JP2969007B2 - Non-reducing dielectric porcelain composition - Google Patents
Non-reducing dielectric porcelain compositionInfo
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- JP2969007B2 JP2969007B2 JP3023982A JP2398291A JP2969007B2 JP 2969007 B2 JP2969007 B2 JP 2969007B2 JP 3023982 A JP3023982 A JP 3023982A JP 2398291 A JP2398291 A JP 2398291A JP 2969007 B2 JP2969007 B2 JP 2969007B2
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- dielectric
- reducing dielectric
- composition
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- load life
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Description
【0001】[0001]
【産業上の利用分野】本発明は非還元性誘電体磁器組成
物に係り、特に高誘電率で、かつ誘電体損失が小さく高
温での電圧印加に対する寿命(高温負荷寿命)の良好な
高信頼性の誘電体磁器組成物に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a non-reducing dielectric porcelain composition, and more particularly to a high-reliability, high-reliability, low-dielectric-loss small-lifetime high-temperature life (high-temperature load life) with high voltage application. The present invention relates to a conductive dielectric ceramic composition.
【0002】[0002]
【従来の技術】通信機、電子計算機、テレビ受像機等の
電子機器に用いられるIC回路素子等に広く使用されて
いる積層セラミック・コンデンサは小型で大容量のもの
が好ましい。2. Description of the Related Art A multilayer ceramic capacitor widely used for an IC circuit element or the like used in electronic equipment such as a communication device, an electronic computer, and a television receiver preferably has a small size and a large capacity.
【0003】このような小型で大容量の積層セラミック
・コンデンサは、例えばBaTiO3 の如き、チタン酸
塩を主成分とした誘電体材料を使用することにより製造
することができる。[0003] Multilayer ceramic capacitor having a large capacity such a small, for example such as BaTiO 3, can be produced by using a dielectric material mainly composed of titanium salt.
【0004】従来、積層セラミック・コンデンサを製造
する方法は大別して印刷法及びシート法がある。Heretofore, methods for manufacturing a multilayer ceramic capacitor are roughly classified into a printing method and a sheet method.
【0005】前者は、誘電体のスラリーを作った後これ
を例えば、スクリーン印刷により所定形状に印刷し、乾
燥後その上に電極ペーストを印刷し、この電極ペースト
が乾燥した後に次の誘電体スラリーを印刷するという方
法を繰返すことにより、誘電体層と内部電極層を積層す
るものである。[0005] In the former method, after a dielectric slurry is prepared, it is printed in a predetermined shape by, for example, screen printing, dried, and then an electrode paste is printed thereon. Is repeated to laminate the dielectric layer and the internal electrode layer.
【0006】後者は、誘電体シートを例えばドクターブ
レード法で作成し、その上に電極ペーストを印刷し、こ
れを複数枚積み重ねて熱圧着し積層化する。In the latter case, a dielectric sheet is formed by, for example, a doctor blade method, an electrode paste is printed thereon, and a plurality of the sheets are stacked and thermocompression bonded.
【0007】このように適当な方法により積層化したも
のを空気中1250℃〜1400℃で焼成して焼結体を
作り、内部電極と導通する外部引出し電極をこれに焼付
けることにより積層セラミック・コンデンサを得てい
た。[0007] The laminated body is fired at a temperature of 1250 ° C to 1400 ° C in air to form a sintered body, and an external lead-out electrode, which is electrically connected to the internal electrode, is baked on the sintered body. I was getting a capacitor.
【0008】これらの方法ではコンデンサの電極となる
内部電極層と誘電体層を同時に焼成するため、内部電極
の材料としては誘電体が焼結する温度内で金属電極が形
成できること、空気中で上記の温度に加熱しても酸化し
たり、誘電体と反応しないことが必要である。In these methods, since the internal electrode layer serving as the electrode of the capacitor and the dielectric layer are simultaneously fired, the material of the internal electrode is that a metal electrode can be formed within the temperature at which the dielectric sinters. It is necessary that the material does not oxidize or react with the dielectric even when heated to the above temperature.
【0009】このため、これらの条件を満たすものとし
て白金やパラジウムまたはその合金などの貴金属が主に
使用されていた。For this reason, precious metals such as platinum, palladium and alloys thereof have been mainly used to satisfy these conditions.
【0010】しかしながらこれらの貴金属は非常に安定
ではあるが、高価であって積層セラミック・コンデンサ
のコストに占める割合が20〜50%程度と非常に大き
く、静電容量の大きいもの程積層数が増加する為、その
コストアップの最大の原因になっていた。However, although these noble metals are very stable, they are expensive and their share in the cost of the multilayer ceramic capacitor is very large, about 20 to 50%, and the number of layers increases as the capacitance increases. Therefore, it was the biggest cause of the cost increase.
