JPH0212889B2 - - Google Patents
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- Publication number
- JPH0212889B2 JPH0212889B2 JP61314623A JP31462386A JPH0212889B2 JP H0212889 B2 JPH0212889 B2 JP H0212889B2 JP 61314623 A JP61314623 A JP 61314623A JP 31462386 A JP31462386 A JP 31462386A JP H0212889 B2 JPH0212889 B2 JP H0212889B2
- Authority
- JP
- Japan
- Prior art keywords
- dielectric constant
- pbo
- composition
- zro
- present
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
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- 239000000203 mixture Substances 0.000 claims description 33
- 239000000919 ceramic Substances 0.000 claims description 12
- 229910021193 La 2 O 3 Inorganic materials 0.000 claims description 5
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 5
- HTUMBQDCCIXGCV-UHFFFAOYSA-N lead oxide Chemical compound [O-2].[Pb+2] HTUMBQDCCIXGCV-UHFFFAOYSA-N 0.000 description 8
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000003990 capacitor Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Inorganic materials [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 229910001923 silver oxide Inorganic materials 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 239000003112 inhibitor Substances 0.000 description 2
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052573 porcelain Inorganic materials 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 description 1
- 229910004774 CaSnO3 Inorganic materials 0.000 description 1
- 229910002971 CaTiO3 Inorganic materials 0.000 description 1
- 229910002976 CaZrO3 Inorganic materials 0.000 description 1
- 229910020203 CeO Inorganic materials 0.000 description 1
- -1 La2BO3 Inorganic materials 0.000 description 1
- 229910017676 MgTiO3 Inorganic materials 0.000 description 1
- 229910003781 PbTiO3 Inorganic materials 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910002367 SrTiO Inorganic materials 0.000 description 1
- 229910002370 SrTiO3 Inorganic materials 0.000 description 1
- 229910010252 TiO3 Inorganic materials 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229910000464 lead oxide Inorganic materials 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N zinc oxide Inorganic materials [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Landscapes
- Compositions Of Oxide Ceramics (AREA)
- Inorganic Insulating Materials (AREA)
Description
［産業上の利用分野］
本発明は高誘電率磁器組成物に係り、特に誘電
率の温度特性及びバイアス特性に優れることか
ら、例えば高圧コンデンサ等の誘電体材料として
好適な高誘電率磁器組成物に関する。
［従来の技術］
従来、高誘電率磁器組成物としては、チタン酸
バリウム（BaTiO3）を主体とする組成物が一般
に使用されている。即ち、BaTiO3を基体とし、
これにキユリー点を室温付近に移動させるシフタ
ー剤と容量温度特性を改善するデプレツサ剤、さ
らに焼結促進剤、還元防止剤などを加えた組成と
するのが一般的である。
シフター剤としては、BaSnO3、BaZrO3、
CaZrO3、CaSnO3、SrTiO3、PbTiO3、La2BO3、
CeO2などが用いられ、デプレツサ剤としては、
CaTiO3、MgTiO3、Bi2（SnO3）3、Bi2（TiO3）3、
