KR0145122B1 - Dielectric ceramic compositions - Google Patents
Dielectric ceramic compositionsInfo
- Publication number
- KR0145122B1 KR0145122B1 KR1019950052731A KR19950052731A KR0145122B1 KR 0145122 B1 KR0145122 B1 KR 0145122B1 KR 1019950052731 A KR1019950052731 A KR 1019950052731A KR 19950052731 A KR19950052731 A KR 19950052731A KR 0145122 B1 KR0145122 B1 KR 0145122B1
- Authority
- KR
- South Korea
- Prior art keywords
- dielectric
- multilayer ceramic
- dielectric constant
- composition
- breakdown voltage
- Prior art date
Links
- 239000000203 mixture Substances 0.000 title claims abstract description 22
- 239000000919 ceramic Substances 0.000 title claims abstract description 14
- 229910021193 La 2 O 3 Inorganic materials 0.000 claims description 6
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 6
- 239000003985 ceramic capacitor Substances 0.000 abstract description 14
- 238000009413 insulation Methods 0.000 abstract description 14
- 230000015556 catabolic process Effects 0.000 abstract description 13
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 4
- 238000005245 sintering Methods 0.000 abstract description 4
- 230000010485 coping Effects 0.000 abstract 1
- 239000003989 dielectric material Substances 0.000 abstract 1
- 238000000034 method Methods 0.000 description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 239000000654 additive Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910017493 Nd 2 O 3 Inorganic materials 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005686 electrostatic field Effects 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
- H01G4/06—Solid dielectrics
- H01G4/08—Inorganic dielectrics
- H01G4/12—Ceramic dielectrics
- H01G4/1209—Ceramic dielectrics characterised by the ceramic dielectric material
- H01G4/1218—Ceramic dielectrics characterised by the ceramic dielectric material based on titanium oxides or titanates
- H01G4/1227—Ceramic dielectrics characterised by the ceramic dielectric material based on titanium oxides or titanates based on alkaline earth titanates
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3227—Lanthanum oxide or oxide-forming salts thereof
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3251—Niobium oxides, niobates, tantalum oxides, tantalates, or oxide-forming salts thereof
- C04B2235/3255—Niobates or tantalates, e.g. silver niobate
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3262—Manganese oxides, manganates, rhenium oxides or oxide-forming salts thereof, e.g. MnO
- C04B2235/3267—MnO2
Landscapes
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Power Engineering (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Inorganic Insulating Materials (AREA)
Abstract
본 발명은 미국 EIA에서 정한 Y5U 규격특성을 만족시키며 높은 유전율과 절연 저항과 절연 파괴 전압이 높고, 결정립의 입경이 작고 치밀한 소결 상태를 나타내고 적층 세라믹 콘덴서 제조용 유전체 조성물에 관한 것이다.The present invention relates to a dielectric composition for manufacturing multilayer ceramic capacitors, which satisfies the Y5U standard characteristics defined by the US EIA, exhibits high dielectric constant, high insulation resistance, high dielectric breakdown voltage, small grain size and compact sintered state.
최근의 제품의 소형화와 고용량화에 대응하기 위하여 정전 용량을 높히기 위해서 높은 유전율을 갖는 유전체를 사용하고 유전체 두께를 얇게 하고, 고신뢰성의 적층 세라믹 콘덴서를 제조하기 위해서 소결후 유전체의 결정립이 미세하고 치밀하며 높은 절연 저항과 높은 절연 파괴 전압을 갖는 유전체의 개발이 필수적이다.In order to cope with the recent miniaturization and high capacity, the dielectric having high dielectric constant is used to increase the capacitance, the dielectric thickness is thin, and the grain of the dielectric is fine and dense after sintering to manufacture a highly reliable multilayer ceramic capacitor. Development of dielectrics with high insulation resistance and high dielectric breakdown voltage is essential.
본 발명의 세라믹 유전체 조성물을 적층 세라믹 콘덴서에 이용하면 유전체 층의 두께를 얇게할 수 있어 원가 절감의 효과가 클 뿐 아니라, 소형화 및 고용량화에 대응할 수 있는 고신뢰성의 제품을 생산할 수 있다.When the ceramic dielectric composition of the present invention is used in a multilayer ceramic capacitor, the thickness of the dielectric layer can be reduced, so that the cost reduction effect is large, and a high reliability product capable of coping with miniaturization and high capacity can be produced.
Description
제1도는 적층 세라믹 콘덴서의 개략도이다.1 is a schematic diagram of a multilayer ceramic capacitor.
