JPH0355710A - Low temperature sintered porcelain material - Google Patents
Low temperature sintered porcelain materialInfo
- Publication number
- JPH0355710A JPH0355710A JP19003689A JP19003689A JPH0355710A JP H0355710 A JPH0355710 A JP H0355710A JP 19003689 A JP19003689 A JP 19003689A JP 19003689 A JP19003689 A JP 19003689A JP H0355710 A JPH0355710 A JP H0355710A
- Authority
- JP
- Japan
- Prior art keywords
- temperature
- mol
- dielectric
- cuo
- temperature sintered
- 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.)
- Granted
Links
- 239000000463 material Substances 0.000 title claims abstract description 32
- 229910052573 porcelain Inorganic materials 0.000 title claims abstract description 20
- 239000000203 mixture Substances 0.000 abstract description 4
- 230000007423 decrease Effects 0.000 abstract description 3
- 238000005245 sintering Methods 0.000 abstract description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract 2
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 abstract 1
- 239000003989 dielectric material Substances 0.000 description 10
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 6
- 239000002131 composite material Substances 0.000 description 6
- 239000000696 magnetic material Substances 0.000 description 6
- 238000010304 firing Methods 0.000 description 5
- 238000009413 insulation Methods 0.000 description 4
- 239000003990 capacitor Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- 229910007565 Zn—Cu Inorganic materials 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000002305 electric material Substances 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Landscapes
- Inorganic Insulating Materials (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
この発明は低温焼結磁器材料に関し、特に１０００℃以
下の低温で焼威可能で、たとえば、低容量のＥＭＩフィ
ルタ用の誘電体材料あるいは磁性体と誘電体とを一体焼
結したＬＣ複合チップＥＭ■フィルタ用の誘電体材料と
して使用するのに好適な低温焼結磁器材料に関する。Detailed Description of the Invention (Industrial Application Field) The present invention relates to low-temperature sintered porcelain materials, particularly those that can be fired at a low temperature of 1000°C or less, and are suitable for use as dielectric materials or magnetic materials for low-capacity EMI filters, for example. The present invention relates to a low-temperature sintered porcelain material suitable for use as a dielectric material for an LC composite chip EM filter in which a body and a dielectric are integrally sintered.
（従来技術）
従来、１０００℃以下で焼成が可能である低温焼結磁器
材料としては、ｐｂ系複合ベロブスヵイト材料に代表さ
れるが、ｐｂ系材料は、誘電率εが１０００以上と大き
いうえに、誘電率εの温度変化率も−２５℃〜＋８５℃
で±５０％と大きい。(Prior art) Conventionally, a low-temperature sintered porcelain material that can be fired at 1000°C or lower is represented by a PB-based composite berovskite material. Temperature change rate of dielectric constant ε is also -25℃ to +85℃
It is large at ±50%.
したがって、ｐｂ系材料では、数１ ０ｐＦの低容量を
取得しにくい。Therefore, with pb-based materials, it is difficult to obtain a capacitance as low as several 10 pF.
さらに、低温焼結磁器材料としては、ＴＣ系材料（ＮＰ
＝０）もある。ＴＣ系材料においては、７， ｒ Ｑ
ｚ Ａ ｌ ｚ○３ＳｉＯ！（ガラス成分）系材料が
約１０００℃で焼成可能であるが、誘電率εがＩＯ前後
と小さい。Furthermore, as low-temperature sintered porcelain materials, TC-based materials (NP
=0) is also available. In TC-based materials, 7, r Q
z A l z○3SiO! (Glass component) type material can be fired at about 1000°C, but the dielectric constant ε is small at around IO.
そこで、誘電率εが！００前後の低温焼結磁器材料とし
て、特公昭６２−５７０４２号にＴｉＯｚ−ＣｕＯ−Ｍ
ｎ系材料が、特開昭６０−１０６１２０号にＴｉＯ２−
Ｎｉ○−Ｃ ｕ Ｏ − Ｍ ｎ系材料がそれぞれ開示
され、それらの材料が、ＬＣ複合チップ用の誘電体材料
として用いられている。Therefore, the dielectric constant ε! As a low temperature sintered porcelain material around 00, TiOz-CuO-M was published in Japanese Patent Publication No. 62-57042
The n-based material is TiO2-
Ni○-CuO-Mn-based materials are disclosed, respectively, and these materials are used as dielectric materials for LC composite chips.