NiSnO3、MgZrO3、MgSnO3などが用いられて
いる。また焼結促進剤としては、Al2O3、SiO2、
ZnO、CeO2、B2O3、Nb2O5、WO3などが用いら
れ、還元防止剤としては、MnO2、FeO3、CuO
などが用いられている。
［発明が解決しようとする問題点］
しかしながら、BaTiO3を主成分とする高誘電
率磁器組成物は、直流バイアス下での誘電率が著
しく低下するため高圧コンデンサ用磁器組成物と
しては適当でなかつた。
一方、バイアス特性の良好な組成物として、
SrTiO3にPbTiO3、MgTiO3、Bi2O3、TiO3等を
添加した材料系が提案されているが、一般にこれ
らの系は誘電率が小さいという欠点があり、バイ
アス特性がよいにもかかわらず、直流バイアス下
での誘電率が大きい組成は極めて限られた範囲に
限定されているため、実用性の低いものであつ
た。
［問題点を解決するための手段及び作用］
本発明のうち第１の発明に係る高誘電率磁器組
成物は、下記一般式で示される組成を有する。
（１−ａ−ｂ）PbO・ａ／２La2O3・bSrO・
（１−ｃ）ZrO2・cTiO2
［式中、0.08≦ａ≦0.16
0.04≦ｂ≦0.30
0.20≦ｃ≦0.35］
また、本発明のうち第２の発明に係る高誘電率
磁器組成物は、上記高誘電率磁器組成物におい
て、PbO＋LaO3/2＋SrOのモル数の４モル％以下
をAgO1/2で置換したものである。
以下、本発明についてその作用とともに更に詳
細に説明する。
PbO、La2O3、ZrO2、TiO2よりなるペロブス
カイト型化合物（PLZT）は、その組成比によ
り、強誘電相、反強誘電相、常誘電相をとるが、
その中で反強誘電相は、バイアス特性がよいこと
が知られている。しかしながら、誘電率及び誘電
率温度特性の点でいまだ満足できるものではなか
つた。
本発明者らは、PbO、La2O3、ZrO2、TiO2よ
りなるペロブスカイト型化合物においてPbをSr
で置換することにより、バイアス特性を悪化させ
ることなく誘電率及び誘電率温度特性が改善され
ること、また、Srを含むPLZTに更にAgを固溶
させることにより誘電率温度特性がいつそう改善
され、バイアス特性も良くなることを見出し、本
発明を完成させたものである。
前記一般式中、ａが0.08未満であると得られる
組成物の誘電率が小さくなり、誘電率温度特性も
悪化する。また、ａが0.16を超えると、誘電率が
小さくなる。このため、ａは0.08以上0.16以下の
範囲とする。
また、ｂが0.04未満でも、0.30を超えても、得
られる組成物は、誘電率が小さくなつたり、誘電
率温度特性が悪化したりする。このため、ｂは
0.04以上0.30以下の範囲とする。
ｃが0.20未満では、得られる組成物の誘電率が
小さくなり、ｃが0.35を超えると誘電率温度特性
が悪化する。このため、ｃは0.03以上0.35以下の
範囲とする。
本発明の組成物中に酸化銀が含まれる場合に
は、得られる組成物の誘電率温度特性及びバイア
ス特性が更に向上するという効果がある。
しかるに、酸化銀をAgO1/2と表わした時、
AgO1/2の割合がPbO＋LaO3/2＋SrOのモル数の４
モル％を超える場合には、得られる組成物の誘電
率を小さくする。このため、AgO1/2を添加する
場合、ｄは0.04以下とする。
このような本発明の高誘電率磁器組成物を製造
するには、例えば、酸化鉛、酸化ランタン、酸化
ジルコニウム、酸化チタン、酸化ストロンチウ
ム、酸化銀等の粉末を、所定の割合となるよう秤
量し、湿式ボールミル等を用いて十分に混合す
る。次にこの混合物を乾燥した後、必要に応じ、
900〜1000℃の範囲で数時間程度仮焼する。この
仮焼は必ずしも行う必要はないが、これを行うこ
とにより粒子がより均一化され、誘電特性が向上
する傾向がある。仮焼を行つた場合には、仮焼物
を更に湿式ボールミル等で粉砕し、乾燥後、ポリ
ビニルアルコールなどの適当な有機バインダを加
えて、顆粒を作り、これを所定の形状にプレス成
形した後、焼成を行う。この焼成は、1200〜1300
℃の温度範囲で0.5〜数時間程度行う。（勿論、こ
れらの製造条件は最も好適な数値であつて、本発
明の磁器組成物は上記以外の条件もしくは方法に
よつて製造されても良い。）
本発明で限定される組成比の高誘電率磁器組成
物は、バイアス特性及び誘電率温度特性に優れて
いる。従つて、このような組成物は例えば小型大
容量の高圧コンデンサ材料として好適である。
［実施例］
以下に本発明を実施例を挙げて更に具体的に説
明するが、本発明はその要旨を超えない限り、以
下の実施例に限定されるものではない。
実施例 １
原料としててPbO、La2O3、ZrO2、TiO2、
SrCO3、Ag2Oを使用し、これらを第１表に示す
配合比となるように秤量し、ボールミル中で20時
間湿式混合した。次いで、混合物を脱水、乾燥
後、900〜1000℃で２時間保持して仮焼し、再び
ボールミル中で20時間湿式粉砕した後、脱水、乾
燥した。
得られた粉末に、有機バインダを加え、成形圧
力3ton／cm2で、直径16mm、厚さ0.8mmの円板に加
圧成形した。この成形物をマグネシア磁器容器に
入れて、PbO雰囲気で第１表に示す如く、1200〜
1300℃の温度で１時間焼成した。
得られた円板形状の誘電体の両面に、銀電極を
700〜800℃で焼付けて、その電気的特性を調べ
た。
結果を第１表に示す。
なお、誘電率及び誘電損失は、25℃において、
1KHz、1Vrmsにて測定し、比抵抗は印加電圧
100Vにて、１分値の測定により求めた。また、
温度特性は、25℃の誘電率に対する−25℃〜85℃
の温度範囲における変化率により示されている。
バイアス特性は、直流バイアスゼロにおける誘電
率に対する3KV／mm直流バイアス下での誘電率
の変化率により示されている。
第１表からも明らかなように、本発明の範囲内
の組成物は、いずれも、誘電率が大きいにもかか
わらず、誘電率の温度変化が著しく小さく、バイ
アス特性も優れている。また、Ag2Oは誘電率温
度特性及びバイアス特性を向上させる効果があ
る。
