따른 d33및 압축파괴강도 변화를 도시하였다.In addition, based on this, the change of d 33 and compressive fracture strength according to WO 3 addition amount and the change of d 33 and compressive fracture strength according to Sr substitution amount are shown in FIG. 2 and FIG. 3.
여기서 x는 압축파괴강도를 의미하며, o는 압전상수를 의미한다.Where x stands for compressive fracture strength and o stands for piezoelectric constant.
[표 1]TABLE 1
*는 비교예* Is a comparative example
Claims (3)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1019880014645A KR960006244B1 (en) | 1988-11-08 | 1988-11-08 | Piezo electric composition |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1019880014645A KR960006244B1 (en) | 1988-11-08 | 1988-11-08 | Piezo electric composition |
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| Publication Number | Publication Date |
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| KR900007754A KR900007754A (en) | 1990-06-01 |
| KR960006244B1 true KR960006244B1 (en) | 1996-05-11 |
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| KR1019880014645A KR960006244B1 (en) | 1988-11-08 | 1988-11-08 | Piezo electric composition |
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