【0011】この問題に対処するためにNi、Cu、F
e合金等の安価な卑金属を電極として使用する試みが従
来から行われている。To address this problem, Ni, Cu, F
Attempts have been made to use inexpensive base metals such as e-alloys as electrodes.
【0012】[0012]
【発明が解決しようとする課題】ところが、卑金属の電
極材料として例えばNiを使用すると、Niは空気中で
誘電体層と同時に焼成された時に酸化し、誘電体層内に
Niが拡散して、金属電極層が形成されず絶縁化してし
まう。このため電極としての機能を果さなくなる。However, when Ni is used as a base metal electrode material, for example, Ni is oxidized when baked in air at the same time as the dielectric layer, and Ni diffuses into the dielectric layer. The metal electrode layer is not formed, and becomes insulated. For this reason, the function as an electrode cannot be performed.
【0013】それ故Niの酸化を防止するために、中性
あるいは還元性雰囲気中で焼成することになるが、この
場合には誘電体材料が還元され、誘電体層の比抵抗が非
常に低いものとなってしまい、特に高温での電圧印加に
対する寿命が短かくなる。このためコンデンサ用誘電体
材料として使用できないという問題点を有する。Therefore, in order to prevent the oxidation of Ni, firing is performed in a neutral or reducing atmosphere. In this case, however, the dielectric material is reduced and the specific resistance of the dielectric layer is very low. In particular, the service life for applying a voltage at a high temperature is shortened. Therefore, it has a problem that it cannot be used as a dielectric material for capacitors.
【0014】従って本発明の目的は、積層セラミック・
コンデンサに用いる誘電体材料として、Ni等の卑金属
と同時に中性あるいは還元性雰囲気中で焼成しても還元
されない非還元性でありかつ誘電率が高く、誘電体損失
が小さく、絶縁抵抗が高く、高温での電圧印加に対する
寿命が長い誘電体磁器組成物を提供するものである。Accordingly, an object of the present invention is to provide a laminated ceramic
As a dielectric material used for the capacitor, it is non-reducing and not reduced even when fired in a neutral or reducing atmosphere simultaneously with a base metal such as Ni and has a high dielectric constant, a small dielectric loss, a high insulation resistance, An object of the present invention is to provide a dielectric porcelain composition having a long life to the application of a voltage at a high temperature.
【0015】[0015]
【課題を解決するための手段】前記の目的を達成するた
め、本発明者は鋭意研究の結果、チタン酸バリウムを主
成分とする多結晶固溶体からなり、該固溶体の組成式が {Ba(1-x)Cax}A・{Ti(1-y)Zry}B・O3 +aM1 +bM2 +cM3 で示される組成物において、M1 、M2 、M3 が M1 :Mn、Crの化合物の少なくとも1種 M2 :Siの化合物 M3 :Nb化合物 であり、かつx、y、A、B、a、b、cが 0≦x≦24(モル%) 8≦y≦22(モル%) 1.000 ≦A/B ≦1.040 0.05≦a≦1.0 0.05≦b≦1.0 0.05≦c≦0.5 (ただしa、b、cは酸化物換算での主成分に対する重
量%である)の範囲にある組成物である誘電体磁器組成
物が前記の問題点を解決することを見出した。Means for Solving the Problems In order to achieve the above object, the present inventors have conducted intensive studies and as a result, have made a polycrystalline solid solution containing barium titanate as a main component, and the composition formula of the solid solution is {Ba (1 -x) In a composition represented by Cax} Ay {Ti (1-y) Zry} B ・ O 3 + aM 1 + bM 2 + cM 3 , M 1 , M 2 and M 3 are compounds of M 1 : Mn and Cr At least one compound of M 2 : Si M 3 : Nb compound, and x, y, A, B, a, b, c are 0 ≦ x ≦ 24 (mol%) 8 ≦ y ≦ 22 (mol%) 1.000 ≦ A / B ≦ 1.040 0.05 ≦ a ≦ 1.0 0.05 ≦ b ≦ 1.0 0.05 ≦ c ≦ 0.5 (where a, b, and c are weight% with respect to the main component in terms of oxide) Has been found to solve the above-mentioned problems.