（発明が解決しようとする課題）
？電体となる材料と磁性体となる材料とを貼り合わせ一
体焼結することによってＬＣ複合チップが得られるが、
その誘電体としてＢＴ系材料を用いれば、１２００〜１
３００℃の高い焼成温度が必要となる。ところが、電極
材料のコストおよびエネルギ的コストなどの観点から、
焼成温度は低い方が望ましい。(Problem that the invention seeks to solve)? An LC composite chip can be obtained by bonding together an electric material and a magnetic material and sintering them together.
If a BT-based material is used as the dielectric, 1200~1
A high firing temperature of 300°C is required. However, from the viewpoint of electrode material cost and energy cost,
A lower firing temperature is desirable.
そこで、誘電体としてｐｂ系複合ペロブス力イト材料を
用い、磁性体としてＮ＋−Ｚｎ−Ｃｕフェライトを用い
れば、約ｔｏｏｏ℃で一体焼結させることによってＬＣ
？Ｊｊ合チップが得られるが、磁性体から誘電体へのＦ
ｅなとの元素の拡散によりコンデンサ部の諸特性が劣化
し実用に供せないものとなる場合もある。Therefore, if a PB-based composite perovskite material is used as the dielectric material and N+-Zn-Cu ferrite is used as the magnetic material, LC
? Jj joint chip is obtained, but F from magnetic material to dielectric material
In some cases, the various characteristics of the capacitor section deteriorate due to the diffusion of elements such as e, making it unusable for practical use.
また、ｐｂ系材料を用いてコンデンサ部の諸特性を満足
させても、その誘電率εが１０００以上と大きいため、
数１０ｐＦの小容量を取得するのは困難である．そのｐ
ｂ系材料としてＰｂ（Ｎｉ＋／ｆｆ Ｎｂｘｉｓ
） Ｏｓ ＰｂＴｉＯｚ Ｐｂ
（Ｚｎ１７■Ｗｌ／■）Ｏ，系材料が挙げられるが、
誘電率εの温度変化が大き過ぎて、それをＥＭＩフィル
タの材料として用いた場合、挿入損失の周波数特性が変
化し、カット・オフ周波数がシフトしてしまう・これは
、一般に、ｐｂ系材料の誘電率εの温度変化率が大きい
からである。Furthermore, even if the various characteristics of the capacitor part are satisfied using a PB-based material, its dielectric constant ε is as large as 1000 or more.
It is difficult to obtain a small capacitance of several tens of pF. That p
Pb(Ni+/ff Nbxis
) Os PbTiOz Pb
(Zn17■Wl/■)O, type materials are mentioned,
If the temperature change in the dielectric constant ε is too large and it is used as a material for an EMI filter, the frequency characteristics of insertion loss will change and the cut-off frequency will shift. This is because the temperature change rate of the dielectric constant ε is large.
それゆえに、この発明の主たる目的は、１０００℃以下
で焼結でき、しかも、１７〜８０の誘電率εを有し、か
つ、誘電率εの温度変化率の小さい、低温焼結磁器材料
を提供することである。Therefore, the main object of the present invention is to provide a low-temperature sintered porcelain material that can be sintered at temperatures below 1000°C, has a dielectric constant ε of 17 to 80, and has a small temperature change rate of the dielectric constant ε. It is to be.
（課題を解決するための手段）
この発明は、ＺｒＯｚを４４．０ 〜９９．５モル％、
Ｔｉｅｚを０〜４４．７７５モル％、およびＣｕＯを０
．５〜１５モル％含み、それらの合計が１００モル％と
なる、低温焼結磁器材料である．
（発明の効果）
この発明によれば、１０００℃以下で焼結でき、しかも
、１７〜８０の誘電率εを有し、かつ、誘電率εの温度
変化率の小さい、低温焼結磁器材料が得られる．
したがって、この発明にかかる低温焼結磁器材料は、そ
れをたとえばＬＣ複合チ・ノプＥＭＩフィルタの誘電体
材料として使用できるほか、それを単独の誘電体材料と
して用いることもできる。(Means for Solving the Problems) This invention contains ZrOz in an amount of 44.0 to 99.5 mol%,
Tiez 0-44.775 mol% and CuO 0
．． It is a low-temperature sintered porcelain material containing 5 to 15 mol%, with a total of 100 mol%. (Effects of the Invention) According to the present invention, there is a low-temperature sintered porcelain material that can be sintered at 1000°C or lower, has a dielectric constant ε of 17 to 80, and has a small temperature change rate of the dielectric constant ε. can get. Therefore, the low temperature sintered porcelain material according to the present invention can be used, for example, as a dielectric material of an LC composite chip EMI filter, and can also be used as a single dielectric material.