제2도는 EIA의 적층 세라믹 콘덴서에 대한 Y5U 온도 특성규격을 나타내는 유전율의 온도 특성 범위와 본 발명의 실시예 3에 따른 유전율의 온도 특성을 도시한 것이다.Figure 2 shows the temperature characteristic range of the dielectric constant showing the Y5U temperature characteristic specification for the multilayer ceramic capacitor of the EIA and the temperature characteristic of the dielectric constant according to the third embodiment of the present invention.
*도면의 주요부분에 대한 부호의 설명* Explanation of symbols for main parts of the drawings
1 : 유전체 2 : 내부전극1 dielectric 2 internal electrode
3 : 외부전극 A : Y5U규격에서 정한 유전율의 온도 특성범위3: External electrode A: Temperature characteristic range of dielectric constant specified in Y5U standard
B : 실시예 3에 따른 조성물의 유전율의 온도특성(temperature characteristics ; T.C)B: temperature characteristics (T.C) of the dielectric constant of the composition according to Example 3
본 발명의 민생용 및 산업용 전자 기기 등에 사용되는 대표적인 부품의 하나인 적층 세라믹 콘덴서 제조용 유전체 조성물에 관한 것으로, 특히 미국 EIA(Electronic Industrial Association)에서 정한 Y5U 규격특성(-30℃∼+85℃의 온도 범위에서 25℃에서의 유전율을 기준으로 하여 온도 변화에 따른 유전율의 변화율이 +22%∼-56% 이내)을 만족시키는 동시에 8,200∼9,300정도의 높은 유전율과 절연 저항이 1013Ωcm 이상이고, 절연 파괴 전압이 14KV/mm 이상이며, 결정립의 입경이 작고 치밀한 소결 상태를 나타낼 수 있는 세라믹 유전체 조성물에 관한 것이다.The present invention relates to a dielectric composition for manufacturing a multilayer ceramic capacitor, which is one of the typical components used in consumer and industrial electronic devices, and the like, in particular, a Y5U standard characteristic (-30 ° C. to + 85 ° C. temperature) defined by the US EIA (Electronic Industrial Association). Range of dielectric constant at 25 ° C based on the dielectric constant at 25 ℃ within + 22% to -56%), and has a high dielectric constant of 8,200 to 9,300 and insulation resistance of 10 13 Ωcm or more, and insulation It relates to a ceramic dielectric composition having a breakdown voltage of 14 KV / mm or more and having a small grain size and exhibiting a dense sintered state.
표적실장이란 기판의 면과 부품의 면을 면과 면의 대응방식으로 접속하는 방법을 말한다.Target mounting refers to a method of connecting the surface of a board | substrate and the surface of a component by the surface-to-surface correspondence method.
여기에서 유전체(Dielectric Substance)란 정전기장을 가할 때 전기분극(電氣分極)은 생기나 직류전류는 생기지 않는 물질을 말한다.Here, dielectric substance refers to a substance in which electric polarization occurs but no direct current occurs when an electrostatic field is applied.
최근 적층 세라믹 콘덴서는 각종 전자 기기의 소형, 경량화의 추세에 따라 표면 실장이 가능하고 부품 자체의 소형화와 단위 체적당 높은 정전용량을 나타내는 특성에 기인하여, 캠코더, 하드디스크 드라이브 등의 각종 전자 제품의 수동 소자로 광범위하게 사용되고 있으며, 앞으로도 그 이용 범위는 더욱 확대될 것으로 기대되고 있다.Recently, multilayer ceramic capacitors can be surface-mounted according to the trend of miniaturization and weight reduction of various electronic devices, and due to the miniaturization of components and high capacitance per unit volume, the use of various electronic products such as camcorders and hard disk drives It is widely used as a passive device, and its use is expected to expand further.
이와같은 적층 세라믹 콘덴서의 내부 구조는 제1도에 나타나 있듯이 세라믹 유전체(1)의 내부에 교차적으로 내부 전극(2)이 형성되고, 그 내부 전극(2)의 일단이 외부로 노출된 세라믹 유전체(1)의 양 측면에 외부 전극(3)이 형성되도록 이루어 진다.As shown in FIG. 1, the internal structure of the multilayer ceramic capacitor has a ceramic dielectric in which an internal electrode 2 is formed alternately inside the ceramic dielectric 1, and one end of the internal electrode 2 is exposed to the outside. The external electrodes 3 are formed on both sides of (1).
이러한 내부 구조에 있어서 적층 세라믹 콘덴서를 사용할 때 중요한 선택 기준이 되는 정전 용량(electrostatic capacitance)은 유전체의 고유값인 유전율(Dielectric Constant), 내부 전극의 유효한 대향 면적과 적층수에 비례하고, 유전체층의 두께에는 반비례하게 된다. 정전 용량은 콘덴서에서 전하를 축적할 수 있는 능력을 나타내며 단위는 파라드(farad, F)이다.Electrostatic capacitance, which is an important selection criterion when using a multilayer ceramic capacitor in such an internal structure, is proportional to the dielectric constant which is an intrinsic value of the dielectric, the effective opposing area of the internal electrode and the number of stacked layers, and the thickness of the dielectric layer. Is inversely proportional. Capacitance refers to the ability to accumulate charge in a capacitor and is in units of farad (F).
따라서 최근의 제품의 소형화와 고용량화에 대응하기 위하여 규정된 크기의 적층 세라믹 콘덴서에 있어서 정전 용량을 높히기 위해서는 높은 유전율을 갖는 유전체의 사용과 유전체 두께를 얇게 할 필요성이 대두되고 있다.Therefore, in order to increase the capacitance of a multilayer ceramic capacitor of a prescribed size in order to cope with the recent miniaturization and high capacity of the product, the use of a dielectric having a high dielectric constant and the thickness of the dielectric have emerged.
특히 고신뢰성의 적층 세라믹 콘덴서를 제조하기 위해서는 소결 후 유전체의 결정립이 미세하고 치밀하며 높은 절연 저항과 높은 절연 파괴 전압을 갖게 되는 유전체의 사용이 필수 불가결한 요소가 된다.In particular, in order to manufacture a highly reliable multilayer ceramic capacitor, it is essential to use a dielectric having a fine and dense dielectric grain after sintering and having a high insulation resistance and a high dielectric breakdown voltage.
그러나 종래의 세라믹 유전체 조성물은 BaTiO3를 주성분으로 하여 CaZrO3,CaSnO3등이 첨가된 조성물을 사용하였으나 이러한 조성물은 비교적 높은 유전율을 갖는 반면에 결정립의 입경이 10∼20㎛ 정도로 크게 되어 절연 파괴 전압이 낮아지는 단점이 있으며 이로 인하여 고신뢰성의 제품을 제조하기 어려웠다.However, conventional dielectric ceramic composition as a main component and a BaTiO 3 CaZrO 3, CaSnO 3, etc. are used, but the additive composition this composition is largely a particle diameter of the crystal grains, while having a relatively high dielectric constant so 10~20㎛ breakdown voltage This has the disadvantage of being lowered, which makes it difficult to manufacture high reliability products.
또한 일본 공고특허 소 60-51202호, 소 59-86101호, 소60-51205호에서는 상술한 조성물의 단점인 절연 파괴 전압을 향상시키기 위하여 BaTiO3에 Sm2O3, CeO2, Dy2O3를 첨가하여 결정립의 입경을 2∼3㎛ 정도로 작게 함으로서 절연 파괴 전압을 향상시켰으나 절연 저항이 5 X 1013Ωcm 이하를 나타낼 뿐만 아니라, 온도 특성에 있어서도 Y5U 규격 특성을 만족시키지 못하고 Y5V 온도 특성(-30℃∼+85℃에서의 온도 범위에서 +25℃를 기준으로한 온도에 따른 유전율의 변화율이 +22∼-82% 이내)을 나타내었기 때문에 Y5U 특성의 고신뢰성 적층 세라믹 콘덴서의 제조에는 어려움이 있다.In addition, Japanese Patent Publication Nos. 60-51202, 59-86101, and 60-51205 disclose Sm 2 O 3 , CeO 2 , Dy 2 O 3 in BaTiO 3 in order to improve the dielectric breakdown voltage, which is a disadvantage of the above-mentioned composition. The dielectric breakdown voltage was improved by reducing the grain size of the crystal grains by 2 to 3㎛, but the insulation resistance was 5 X 10 13 Ωcm or less, and the Y5U temperature characteristics (- Difficult to change dielectric constant with temperature based on + 25 ℃ in the temperature range from 30 ℃ to + 85 ℃ within + 22 ~ -82%), making it difficult to manufacture high reliability multilayer ceramic capacitors with Y5U characteristics. have.