【0016】[0016]
【実施例】出発原料として、BaCO3 、TiO2 、Z
rO2 、CaCO3 、MrOまたはCr2 O3 、SiO
2 、Nb2 O5 を用い、焼成後の組成がそれぞれ表1、
表2の如くになるように秤量し混合する。EXAMPLES As starting materials, BaCO 3 , TiO 2 , Z
rO 2 , CaCO 3 , MrO or Cr 2 O 3 , SiO
2 and Nb 2 O 5 , the compositions after firing were as shown in Table 1,
Weigh and mix as shown in Table 2.
【0017】その後脱水乾燥させ1050℃〜1240
℃で2時間仮焼成する。この仮焼成体を微粉砕し、脱水
・乾燥して粉末とする。After that, it is dehydrated and dried at 1050 ° C. to 1240
Temporarily bake at 2 ° C. for 2 hours. The calcined body is finely pulverized, dehydrated and dried to obtain a powder.
【0018】得られた粉末に適当量の有機バインダを加
え、厚さ20μmと厚さ100μmのシートを得る。An appropriate amount of an organic binder is added to the obtained powder to obtain a sheet having a thickness of 20 μm and a thickness of 100 μm.
【0019】次にまず厚さ20μmのシートの両面に、
Ni粉末をビヒクル中に分散させた電極ペーストをスク
リーン印刷により塗布し電極とする。さらにこの上下両
面に厚さ100μmのシートを熱圧着により圧着する。
この100μmのシートは焼成後のハンドリングを考慮
し、素体強度を上げるためのものであり、電気的特性に
は何等影響を及ぼさない。Next, first, on both sides of a sheet having a thickness of 20 μm,
An electrode paste in which Ni powder is dispersed in a vehicle is applied by screen printing to form an electrode. Further, a sheet having a thickness of 100 μm is pressed on both upper and lower surfaces by thermocompression.
The sheet having a thickness of 100 μm is provided to increase the strength of the element body in consideration of handling after firing, and does not affect the electrical characteristics at all.
【0020】熱圧着したシートを3.9 ×1.9mm の寸法に
切断しこれをジルコニア板の上にのせ、匣鉢の中に入れ
て500℃まで空気中で加熱し有機バインダを燃焼さ
せ、その後N2 中またはN2 +H2 中で1300℃〜1
400℃で2時間焼成する。The thermocompression-bonded sheet is cut to a size of 3.9 × 1.9 mm, placed on a zirconia plate, placed in a sagger, heated to 500 ° C. in air to burn the organic binder, and then N 2 1300 ° C to 1 in water or N 2 + H 2
Bake at 400 ° C. for 2 hours.
【0021】焼成後の素地寸法は約3.2 ×1.6mm とな
る。The size of the green body after firing is about 3.2 × 1.6 mm.
【0022】その後空気+N2 中で800℃〜1100
℃で2時間アニーリングしてサンプルを得る。After that, 800 ° C. to 1100 in air + N 2
Anneal at 2 ° C. for 2 hours to obtain a sample.
【0023】このサンプルの端部にIn−Gaを塗布し
外部引出し電極として、電気的特性を測定した。In-Ga was applied to the end of the sample, and its electrical characteristics were measured as an external lead electrode.
【0024】電気的特性は、比誘電率(ε)、誘電体損
失(tanδ、%)、絶縁抵抗(IR、Ω、25VD
C、60秒値)、高温負荷寿命(200℃で100VD
Cを印加し、6mA以上電流が流れるまでの時間HR)
を測定する。Electrical characteristics include relative permittivity (ε), dielectric loss (tan δ,%), insulation resistance (IR, Ω, 25 VD
C, 60 seconds value), high temperature load life (100VD at 200 ° C)
Time HR until C is applied and a current of 6 mA or more flows.
Is measured.
【0025】その結果を表1、表2に示す。なお、表
1、表2において*印の付与されているものは、本発明
の範囲外のものであり、本発明の実施例のものと比較の
ために提示する。The results are shown in Tables 1 and 2. In Tables 1 and 2, those marked with an asterisk are out of the scope of the present invention and are presented for comparison with those of the examples of the present invention.
【0026】[0026]
【表1】 [Table 1]
【0027】[0027]
【表2】 [Table 2]
【0028】表1、表2より明らかなように、本発明の
ものは比誘電率が7000以上と特に高く、tanδは
0.8 %〜4.5%と小さな値を示しており、かつ高温での
負荷寿命が60時間〜120時間と長いものである。ま
た常温における絶縁抵抗IRも高い値を示している。As is clear from Tables 1 and 2, the material of the present invention has a particularly high relative dielectric constant of 7000 or more, and the tan δ is
It shows a small value of 0.8% to 4.5%, and has a long load life at a high temperature of 60 hours to 120 hours. Further, the insulation resistance IR at room temperature also shows a high value.
【0029】次に本発明の各組織範囲の数値限定の理由
について説明する。Next, the reason for limiting the numerical value of each tissue range according to the present invention will be described.
【0030】まず、xが24より大きくなると、比誘電
率εs が低下し、高温負荷寿命も非常に短かくなる(例
えば表2の試料No. 20参照)。First, when x is larger than 24, the relative dielectric constant εs is reduced, and the high-temperature load life is also very short (for example, see Sample No. 20 in Table 2).
【0031】yが8より小さくなると、比誘電率εs が
低下し、誘電体損失tanδも大きくなる(例えば表2
の試料No. 28参照)。When y is smaller than 8, the relative permittivity εs decreases and the dielectric loss tan δ also increases (for example, see Table 2).
Sample No. 28).
【0032】yが22より大きくなると、比誘電率εs
が低下する(例えば表2の試料No.24参照)。When y exceeds 22, the relative dielectric constant εs
(For example, see Sample No. 24 in Table 2).
【0033】また、A/B が1.000 より小さくなると、誘
電体が還元し、絶縁抵抗IRが低くなり、高温負荷寿命
が短くなる(例えば表1の試料No. 15参照)。On the other hand, when A / B is smaller than 1.000, the dielectric material is reduced, the insulation resistance IR is reduced, and the high temperature load life is shortened (for example, see Sample No. 15 in Table 1).
【0034】A/B が1.040 より大きくなると、焼結不足
となり、比誘電率εs が低下し、誘電体損失tanδが
大きく絶縁抵抗IRが低下し高温負荷寿命も短くなる
(例えば表2の試料No. 19参照)。When A / B exceeds 1.040, sintering becomes insufficient, the relative dielectric constant εs decreases, the dielectric loss tanδ increases, the insulation resistance IR decreases, and the high-temperature load life decreases (for example, sample No. 2 in Table 2). 19).
【0035】さらにaが0.05より小さくなると、誘電体
損失tanδが大きく高温負荷寿命が短かくなる(例え
ば表1の試料No. 6参照)。Further, when a is smaller than 0.05, the dielectric loss tan δ is large and the high-temperature load life is short (for example, see Sample No. 6 in Table 1).
【0036】aが1.0 より大きくなると、比誘電率εs
が低下し、高温負荷寿命も短かくなる(例えば表1の試
料No. 10参照)。When a is larger than 1.0, the relative dielectric constant εs
And the high-temperature load life is shortened (for example, see Sample No. 10 in Table 1).
【0037】bが0.05より小さくなると、比誘電率εs
が低下し、高温負荷寿命も短くなる(例えば表1の試料
No. 1参照)。When b is smaller than 0.05, the relative dielectric constant εs
And the high temperature load life is shortened (for example, the sample in Table 1)
No. 1).
【0038】bが1.0 より大きくなると、比誘電率εs
が低下し、高温負荷寿命も短かくなる(例えば表1の試
料No. 5参照)。When b exceeds 1.0, the relative dielectric constant εs
And the high-temperature load life is shortened (for example, see Sample No. 5 in Table 1).
【0039】cが0.05より小さくなると、高温負荷寿命
が短かくなる(例えば表1の試料No. 11参照)。When c is smaller than 0.05, the high temperature load life is shortened (for example, see Sample No. 11 in Table 1).
【0040】cが0.5 より大きくなると、誘電体が還元
し、絶縁抵抗IRが低くなり、高温負荷寿命が短くなる
(例えば表1の試料No. 14参照)。When c exceeds 0.5, the dielectric material is reduced, the insulation resistance IR is reduced, and the high-temperature load life is shortened (for example, see Sample No. 14 in Table 1).
【0041】要約すれば、M1 、M2 、M3 を前記の如
く選択し、またa、b、cをこれまた前記の如く選択す
ることにより高温負荷寿命を改善することができる。In summary, selecting M 1 , M 2 , and M 3 as described above and selecting a, b, and c as described above also improves the high temperature load life.
【0042】またxが前記の値より多すぎると比誘電率
εs が低下し、またyが前記の値より少ないとキュリー
点が高温側にあり常温での比誘電率εs が低下し、誘電
体損失tanδも大きい。yが前記の値より多すぎると
キュリー点が低温側に移動するため比誘電率εsが低下
する。If x is more than the above value, the relative permittivity εs decreases. If y is less than the above value, the Curie point is on the high temperature side, and the relative permittivity εs at room temperature decreases. The loss tan δ is also large. If y is more than the above value, the Curie point moves to the low temperature side, so that the relative dielectric constant εs decreases.