[Industrial Application Field] The present invention relates to a high-permittivity ceramic composition, and in particular, it is suitable as a dielectric material for high-voltage capacitors, etc., because it has excellent dielectric constant temperature characteristics and bias characteristics. Regarding. [Prior Art] Conventionally, compositions containing barium titanate (BaTiO 3 ) as a main component have generally been used as high dielectric constant ceramic compositions. That is, BaTiO 3 is used as a base,
The composition generally includes a shifter agent that moves the Curie point to near room temperature, a depressor agent that improves the capacity temperature characteristics, and further contains a sintering accelerator, a reduction inhibitor, and the like. As the shifter agent, BaSnO 3 , BaZrO 3 ,
CaZrO3 , CaSnO3 , SrTiO3 , PbTiO3 , La2BO3 ,
CeO 2 etc. are used as depressor agents.
CaTiO3 , MgTiO3 , Bi2 ( SnO3 ) 3 , Bi2 ( TiO3 ) 3 ,
NiSnO 3 , MgZrO 3 , MgSnO 3 and the like are used. In addition, as a sintering accelerator, Al 2 O 3 , SiO 2 ,
ZnO, CeO 2 , B 2 O 3 , Nb 2 O 5 , WO 3 , etc. are used, and as reduction inhibitors, MnO 2 , FeO 3 , CuO
etc. are used. [Problems to be Solved by the Invention] However, high permittivity ceramic compositions containing BaTiO 3 as a main component are not suitable as ceramic compositions for high voltage capacitors because the dielectric constant under direct current bias decreases significantly. Ta. On the other hand, as a composition with good bias characteristics,
Material systems in which PbTiO 3 , MgTiO 3 , Bi 2 O 3 , TiO 3 , etc. are added to SrTiO 3 have been proposed, but these systems generally have the disadvantage of a small dielectric constant, and although they have good bias characteristics, First, compositions with a high dielectric constant under direct current bias are limited to an extremely limited range, and are therefore impractical. [Means and effects for solving the problems] The high dielectric constant ceramic composition according to the first aspect of the present invention has a composition represented by the following general formula. (1-a-b) PbO・a/2La 2 O 3・bSrO・
(1-c) ZrO 2 ·cTiO 2 [wherein, 0.08≦a≦0.16 0.04≦b≦0.30 0.20≦c≦0.35] Furthermore, the high dielectric constant ceramic composition according to the second invention of the present invention is In the above-mentioned high dielectric constant ceramic composition, 4 mol % or less of the number of moles of PbO + LaO 3/2 + SrO is replaced with AgO 1/2 . Hereinafter, the present invention will be explained in more detail along with its effects. A perovskite compound (PLZT) consisting of PbO, La 2 O 3 , ZrO 2 , and TiO 2 takes a ferroelectric phase, an antiferroelectric phase, or a paraelectric phase depending on its composition ratio.