また、この発明にかかる低温焼結磁器材料は、たとえば
低温焼結基板と一体焼成することも可能である。Furthermore, the low-temperature sintered porcelain material according to the present invention can be integrally fired with, for example, a low-temperature sintered substrate.
この発明の上述の目的，その他の目的．特徴および利点
は、図面を参照して行う以下の実施例の詳細な説明から
一層明らかとなろう。The above objectives and other objectives of this invention. Features and advantages will become more apparent from the following detailed description of the embodiments with reference to the drawings.
（実施例）
まず、原料として、ｚｒｏ，，ＴｉＣｈおよびＣｕＱを
別表に示す組或となるように秤量し調合し、それにイオ
ン交換水および酢酸ビニル系バインダを５重量％加え、
直径５朋のジルコニアボールを玉石としてボソトミルで
２４時間混合，粉砕した．
そして、それを蒸発乾燥，整粒の工程を経て、２．５ｔ
／一で乾式プレス或形を行って、直径ｌＱｍｍ，厚さ０
．８關の戒形体ユニットを得た。(Example) First, as raw materials, zro, TiCh, and CuQ were weighed and mixed to have the composition shown in the attached table, and 5% by weight of ion-exchanged water and vinyl acetate binder were added thereto.
Zirconia balls with a diameter of 5 mm were used as cobblestones and mixed and crushed for 24 hours in a bosoto mill. Then, through the process of evaporation drying and sizing, 2.5 tons of
/Dry press or shape with diameter 1Qmm, thickness 0
．． Obtained a 8-piece precept unit.
それから、その成形体ユニットを空気中・ １０００℃
で２時間焼成して、磁器を形威した。そして、その磁器
の両主面に電極を形威して、試料１〜３７を得た。Then, the molded unit was heated in air at 1000°C.
The porcelain was fired for two hours to give it its shape. Then, electrodes were formed on both main surfaces of the porcelain to obtain samples 1 to 37.
それらの試料１〜３７について、誘電体率ε，誘電体損
Ｄ． Ｆ （％）および比抵抗ρ（Ω・ｅｌｍ）など
を測定した。その測定結果を別表に示す。Regarding those samples 1 to 37, dielectric constant ε, dielectric loss D. F (%), specific resistance ρ (Ω·elm), etc. were measured. The measurement results are shown in the attached table.
この発明にかかる低温焼結磁器材料の組成範囲を限定し
た理由は次の通りである。The reason for limiting the composition range of the low temperature sintered porcelain material according to the present invention is as follows.
ＣｕＯの添加量が１５モル％を超えると絶縁抵抗が著し
く低下する。また、ＣｕＯの添加量が０５モル％未満で
は、極めて焼結性が悪い。なお、ＣｕＯの添加量が０．
５モル％では、必ずしも焼結性がよいとは言えないが、
ＺｒＯ，およびＣｕＯの微粉末化および混合度を強める
など粉末特性を改善することによって、焼結性の向上が
図られているので、ＣｕＯの添加量が０．５モル％のも
のも、この発明の範囲内とした。When the amount of CuO added exceeds 15 mol %, the insulation resistance decreases significantly. Furthermore, if the amount of CuO added is less than 0.5 mol %, sinterability is extremely poor. Note that when the amount of CuO added is 0.
Although it cannot be said that sinterability is necessarily good at 5 mol%,
Since the sinterability is improved by improving the powder properties such as finely powdering ZrO and CuO and increasing the mixing degree, the present invention also has the added amount of CuO of 0.5 mol%. was within the range of
Ｚ ｒ ０２ ： Ｔ ｉ Ｏｔのモル比が５５ ：
４５である場合を基準にしたとき、その基準を超える
よう？Ｔｉ○２が増加すると、ＣｕＯの添加量に対する
絶縁抵抗の低下が著しく、焼成温度およびＣｕＯの添加
量の管理幅が狭くなる傾向にある。それに対して、この
発明にかかる低温焼結磁器材料の範囲は、Ｚｒ○ｚ：Ｔ
ｉｏｚのモル比が５５＝４５〜１００：０の範囲にあり
、誘電体特性が焼或温度およびＣｕＯの添加量の影響に
対して安定な領域である。The molar ratio of Z r 02 : T i Ot is 55:
If the standard is 45, does it exceed that standard? As Ti○2 increases, the insulation resistance decreases significantly with respect to the amount of CuO added, and the control range for the firing temperature and amount of CuO tends to become narrower. On the other hand, the range of the low temperature sintered porcelain material according to the present invention is Zr○z:T
The molar ratio of ioz is in the range of 55=45 to 100:0, which is a region in which dielectric properties are stable against the effects of annealing temperature and the amount of CuO added.