한편, 대한 민국 특허공보 제 94-5088호, 제 94-8692호에서는 BaTiO3에 CeO2와 Nd2O3같은 회토류 산화물과 TiO2등을 첨가하여 결정립의 입경을 2∼3㎛ 정도로 작게 하고 절연 저항도 1013Ωcm 이상으로 향상된 조성물을 제공하였으나, 유전율이 10,000 이하로 낮을 뿐만 아니라 온도 특성 또한 Y5U 특성을 만족하지 못하여 Y5U 특성의 고신뢰성 적층 세라믹 콘덴서의 제조에는 미흡한 점이 많았다.On the other hand, in Korean Patent Publication Nos. 94-5088 and 94-8692, the particle size of the crystal grains is reduced to about 2 to 3 μm by adding rare earth oxides such as CeO 2 and Nd 2 O 3 and TiO 2 to BaTiO 3 . The insulation resistance was improved to 10 13 Ωcm or more, but the dielectric constant was lower than 10,000 and the temperature characteristics also failed to satisfy the Y5U characteristics, which was insufficient for the production of high reliability multilayer ceramic capacitors having Y5U characteristics.
본 발명의 목적은 이러한 문제점들을 해결하여 결정립의 입경이 작고 치밀한 소결 상태를 나타내며, 높은 절연 저항과 높은 절연 파괴 전압을 갖는 동시에 Y5U 온도 특성규격을 만족하는 고유전율의 세라믹 유전체 조성물을 제공하는데 있다.SUMMARY OF THE INVENTION An object of the present invention is to solve the above problems and to provide a ceramic dielectric composition having a high dielectric constant having a small grain size and dense sintered state, having a high insulation resistance and a high dielectric breakdown voltage and satisfying the Y5U temperature characteristic specification.
이러한 목적을 달성하기 위하여 본 발명에서는 96.00∼97.10중량%의 BaTiO3를 주성분으로하고 여기에 1.60∼2.35중량%의 La2O3, 0.20∼0.95중량%의 TiO2, 0.40∼0.98중량%의 Nb 2 O5및 0.20∼0.35중량%의 MnO2를 첨가하여 세라믹 유전체 조성물을 구성하였다. 여기에서 중량%는 세라믹 조성 물 전체 중량을 기준으로 한 것이다.In order to achieve this object, in the present invention, 96.00 to 97.10% by weight of BaTiO 3 is the main component, and 1.60 to 2.35% by weight of La 2 O 3 , 0.20 to 0.95% by weight of TiO 2 , and 0.40 to 0.98% by weight of Nb. 2 0 5 and 0.20 to 0.35% by weight of MnO 2 were added to form a ceramic dielectric composition. The weight percentages here are based on the total weight of the ceramic composition.
본 발명의 상기 유전체 조성물 구성에 있어서, La2O3는 약 125℃에 위치하게 되는 BaTiO3의 큐리온도(Curie Temperature)를 상온으로 이동시키는 이동제(shifter)로서의 역활과 유전율을 향상시키며, TiO2s와 함께 소결 과정 중에서 액상을 형성하여 1280℃에서 소결을 가능하게 해주며, 결정립의 성장을 억제하는 효과를 나타낸다.In the dielectric composition of the present invention, La 2 O 3 improves the role and dielectric constant as a shifter for moving the Curie Temperature of BaTiO 3 located at about 125 ° C. to room temperature, and the TiO 2s Together with the formation of a liquid phase during the sintering process to enable the sintering at 1280 ℃, it has the effect of suppressing the growth of grains.
Nb2O5는 이동제로서의 역할과 온도에 따른 유전율의 편차를 작게 하는 데 효과적이며 또한 결정립의 성장을 억제하여 결정립을 작고 균일하게 성장시키게 한다Nb 2 O 5 is effective in reducing the variation of permittivity with temperature as a transfer agent and temperature, and also suppresses the growth of grains and makes grains grow small and uniform.
MnO2형태로 첨가하는 Mn 은 다양한 원자가를 갖을 수 있기 때문에 주성분인 BaTiO3와Mn added in the form of MnO 2 may have various valences, and therefore, BaTiO 3 and
BaTiO3와 반응하는 각 첨가물들의 전체적인 원자가를 보상하여 중성화 작용을 함으로서 유전 손실을 감소시키고 절연 저항을 증가시키는 역활을 하게 된다.By neutralizing by compensating the overall valence of each additive reacting with BaTiO 3 , it plays a role of reducing dielectric loss and increasing insulation resistance.