Among them, the antiferroelectric phase is known to have good bias characteristics. However, the dielectric constant and the dielectric constant-temperature characteristics are still not satisfactory. The present inventors replaced Pb with Sr in a perovskite compound consisting of PbO, La 2 O 3 , ZrO 2 , and TiO 2 .
The dielectric constant and dielectric constant-temperature characteristics are improved without deteriorating the bias characteristics, and the dielectric constant-temperature characteristics are improved by dissolving Ag in Sr-containing PLZT. They discovered that the bias characteristics were also improved, and completed the present invention. In the general formula, if a is less than 0.08, the dielectric constant of the resulting composition will be low, and the dielectric constant temperature characteristics will also deteriorate. Moreover, when a exceeds 0.16, the dielectric constant becomes small. Therefore, a should be in the range of 0.08 or more and 0.16 or less. Furthermore, even if b is less than 0.04 or more than 0.30, the resulting composition will have a low dielectric constant or deteriorated dielectric constant temperature characteristics. Therefore, b is
The range shall be 0.04 or more and 0.30 or less. When c is less than 0.20, the dielectric constant of the resulting composition becomes small, and when c exceeds 0.35, the dielectric constant-temperature characteristics deteriorate. Therefore, c is in the range of 0.03 or more and 0.35 or less. When silver oxide is contained in the composition of the present invention, there is an effect that the dielectric constant temperature characteristics and bias characteristics of the resulting composition are further improved. However, when silver oxide is expressed as AgO 1/2 ,
The ratio of AgO 1/2 is 4 of the number of moles of PbO + LaO 3/2 + SrO
If it exceeds mol%, the dielectric constant of the resulting composition is reduced. Therefore, when adding AgO 1/2 , d should be 0.04 or less. In order to manufacture such a high dielectric constant ceramic composition of the present invention, for example, powders of lead oxide, lanthanum oxide, zirconium oxide, titanium oxide, strontium oxide, silver oxide, etc. are weighed to a predetermined ratio. Mix thoroughly using a wet ball mill or the like. Then, after drying this mixture, if necessary,
Calcinate at a temperature of 900 to 1000℃ for several hours. Although it is not necessary to perform this calcination, it tends to make the particles more uniform and improve the dielectric properties. In the case of calcining, the calcined product is further pulverized using a wet ball mill, etc. After drying, a suitable organic binder such as polyvinyl alcohol is added to form granules, which are then press-molded into a predetermined shape. Perform firing. This firing is 1200~1300
It is carried out for about 0.5 to several hours at a temperature range of ℃. (Of course, these manufacturing conditions are the most suitable values, and the ceramic composition of the present invention may be manufactured using conditions or methods other than those described above.) The ceramic composition has excellent bias characteristics and dielectric constant temperature characteristics. Therefore, such a composition is suitable, for example, as a material for a small-sized, large-capacity, high-voltage capacitor. [Examples] The present invention will be described in more detail below with reference to Examples, but the present invention is not limited to the following Examples unless it exceeds the gist thereof. Example 1 Raw materials include PbO, La 2 O 3 , ZrO 2 , TiO 2 ,
SrCO 3 and Ag 2 O were weighed to have the compounding ratio shown in Table 1, and wet mixed in a ball mill for 20 hours. Next, the mixture was dehydrated and dried, then calcined by holding at 900 to 1000°C for 2 hours, wet milled again in a ball mill for 20 hours, and then dehydrated and dried. An organic binder was added to the obtained powder, and the mixture was pressure-molded into a disk having a diameter of 16 mm and a thickness of 0.8 mm at a molding pressure of 3 tons/cm 2 . This molded product was placed in a magnesia porcelain container and heated in a PbO atmosphere for 1,200~
It was baked at a temperature of 1300°C for 1 hour. Silver electrodes were placed on both sides of the resulting disk-shaped dielectric.
