JPH0332162B2 - - Google Patents
Info
- Publication number
- JPH0332162B2 JPH0332162B2 JP56054139A JP5413981A JPH0332162B2 JP H0332162 B2 JPH0332162 B2 JP H0332162B2 JP 56054139 A JP56054139 A JP 56054139A JP 5413981 A JP5413981 A JP 5413981A JP H0332162 B2 JPH0332162 B2 JP H0332162B2
- Authority
- JP
- Japan
- Prior art keywords
- composition
- present
- dielectric constant
- pbo
- mgo
- 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
Links
- 239000000203 mixture Substances 0.000 claims description 22
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 9
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 9
- 239000000395 magnesium oxide Substances 0.000 claims description 9
- HTUMBQDCCIXGCV-UHFFFAOYSA-N lead oxide Chemical compound [O-2].[Pb+2] HTUMBQDCCIXGCV-UHFFFAOYSA-N 0.000 claims description 8
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 7
- 239000000919 ceramic Substances 0.000 claims description 6
- 239000011777 magnesium Substances 0.000 claims description 5
- FKSZLDCMQZJMFN-UHFFFAOYSA-N [Mg].[Pb] Chemical compound [Mg].[Pb] FKSZLDCMQZJMFN-UHFFFAOYSA-N 0.000 claims 1
- NKTZYSOLHFIEMF-UHFFFAOYSA-N dioxido(dioxo)tungsten;lead(2+) Chemical compound [Pb+2].[O-][W]([O-])(=O)=O NKTZYSOLHFIEMF-UHFFFAOYSA-N 0.000 claims 1
- NKZSPGSOXYXWQA-UHFFFAOYSA-N dioxido(oxo)titanium;lead(2+) Chemical compound [Pb+2].[O-][Ti]([O-])=O NKZSPGSOXYXWQA-UHFFFAOYSA-N 0.000 claims 1
- 229910052742 iron Inorganic materials 0.000 claims 1
- 229910000464 lead oxide Inorganic materials 0.000 claims 1
- 239000003990 capacitor Substances 0.000 description 6
- 229910052573 porcelain Inorganic materials 0.000 description 5
- 230000007423 decrease Effects 0.000 description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- 239000003989 dielectric material Substances 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 229910020215 Pb(Mg1/3Nb2/3)O3PbTiO3 Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910002367 SrTiO Inorganic materials 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052454 barium strontium titanate Inorganic materials 0.000 description 1
- 229910002113 barium titanate Inorganic materials 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
- 239000011230 binding agent Substances 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 description 1
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 description 1
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Compositions Of Oxide Ceramics (AREA)
- Ceramic Capacitors (AREA)
- Inorganic Insulating Materials (AREA)
Description
本発明は1000℃以下の低温で焼結できる高誘電
率磁器組成物に関するものである。
従来、高誘電率誘電体はチタン酸バリウム，チ
タン酸ストロンチウムを主成分とするものが広く
実用化されていた。
しかしながら、これらのBaTiO3，SrTiO3を主
成分とするものは通常1300〜1400℃の高温で焼結
しなければならず、高品質の積層コンデンサ及び
厚膜コンデンサを製造しようとすれば、この焼結
温度に適した内部電極として、白金，パラジウム
等の高価な貴金属を使用しなければならないとい
う欠点がある。
そこで低価格の銀を主成分とする安価な内部電
極の使用を可能とするためにも、できる限り900
〜1000℃付近の低温温度で焼結できる誘導体の材
料が強く要望される。
本発明の目的は、低温で焼結できるとともに誘
電率が高く、しかも誘導損失が小さく、かつ比抵
抗が高い、誘電体特性の優れた高誘電率磁器組成
物を提供するものである。
本発明はPb（Fe2/3W1/3）O3−Pb（Mg1/3−
Nb2/3）O3−PbTiO3の三成分系組成ならびに
PbO，MgOを過剰に添加させたことにより、室
温で誘導率を著しく増加させ、かつ比抵抗を増加
させ、しかも1000℃以下の低温で焼結できる高性
能な高誘電率磁器組成物を発明したものである。
すなわち、本発明の磁器組成物は
Pb（Fe2/3W1/3）O3，Pb（Mg1/3Nb2/3）O3，
PbTiO3，PbOおよびMgOよりなる組成物を、
〔Pb（Fe2/3W1/3）O3〕X〔Pb（Mg1/3Nb2/3）O3〕Y
〔PbTiO3〕Z＋Awt％PbO＋Bwt％MgOと表した
時に、Ｘ，Ｙ，Ｚ，Ａ，Ｂの範囲が
Ｘ＝0.01〜0.20
Ｙ＝0.60〜0.98
Ｚ＝0.01〜0.20
（但し、Ｘ＋Ｙ＋Ｚ＝１）
０≦Ａ≦20
０≦Ｂ≦５
よりなることを特徴とするものである。
本発明の磁器組成物は積層コンデンサ、厚膜コ
ンデンサの誘電体として適用できる。本発明の高
誘電率磁器組成物を製造すれば、1000℃以下で安
易に焼結が可能なため、積層コンデンサ，厚膜コ
ンデンサの製造に内部電極として銀系金属を使用
できることが可能で、コンデンサを安価に製造で
きる。
以下、本発明を実施例にて詳細に説明する。原
料酸化物として酸化鉛（PbO），酸化第二鉄
（Fe2O3），酸化タングステン（WO3），酸化チタ
ン（TiO2），五酸化ニオブ（Nb2O5），酸化マグ
ネシウム（MgO）の各原料を下記の第１表に示
した組成に全体が200ｇになるように秤量した。
これらとともにメノウ石300ｇ、純水200ｇをボー
ルミルで混合させ、スラリー化した後に固化乾燥
させる。次に、アルミナルツボで700〜850℃で仮
焼した。この仮焼粉末30ｇと５％PVA溶液をバ
インダーとして加え、約700Kg／cm2の圧力で直径
20mm，厚さ１mmの円板に成形し、これを900〜
1000℃で１時間焼成して焼結体を得た。得られた
焼結体には導電性銀ペーストを塗布して電極を形
成し、電気的諸特性の測定試料とした。諸電率及
び誘電損失は1KHz、温度25℃で測定した。比抵
抗は直流100Vを印加して室温で測定した。その
結果を第２表に示している。
The present invention relates to a high dielectric constant ceramic composition that can be sintered at a low temperature of 1000°C or lower. Conventionally, high permittivity dielectrics containing barium titanate and strontium titanate as main components have been widely put into practical use. However, these materials whose main components are BaTiO 3 and SrTiO 3 must be sintered at a high temperature of 1,300 to 1,400°C, and this sintering is necessary to produce high-quality multilayer capacitors and thick film capacitors. A drawback is that an expensive noble metal such as platinum or palladium must be used as an internal electrode suitable for the freezing temperature. Therefore, in order to enable the use of inexpensive internal electrodes that are mainly composed of low-priced silver, we
There is a strong demand for dielectric materials that can be sintered at low temperatures around ~1000°C. An object of the present invention is to provide a high-permittivity ceramic composition that can be sintered at low temperatures, has a high dielectric constant, has low induction loss, and has high specific resistance, and has excellent dielectric properties. The present invention is based on Pb(Fe 2/3 W 1/3 ) O 3 −Pb(Mg 1/3 −
Nb 2/3 ) O 3 −PbTiO 3 ternary composition and
By adding excessive amounts of PbO and MgO, we have invented a high-permittivity porcelain composition that significantly increases the dielectric constant and resistivity at room temperature, and can be sintered at low temperatures below 1000℃. It is something. That is, the ceramic composition of the present invention contains Pb(Fe 2/3 W 1/3 )O 3 , Pb(Mg 1/3 Nb 2/3 )O 3 ,
A composition consisting of PbTiO 3 , PbO and MgO is expressed as [Pb (Fe 2/3 W 1/3 ) O 3 ] X [Pb (Mg 1/3 Nb 2/3 ) O 3 ] Y
[PbTiO 3 ] When expressed as Z + Awt%PbO + Bwt%MgO, the range of X, Y, Z, A, B is ≦A≦20 0≦B≦5. The ceramic composition of the present invention can be applied as a dielectric material for multilayer capacitors and thick film capacitors. If the high dielectric constant ceramic composition of the present invention is manufactured, it can be easily sintered at temperatures below 1000°C, making it possible to use silver-based metals as internal electrodes in the manufacture of multilayer capacitors and thick film capacitors. can be manufactured at low cost. Hereinafter, the present invention will be explained in detail with reference to Examples. Raw material oxides include lead oxide (PbO), ferric oxide (Fe 2 O 3 ), tungsten oxide (WO 3 ), titanium oxide (TiO 2 ), niobium pentoxide (Nb 2 O 5 ), and magnesium oxide (MgO). Each of the raw materials was weighed so that the total amount was 200 g according to the composition shown in Table 1 below.
Together with these, 300 g of agate stone and 200 g of pure water are mixed in a ball mill to form a slurry, which is then solidified and dried. Next, it was calcined at 700 to 850°C in an aluminium crucible. Add 30g of this calcined powder and 5% PVA solution as a binder, and apply a pressure of about 700Kg/cm 2 to
Form into a disc of 20mm and 1mm thick, and heat it to 900~
A sintered body was obtained by firing at 1000°C for 1 hour. The obtained sintered body was coated with conductive silver paste to form electrodes, and used as a sample for measuring various electrical properties. Electrical constants and dielectric losses were measured at 1 KHz and 25°C. The specific resistance was measured at room temperature by applying 100 V DC. The results are shown in Table 2.
【表】
但し、＊印は請求範囲外
また、図は本発明に係る磁器組成物の主成分の
成分組成を示す三角組成図であり、図中の番号は
上記表中の試料No.と対応している。
表からも明らかなように本発明の範囲内のもの
は、誘電率が3000〜15000と高く、誘電損失が0.4
〜3.5％と極めて小さく、また比抵抗は10″Ω・cm
以上で、しかも1000℃以下で焼結が可能である。
すなわち、この組成からずれるものは表に示すよ
うに望ましい特性は得られなかつた。
なお、本発明の組成物を
〔Pb（Fe2/3W1/3）O3〕X〔Pb（Mg1/3Nb2/3）O3〕Y
〔PbTiO3〕Z＋Awt％PbO＋Bwt％MgOと表した
時に、Ｘ，Ｙ，Ｚ，Ａ，Ｂの範囲が
Ｘ＝0.01〜0.20
Ｙ＝0.60〜0.98
Ｚ＝0.01〜0.20
（但し、Ｘ＋Ｙ＋Ｚ＝１）
０≦Ａ≦20
０≦Ｂ≦５
と限定される。この理由はＸが20モル％を超える
と誘電率が低下する。一方、Ｘが１モル％未満に
なると誘電損失が大きくなる。また、Ｚが20モル
％を超えると焼結が不可能になり、逆に１モル％
を切ると誘電率が低下する。ＹはＸ，Ｚから決定
される。次に、Ａは20wt％までは焼結性が増し
誘電率が大きくなるが、20wt％を超えると磁器
がポーラスとなり誘電率が減少し、誘電損失が大
きくなり比抵抗も小さくなる。また、ＢもＡと同
様に5wt％までは特性が向上するが、5wt％を超
えると上記の誘電体特性が劣化する。
以上述べたように本発明の磁器組成物は1000℃
以下の低温で焼結でき、通常のデイスクコンデン
サのみならず、特に大容量の積層コンデンサ用材
料及び大容量厚膜コンデンサ用材料に適し、しか
もより安価な焼成炉の使用を可能とし、かつ熱エ
ネルギーを節約し得る非常に優れた組成物であ
る。[Table] However, * marks are outside the scope of claims. The figure is a triangular composition diagram showing the composition of the main components of the porcelain composition according to the present invention, and the numbers in the figure correspond to the sample numbers in the table above. are doing. As is clear from the table, those within the scope of the present invention have a high dielectric constant of 3000 to 15000 and a dielectric loss of 0.4.
Extremely small ~3.5%, and specific resistance is 10″Ω・cm
Sintering is possible at temperatures above 1000°C or below.
That is, if the composition deviated from this composition, desired characteristics could not be obtained as shown in the table. Note that the composition of the present invention is [Pb(Fe 2/3 W 1/3 ) O 3 ] X [Pb(Mg 1/3 Nb 2/3 ) O 3 ] Y
[PbTiO 3 ] When expressed as Z + Awt%PbO + Bwt%MgO, the range of X, Y, Z, A, B is It is limited to ≦A≦20 0≦B≦5. The reason for this is that when X exceeds 20 mol%, the dielectric constant decreases. On the other hand, when X is less than 1 mol %, dielectric loss increases. Also, if Z exceeds 20 mol%, sintering becomes impossible, and conversely, if Z exceeds 1 mol%
When cut, the dielectric constant decreases. Y is determined from X and Z. Next, up to 20 wt% of A increases the sinterability and increases the dielectric constant, but when it exceeds 20 wt%, the porcelain becomes porous and the dielectric constant decreases, the dielectric loss increases and the resistivity decreases. Further, like A, the characteristics of B improve up to 5 wt%, but when it exceeds 5 wt%, the above-mentioned dielectric characteristics deteriorate. As mentioned above, the porcelain composition of the present invention
It can be sintered at a low temperature of less than This is an excellent composition that can save you a lot of money.
図は本発明に係る磁器組成物の主成分の成分組
成を示す三角組成図である。
The figure is a triangular composition diagram showing the composition of the main components of the porcelain composition according to the present invention.
Claims (1)
マグネシウム・ニオブ酸鉛Pb（Mg1/3Nb2/3）O3，
チタン酸鉛PbTiO3，酸化鉛PbOおよび酸化マグ
ネシウムMgOよりなる組成物を、 〔Pb（Fe2/3W1/3）O3〕X〔Pb（Mg1/3Nb2/3）O3〕Y
〔PbTiO3〕Z＋Awt％PbO＋Bwt％MgOと表した
時に、Ｘ，Ｙ，Ｚ，Ａ，Ｂの範囲が Ｘ＝0.01〜0.20 Ｙ＝0.60〜0.98 Ｚ＝0.01〜0.20 （但し、Ｘ＋Ｙ＋Ｚ＝１） ０≦Ａ≦20 ０≦Ｂ≦５ よりなる高誘電率磁器組成物。[Claims] 1. Iron/lead tungstate Pb (Fe 2/3 W 1/3 ) O 3 ,
Magnesium lead niobate Pb (Mg 1/3 Nb 2/3 ) O 3 ,
A composition consisting of lead titanate PbTiO 3 , lead oxide PbO, and magnesium oxide MgO, [Pb (Fe 2/3 W 1/3 ) O 3 ] X [Pb (Mg 1/3 Nb 2/3 ) O 3 ] Y
[PbTiO 3 ] When expressed as Z + Awt%PbO + Bwt%MgO, the range of X, Y, Z, A, B is A high dielectric constant ceramic composition comprising ≦A≦20 0≦B≦5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP56054139A JPS57168405A (en) | 1981-04-09 | 1981-04-09 | High dielectric porcelain composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP56054139A JPS57168405A (en) | 1981-04-09 | 1981-04-09 | High dielectric porcelain composition |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS57168405A JPS57168405A (en) | 1982-10-16 |
| JPH0332162B2 true JPH0332162B2 (en) | 1991-05-10 |
Family
ID=12962229
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP56054139A Granted JPS57168405A (en) | 1981-04-09 | 1981-04-09 | High dielectric porcelain composition |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS57168405A (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61109204A (en) * | 1984-10-31 | 1986-05-27 | 株式会社村田製作所 | Dielectric porcelain composition |
| JPH01100051A (en) * | 1987-10-12 | 1989-04-18 | Mitsubishi Mining & Cement Co Ltd | Dielectric porcelain composition |
| JP2658121B2 (en) * | 1988-02-03 | 1997-09-30 | 松下電器産業株式会社 | High dielectric materials and capacitors using the same |
| CN104557038B (en) * | 2014-12-30 | 2017-07-07 | 中国科学院声学研究所 | A kind of compound system pyroelectric ceramic material and preparation method thereof |
-
1981
- 1981-04-09 JP JP56054139A patent/JPS57168405A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS57168405A (en) | 1982-10-16 |
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