이상의 각 첨가물들의 조성물 범위에 있어서, La2O3와 TiO2는 상기 범위 이하에서는 소결성이 나빠져서 치밀한 소결체를 얻기 어려우며, 그 이상에서는 유전율은 증가하나 온도 특성을 규격치보다 벗어나게 한다.In the composition range of each of the above additives, La 2 O 3 and TiO 2 is difficult to obtain a dense sintered body due to poor sinterability below the above range, the dielectric constant increases but the temperature characteristic is beyond the standard value.
Nb2O5는 0.40중량% 이하에서는 결정립의 크기가 커지게 되어 절연 파괴 전압이 낮아지게 되며, 0.98중량% 이상으로 첨가하면 유전율이 낮아지게 된다.In the case of Nb 2 O 5 or less, 0.40 wt% or less, the grain size becomes large, resulting in low dielectric breakdown voltage.
또한 MnO2는 0.15중량% 이하에서는 손실값이 높아지며, 0.35중량% 이상에서는 상당한 유전율의 저하와 절연 저항이 오히려 감소하는 경향을 나타낸다.In addition, MnO 2 has a high loss value at 0.15% by weight or less, and a significant decrease in dielectric constant and insulation resistance at 0.35% by weight or more.
이상 상술한 본 발명에 따른 세라믹 유전체 조성물은 결정립의 입경이 작고 치밀한 소결 상태를 나타내고, 유전율이 8,000 이상으로 높으며 절연저항이 1013Ωcm 이상이고 절연 파괴 전압이 14KV/mm 이상인 동시에 Y5U 온도 특성 규격을 만족하게 된다.The ceramic dielectric composition according to the present invention described above has a small grain size, a dense sintered state, a high dielectric constant of 8,000 or more, an insulation resistance of 10 13 Ωcm or more, an insulation breakdown voltage of 14 KV / mm or more, and a Y5U temperature characteristic specification. You will be satisfied.
따라서 본 발명의 세라믹 유전체 조성물을 적층 세라믹 콘덴서의 제조에 이용하면 유전체 층의 두께를 얇게 할 수 있어 원가 절감의 효과가 지대할 뿐만 아니라, 소형화 및 고용량화에 대응할 수 있는 고신뢰성의 제품 생산이 가능해지는 효과가 있다.Therefore, when the ceramic dielectric composition of the present invention is used in the manufacture of a multilayer ceramic capacitor, the thickness of the dielectric layer can be reduced, resulting in a cost reduction effect and a high reliability product that can cope with miniaturization and high capacity. It works.
이하 실시예 및 비교예를 통하여 본 발명의 제조 방법 및 그 효과에 대하여 구체적으로 설명한다. 그러나 본 실시예 만으로 본 발명을 한정하는 것은 아니다.Hereinafter, the production method and effects thereof of the present invention will be described in detail through Examples and Comparative Examples. However, the present invention is not limited only to this embodiment.
[실시예 1∼6]EXAMPLES 1-6
출발 원료로 BaTiO3, La2O3, TiO2, Nb2O5및 MnO2를 표1에 기재된 조성물이 되도록 평량한 뒤, 불순물의 혼입을 방지하기 위하여 나일론 재질의 포트에서 지르코니아볼을 이용하여 탈 이온수와 함께 볼 밀링 방법으로 약 12시간 동안 습식, 혼합하여 분말상 혼합물을 제조한다.BaTiO 3 , La 2 O 3 , TiO 2 , Nb 2 O 5 and MnO 2 as starting materials were weighed out to the composition shown in Table 1, and then zirconia balls were used in a nylon port to prevent impurities from mixing. A powdery mixture was prepared by wet, mixing for about 12 hours by ball milling with deionized water.
균일하게 혼합된 상기 유전체 분말을 120℃ 정도에서 건조한 후, 여기에 폴리비닐 알콜5%수용액을 유전체 분말에 대하여 약 5중량% 첨가하여 조립화한 다음 일축 가압 성형기를 이용하여 직경 10mm의 원판형 성형체로 제작한다. 이때 성형체 두께는 1.0∼1.2mm 정도가 되게 하고 성형 밀도는 약 3.6g/㎤ 가 되게 한다.The uniformly mixed dielectric powder was dried at about 120 ° C., and then granulated by adding about 5% by weight of a 5% aqueous polyvinyl alcohol solution to the dielectric powder, and then using a uniaxial pressure molding machine to form a disk-shaped molded product having a diameter of 10 mm. Made with. In this case, the thickness of the molded body is about 1.0 to 1.2 mm and the molding density is about 3.6 g / cm 3.