It was baked at 700-800℃ and its electrical properties were investigated. The results are shown in Table 1. Note that the dielectric constant and dielectric loss are as follows at 25℃:
Measured at 1KHz, 1Vrms, specific resistance is the applied voltage
It was determined by measuring the value for 1 minute at 100V. Also,
Temperature characteristics are -25℃ to 85℃ for dielectric constant of 25℃
It is shown by the rate of change over a temperature range of .
The bias characteristics are shown by the rate of change of the dielectric constant under a 3 KV/mm DC bias relative to the dielectric constant at zero DC bias. As is clear from Table 1, all of the compositions within the scope of the present invention exhibit extremely small temperature changes in dielectric constant and have excellent bias characteristics, despite having a large dielectric constant. Furthermore, Ag 2 O has the effect of improving dielectric constant temperature characteristics and bias characteristics.
【表】【table】
【表】
［発明の効果］
以上詳述した通り、本発明の磁器組成物は、誘
電率が極めて大きく、しかも誘電率の温度特性、
バイアス特性に優れる。このため、本発明の高誘
電率は、小型大容量の高圧コンデンサ材料等とし
て極めて有用である。[Table] [Effects of the Invention] As detailed above, the porcelain composition of the present invention has an extremely high dielectric constant, and the temperature characteristics of the dielectric constant,
Excellent bias characteristics. Therefore, the high dielectric constant of the present invention is extremely useful as a small-sized, large-capacity, high-voltage capacitor material, etc.
Claims (1)
り、下記一般式で示される組成を有することを特
徴とする高誘電率磁器組成物。 （１−ａ−ｂ）PbO・ａ／２La2O3・bSrO・
（１−ｃ）ZrO2・cTiO2 ［式中、0.08≦ａ≦0.16 0.04≦ｂ≦0.30 0.20≦ｃ≦0.35］ ２ PbO、La2O3、SrO、ZrO2、TiO2及びAg2O
よりなり、下記一般式で示される組成を有するこ
とを特徴とする高誘電率磁器組成物。 （１−ａ−ｂ−ｄ）PbO・ａ／２La2O3・bSrO・ｄ
／２Ag2O・（１−ｃ）ZrO2・cTiO2 ［式中、0.08≦ａ≦0.16 0.04≦ｂ≦0.30 0.20≦ｃ≦0.35 ０＜ｄ≦0.04］[Scope of Claims] 1. A high dielectric constant ceramic composition comprising PbO, La 2 O 3 , SrO, ZrO 2 and TiO 2 and having a composition represented by the following general formula. (1-a-b) PbO・a/2La 2 O 3・bSrO・
(1-c) ZrO 2・cTiO 2 [In the formula, 0.08≦a≦0.16 0.04≦b≦0.30 0.20≦c≦0.35] 2 PbO, La 2 O 3 , SrO, ZrO 2 , TiO 2 and Ag 2 O
A high dielectric constant ceramic composition characterized by having a composition represented by the following general formula. (1-a-b-d) PbO・a/2La 2 O 3・bSrO・d
/2Ag 2 O・(1-c)ZrO 2・cTiO 2 [In the formula, 0.08≦a≦0.16 0.04≦b≦0.30 0.20≦c≦0.35 0<d≦0.04]
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61314623A JPS63162571A (en) | 1986-12-25 | 1986-12-25 | High permittivity ceramic composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61314623A JPS63162571A (en) | 1986-12-25 | 1986-12-25 | High permittivity ceramic composition |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63162571A JPS63162571A (en) | 1988-07-06 |
| JPH0212889B2 true JPH0212889B2 (en) | 1990-03-29 |
Family
ID=18055534
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61314623A Granted JPS63162571A (en) | 1986-12-25 | 1986-12-25 | High permittivity ceramic composition |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63162571A (en) |
-
1986
- 1986-12-25 JP JP61314623A patent/JPS63162571A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS63162571A (en) | 1988-07-06 |
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