【0043】そしてA/B が1.000 より少ないと、つまり
Tirichになると還元に弱くなり、絶縁抵抗IRの
低下を招くことになる、またA/B が1.040 より多いと焼
結不足となる。When A / B is less than 1.000, that is, when Tirich is reached, reduction becomes weak and the insulation resistance IR is reduced. When A / B is more than 1.040, sintering becomes insufficient.
【0044】[0044]
【発明の効果】本発明によれば、中性または還元性雰囲
気中で焼成しても比誘電率が高く、誘電体損失が小さく
かつ高温負荷寿命も長く、絶縁抵抗の高い高信頼性の誘
電体磁器組成物を得ることができる。According to the present invention, a highly reliable dielectric material having a high relative dielectric constant, a small dielectric loss, a long high-temperature load life and a high insulation resistance even when fired in a neutral or reducing atmosphere. A body porcelain composition can be obtained.
【0045】これにより、Ni等の卑金属を内部電極と
する積層セラミック・コンデンサを製造することができ
るようになる。Thus, a multilayer ceramic capacitor using a base metal such as Ni as an internal electrode can be manufactured.
Claims (3)
固溶体からなり、該固溶体の組成式が {Ba(1-x)Cax}A・{Ti(1-y)Zry}B・O3 +aM1 +bM2 +cM3 で示される組成式において、M1 、M2 、M3 が M1 :Mn、Crの化合物の少なくとも1種、 M2 :Siの化合物、 M3 :Nb化合物 であり、かつa、b、cが酸化物換算で 0.05≦a≦1.0 0.05≦b≦1.0 0.05≦c≦0.5 (ただしa、b、cは前記主成分に対する重量%であ
る)の範囲に添加含有したことを特徴とする非還元性誘
電体磁器組成物。1. A polycrystalline solid solution containing barium titanate as a main component, wherein the composition formula of the solid solution is {Ba (1-x) Cax} A. {Ti (1-y) Zry} B.O 3 + aM. In the composition formula represented by 1 + bM 2 + cM 3 , M 1 , M 2 , and M 3 are at least one compound of M 1 : Mn and Cr, a compound of M 2 : Si, a compound of M 3 : Nb, and a, b, and c are added and contained in the range of 0.05 ≦ a ≦ 1.0 0.05 ≦ b ≦ 1.0 0.05 ≦ c ≦ 0.5 (where a, b, and c are weight% with respect to the main component) in terms of oxide. A non-reducing dielectric porcelain composition.
化学式を {Ba(1-x)Cax}・{Ti(1-y)Zry}・O3 とする時、x、yが 0≦x≦0.24 0.08≦y≦0.22 の範囲にあることを特徴とする請求項1記載の非還元性
誘電体磁器組成物。2. When the chemical formula of the polycrystalline solid solution of barium titanate is {Ba (1-x) Cax}. {Ti (1-y) Zry} .O 3 , x and y are 0 ≦ x ≦ 2. The non-reducing dielectric ceramic composition according to claim 1, wherein the value is in the range of 0.24 0.08 ≦ y ≦ 0.22.
組成式を {Ba(1-x)Cax}A・{Ti(1-y)Zry}B・O3 とする
時、 1.000 ≦A/B ≦1.040 の範囲にあることを特徴とする請求項1または請求項2
記載の非還元性誘電体磁器組成物。3. When the composition formula of the polycrystalline solid solution of barium titanate is {Ba (1-x) Cax} A · {Ti (1-y) Zry} B · O 3 , 1.000 ≦ A / B 3. The method according to claim 1, wherein the value is in the range of .ltoreq.1.040.
A non-reducing dielectric ceramic composition as described in the above.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP3023982A JP2969007B2 (en) | 1991-01-24 | 1991-01-24 | Non-reducing dielectric porcelain composition |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
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JP3023982A JP2969007B2 (en) | 1991-01-24 | 1991-01-24 | Non-reducing dielectric porcelain composition |
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JPH04367558A JPH04367558A (en) | 1992-12-18 |
JP2969007B2 true JP2969007B2 (en) | 1999-11-02 |
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JP3023982A Expired - Lifetime JP2969007B2 (en) | 1991-01-24 | 1991-01-24 | Non-reducing dielectric porcelain composition |
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JP (1) | JP2969007B2 (en) |
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JPH04367558A (en) | 1992-12-18 |
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