성형된 시편은 안정호된 지르코니아 세터에 올려놓고 1280∼1320℃ 온도 범위에서 약 2시간 동안 공기분위기의 전기로에서 소결을 행한다.The molded specimen is placed on a stable zirconia setter and sintered in an electric furnace in an air atmosphere for about 2 hours in a temperature range of 1280 to 1320 ° C.
소결된 시편의 양면을 인쇄 도포 방법으로 은 전극을 7mm직경의 원형으로 도포, 건조한 후 800℃에서 10분 동안 열처리하게 되면 전기적 특성을 측정할 수 있는 최종 시편이 만들어지게 된다.Both sides of the sintered specimens were printed and coated with a silver electrode in a circular shape of 7 mm diameter, and then heat-treated at 800 ° C. for 10 minutes to form a final specimen for measuring electrical characteristics.
전기적 특성의 측정에 있어서, 유전율과 유전 손실은 미국 휴렛 팩커드사의 측정기(모델명 : HP 4278A Capacitance Meter)를 이용하여 25℃, 1KHz, 0.5V의 측정 조건으로 측정하고, 유전율의 온도 특성은 상기 측정기와 -30∼+85℃까지 온도 조절이 가능한 항온조를 조합하여 측정하였으며, 절연 저항은 휴렛 팩커드사의 저항측정기(모델명 : HP 4339A High Resistance Meter)를 이용하여 100V의 직류 전압을 1분 동안 인가한 후 측정하였다.In the measurement of the electrical properties, the dielectric constant and dielectric loss were measured at 25 ℃, 1KHz, 0.5V measurement conditions using a Hewlett-Packard company (Model: HP 4278A Capacitance Meter) of the United States, the temperature characteristic of the dielectric constant is The temperature resistance was measured by combining a thermostat with a temperature control from -30 to + 85 ° C. The insulation resistance was measured after applying a DC voltage of 100V for 1 minute using Hewlett Packard's resistance meter (Model: HP 4339A High Resistance Meter). It was.
또한 절연 파괴 전압은 자체 제작한 절연 파괴 전압 측정기를 이용하여 공기중에서 측정시 공기중으로 전류가 흐르는 것(over flash)을 방지하기 위하여 절연유 속에서 측정을 실시하였다.In addition, the dielectric breakdown voltage was measured in the insulating oil to prevent the over-flash current in the air when measured in the air using a self-made dielectric breakdown voltage measuring instrument.
이상과 같은 방법으로 측정한 전기적 특성의 결과치를 표2에 나타내었다.Table 2 shows the results of the electrical characteristics measured by the above method.
[비교예 1∼4][Comparative Examples 1 to 4]
BaTiO3, La2O3, TiO2, Nb2O5및 MnO2를 표1에 기재된 것과 같이 본 발명의 범주를 벗어난 양으로 혼합 제조한 것을 제외하고는 실시예 1∼6에 기재된 것과 동일한 방법으로 세라믹 유전체 조성물로 된 시편을 제작하였으며, 또한 동일한 방법으로 전기적 특성을 측정하여 그 결과치를 표2에 나타내었다.The same method as described in Examples 1 to 6 except that BaTiO 3 , La 2 O 3 , TiO 2 , Nb 2 O 5 and MnO 2 were mixed and prepared in an amount outside the scope of the present invention as shown in Table 1 A specimen made of a ceramic dielectric composition was prepared, and the electrical properties were measured in the same manner, and the results are shown in Table 2.
상술한 실시예 및 비교예로부터 알 수 있듯이 본 발명에 따른 세라믹 유전체 조성물은 결정립의 입경이 2∼3㎛로 작고 치밀한 소결 상태를 나타나고 있으며, 유전율은 8200∼9300 정도로 높고, 유전 손실은 0.7% 이하이며, 절연 저항은 1013Ωcm 이상이고 절연파괴 전압은 14KV/mm 이상인 동시에 Y5U 온도 특성 규격을 만족하고 있었다.As can be seen from the examples and comparative examples described above, the ceramic dielectric composition according to the present invention exhibits a compact and compact sintered state with a grain size of 2 to 3 μm, a dielectric constant of about 8200 to 9300, and a dielectric loss of 0.7% or less. The insulation resistance was 10 13 Ωcm or more, the dielectric breakdown voltage was 14KV / mm or more, and the Y5U temperature characteristic specification was satisfied.
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