これらの関係の一例を、第１図ないし第４図に基づいて
説明する。An example of these relationships will be explained based on FIGS. 1 to 4.
第１図は、この発明の実施例としてＺｒＯ■ ：Ｔｉｅ
２のモル比を８：２とした場合のＣｕＯの添加量（モル
％）と誘電率εおよび誘電体損Ｄ．Ｆ（％）との関係を
示すグラフであり、第２図はその場合のＣｕＯの添加量
（モル％〉と比抵抗ρの対数値Ｌｏｇρとの関係を示す
グラフである。FIG. 1 shows ZrO■:Tie as an embodiment of the present invention.
Addition amount (mol%) of CuO, dielectric constant ε, and dielectric loss D.2 when the molar ratio of D.2 is 8:2. This is a graph showing the relationship between F (%), and FIG. 2 is a graph showing the relationship between the amount of CuO added (mol %) and the logarithm value Logρ of the specific resistance ρ in that case.
一方、第３図は、比較例としてＺｒＯ．：Ｔｉ○２のモ
ル比を２：８とした場合のＣｕＯの添加量（モル％）と
誘電率εおよび誘電体損Ｄ． Ｆ （％）との関係を
示すグラフであり、第４図はその場合のＣｕＯの添加量
（モル％）と比抵抗ρの対数値Ｌｏｇρとの関係を示す
グラフである。On the other hand, FIG. 3 shows ZrO. : Addition amount (mol%) of CuO, dielectric constant ε, and dielectric loss D. when the molar ratio of Ti○2 is 2:8. FIG. 4 is a graph showing the relationship between the amount of CuO added (mol %) and the logarithm value Logρ of the specific resistance ρ in that case.
第１図ないし第４図に示すグラフから明らかなように、
Ｚ ｒ Ｏｚ ： Ｔ ｉ Ｏｚのモル比を２：８と
した比較例では、極めて限られた範囲の組成でないと誘
電体として使用することができない。すなわち、誘電体
特性として焼成温度およびＣｕＯの添加量の依存が強い
のである。それに対して、Ｚｒ Ｏｚ ： Ｔ ｉ
ＯＸのモル比を８：２とした実施例では、焼戊温度およ
びＣｕＯの添加量に対して広い範囲で誘電体として使用
することができる。As is clear from the graphs shown in Figures 1 to 4,
In a comparative example in which the molar ratio of Z r Oz :T i Oz was 2:8, it could not be used as a dielectric unless it had a composition within an extremely limited range. That is, the dielectric properties are strongly dependent on the firing temperature and the amount of CuO added. On the other hand, Zr Oz: T i
In the example in which the molar ratio of OX is 8:2, it can be used as a dielectric material over a wide range of firing temperatures and amounts of CuO added.
また、第５図および第６図に誘電率の温度変化率を示し
た。この場合、第５図には試料番号２２のもの、第６図
には試料番号３３のものを示した。Moreover, the temperature change rate of the dielectric constant is shown in FIGS. 5 and 6. In this case, FIG. 5 shows sample number 22, and FIG. 6 shows sample number 33.
第５図および第６図から明らかなように、この発明にか
かる低温焼結磁器材料によれば、誘電率の温度変化率の
小さいものが得られる。As is clear from FIGS. 5 and 6, the low temperature sintered porcelain material according to the present invention has a small rate of change in dielectric constant with temperature.
なお、この発明にかかる低温焼結磁器材料には、ＭｎＯ
をＭｎ○３に換算して５．０重量％以下添加してもよい
。このようにＭ ｎ Ｏを添加すれば、比抵抗が増し、
絶縁抵抗が改善される。特に磁性体と一体焼結した場合
、磁性体の威分てあるＦｅが誘電体中に拡散する傾向が
あり、誘電体の絶縁抵抗が低下するが、ＭｎＯを添加す
ることにより絶縁抵抗の低下を抑えることができる。Note that the low-temperature sintered porcelain material according to this invention includes MnO
may be added in an amount of 5.0% by weight or less calculated as Mn○3. By adding MnO in this way, the specific resistance increases,
Insulation resistance is improved. In particular, when sintered together with a magnetic material, Fe, which is the dominant force of the magnetic material, tends to diffuse into the dielectric material, reducing the insulation resistance of the dielectric material. It can be suppressed.
第１図はこの発明の一実施例としてＺｒＯ２ ：Ｔ ｉ
○２のモル比を８＝２とした場合におけるＣＵ○の添加
量（モル％）と誘電率εおよび誘電体ｔ員Ｄ． Ｆ
（％）との関係を示すグラフであり、第２図はその場合
におけるＣｕＯの添加量（モル％〉と比抵抗ρの対数値
Ｌｏｇρとの関係を示すグラフである。
第３図は比較例としてＺ ｒ Ｏ２： Ｔ ｉ Ｏｚの
モル比を２：８とした場合におけるＣｕＯの添加壇（モ
ル％）と誘電率εおよび誘電体損Ｄ． Ｆ （％）と
の関係を示すグラフであり、第４図はその場合における
Ｃｕ○の添加量（モル％）と比抵抗ρの対数値Ｌｏｇρ
との関係を示すグラフである。
第５図および第６図は、それぞれ、この発明の実施例に
かかる誘電率の温度変化率を示すグラフである。FIG. 1 shows ZrO2 :T i as an embodiment of the present invention.
Addition amount (mol%) of CU○, dielectric constant ε, and dielectric t member D. when the molar ratio of ○2 is 8=2. F
(%), and FIG. 2 is a graph showing the relationship between the amount of CuO added (mol%) and the logarithm Logρ of the specific resistance ρ in that case. FIG. 3 is a comparative example It is a graph showing the relationship between the CuO addition stage (mol%), the dielectric constant ε, and the dielectric loss D.F (%) when the molar ratio of ZrO2:TiOz is 2:8. Figure 4 shows the amount of Cu○ added (mol%) and the logarithm of the specific resistance ρ in that case.
It is a graph showing the relationship between FIG. 5 and FIG. 6 are graphs showing the rate of change in dielectric constant with temperature according to the embodiment of the present invention, respectively.
Claims (1)
２を０〜４４．７７５モル％、およびＣｕＯを０．５〜
１５モル％含み、 それらの合計が１００モル％となる、低温焼結磁器材料
。 ２ さらに、ＭｎをＭｎＣＯ＿３に換算して５．０重量
％以下含む、特許請求の範囲第１項記載の低温焼結磁器
材料。[Claims] 1 44.0 to 99.5 mol% of ZrO_2, TiO_
0 to 44.775 mol% of 2 and 0.5 to 44.775 mol% of CuO
A low-temperature sintered porcelain material containing 15 mol%, the total of which is 100 mol%. 2. The low-temperature sintered porcelain material according to claim 1, further comprising 5.0% by weight or less of Mn in terms of MnCO_3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19003689A JPH0817059B2 (en) | 1989-07-21 | 1989-07-21 | Low temperature sintered porcelain material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19003689A JPH0817059B2 (en) | 1989-07-21 | 1989-07-21 | Low temperature sintered porcelain material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0355710A true JPH0355710A (en) | 1991-03-11 |
| JPH0817059B2 JPH0817059B2 (en) | 1996-02-21 |
Family
ID=16251294
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP19003689A Expired - Fee Related JPH0817059B2 (en) | 1989-07-21 | 1989-07-21 | Low temperature sintered porcelain material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0817059B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001017926A1 (en) * | 1999-08-26 | 2001-03-15 | Universiteit Twente | Device comprising a member of ceramic material and a method for manufacturing a ceramic material having a low friction coefficient |
-
1989
- 1989-07-21 JP JP19003689A patent/JPH0817059B2/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001017926A1 (en) * | 1999-08-26 | 2001-03-15 | Universiteit Twente | Device comprising a member of ceramic material and a method for manufacturing a ceramic material having a low friction coefficient |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0817059B2 (en) | 1996-02-21 |
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| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |