JP5488954B2 - Polycrystalline ceramic magnetic material, microwave magnetic material, and non-reciprocal circuit device using the same - Google Patents
Polycrystalline ceramic magnetic material, microwave magnetic material, and non-reciprocal circuit device using the same Download PDFInfo
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- 229910052727 yttrium Inorganic materials 0.000 description 3
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 3
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
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- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 2
- 229910052763 palladium Inorganic materials 0.000 description 2
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- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 1
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 1
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- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910003437 indium oxide Inorganic materials 0.000 description 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
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- Soft Magnetic Materials (AREA)
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Description
本発明は、高周波回路部品に使用されるマイクロ波用磁性体材料であり、さらに銀や銅といった電極用材料との同時焼成が可能な多結晶セラミック磁性材料に関する。 The present invention relates to a magnetic material for microwaves used for high-frequency circuit components, and further relates to a polycrystalline ceramic magnetic material that can be simultaneously fired with electrode materials such as silver and copper.
近年、自動車電話、携帯電話、衛星放送など、マイクロ波領域の電磁波を利用する通信技術の進展に伴い、機器の小型化が要求されている。このためには、機器を構成する個々の部品の小型化、低背化の要求が益々増大している。 In recent years, miniaturization of devices has been demanded with the progress of communication technology using electromagnetic waves in the microwave region, such as car phones, mobile phones, and satellite broadcasts. For this purpose, there is an increasing demand for downsizing and low profile of individual parts constituting the equipment.
通信機器の分野において用いられる代表的な高周波回路部品として、たとえば、サーキュレータ、アイソレータなどのマイクロ波非可逆回路素子がある。一般にアイソレータは、信号の伝送方向にはほとんど減衰がなく、かつ逆方向には減衰が大きくなる様な機能を有しており、たとえばマイクロ波帯、ＵＨＦ帯で使用される携帯電話、自動車電話等の移動体通信器の送受信回路に用いられている。 As typical high-frequency circuit components used in the field of communication equipment, for example, there are microwave nonreciprocal circuit elements such as circulators and isolators. In general, an isolator has a function such that there is almost no attenuation in the signal transmission direction and the attenuation is increased in the opposite direction. For example, a cellular phone, a car phone, etc. used in the microwave band and the UHF band. This is used in a transmission / reception circuit of a mobile communication device.
サーキュレータ、アイソレータなどの非可逆回路素子は、互いに絶縁された状態で配置した複数の電極ラインを有する中心導体と、これら中心導体に密接して配置されるマイクロ波用磁性体と、前記中心導体及び前記マイクロ波用磁性体からなる中心導体組立体に直流磁界を印可する永久磁石を備えた構成であって、中心導体とマイクロ波用磁性体は互いに別の部品として製造され、前記中心導体については、従来、銅箔をマイクロ波用磁性体に巻きつけたり、マイクロ波用磁性体に銀ペーストを印刷、焼結して一体的に形成するなど、様々な形態が提案されている。 Non-reciprocal circuit elements such as a circulator and an isolator include a central conductor having a plurality of electrode lines arranged in a state of being insulated from each other, a microwave magnetic body disposed in close contact with the central conductor, the central conductor and The central conductor assembly made of the magnetic material for microwaves includes a permanent magnet that applies a DC magnetic field, and the central conductor and the magnetic material for microwaves are manufactured as separate parts. Conventionally, various forms have been proposed, such as winding a copper foil around a microwave magnetic body, or printing and sintering a silver paste on the microwave magnetic body to form an integral body.
前述したような小型化の要求に応えるため、たとえば特許文献１に記載されるように、中心導体の材料として、パラジウムもしくは白金等の導電性粉末及び有機溶剤を混合してなる導電ペーストを用い、１３００〜１６００℃の温度で、マイクロ波用磁性体材料と中心導体とを一体焼成することが提案されている。
上述したパラジウムまたは白金は、融点が１３００℃以上と高く、ほとんどのマイクロ波用磁性体材料との一体焼成が容易であるという長所をもつ反面、比抵抗が高く、たとえばアイソレータ素子に使用した場合、挿入損失が大きくなるという欠点を有している。 The above-mentioned palladium or platinum has a high melting point of 1300 ° C. or higher and has an advantage that it can be easily fired integrally with most magnetic materials for microwaves, but has a high specific resistance. For example, when used for an isolator element, There is a disadvantage that the insertion loss is increased.
低抵抗の銀や銅を用いる場合、同時焼成可能なように、多結晶セラミック磁性材料にＢｉを置換したものを用いる場合がある。しかしながら、Ｂｉの酸化物は他の構成元素の酸化物に比べて低融点であり、結晶格子内に取り込まれずに粒界に異相として析出する場合があった。
一般に、ガーネットのように単相領域が狭いマイクロ波用磁性体材料は、異相の生成や空孔量の増加などが発生しやすいものであるが、Ｂｉは顕著であって、その異相の生成は、ガーネットの強磁性共鳴半値幅ΔＨや誘電損失ｔａｎδの増大を招く。また異なる色調のため外観状態においても好ましくは無い。
When low resistance silver or copper is used, a polycrystalline ceramic magnetic material in which Bi is substituted may be used so that simultaneous firing is possible. However, Bi oxide has a lower melting point than oxides of other constituent elements, and sometimes precipitates as a heterogeneous phase at the grain boundary without being taken into the crystal lattice.
In general, a microwave magnetic material with a narrow single-phase region, such as garnet, is prone to generation of a different phase or an increase in the amount of vacancies, but Bi is prominent. Garnet's ferromagnetic resonance half width ΔH and dielectric loss tan δ are increased. Moreover, it is not preferable in the appearance state due to the different color tone.
またマイクロ波用非可逆回路素子では永久磁石と組み合わせて使用されるが、マイクロ波用磁性体材料の飽和磁化４πＭｓの温度特性が、永久磁石の温度特性を補償することが理想とされる。 Further, although the microwave non-reciprocal circuit element is used in combination with a permanent magnet, it is ideal that the temperature characteristic of the saturation magnetization 4πMs of the microwave magnetic material compensates the temperature characteristic of the permanent magnet.
そこで本発明は、上述したような問題を解決し、しかも８６０℃以上９５０℃未満の低温で焼成することができ、Ｂｉ置換型においても異相の生成を抑え、強磁性共鳴半値幅ΔＨおよび誘電損失ｔａｎδが小さく、永久磁石の温度特性を補償するような温度係数αｍおよび飽和磁化４πＭｓを有する多結晶セラミック磁性体材料と、マイクロ波磁性体及びこれを用いた非可逆回路素子を提供することを目的とする。 Therefore, the present invention solves the above-described problems and can be fired at a low temperature of 860 ° C. or higher and lower than 950 ° C., suppresses the generation of heterogeneous phases even in the Bi substitution type, and reduces the ferromagnetic resonance half width ΔH and dielectric loss. An object is to provide a polycrystalline ceramic magnetic material having a small tan δ and a temperature coefficient αm and a saturation magnetization of 4πMs so as to compensate for the temperature characteristics of a permanent magnet, a microwave magnetic material, and a nonreciprocal circuit device using the same. And
第１の発明は、主成分が、一般式（Ｙ３．０−ｘ−ｙ−ｚＢｉｘＣａｙＧｄｚ）（Ｆｅ５−α−β−γＩｎαＡｌβＶγ）Ｏ１２で表される組成を有し、ｘ、ｙ、ｚの値が、０．５≦ｘ≦０．９、０．５≦ｙ≦０．９、０≦ｚ≦０．４であり、α、β、γの値が、０．０５≦α≦０．４、０≦β≦０．４５、０．２５≦γ≦０．４５の範囲内にあって、副成分としてＣｕとＺｒとＦｅを含み、その含有量は、前記主成分１００重量部に対して、ＣｕをＣｕＯ換算で０．１重量％≦ＣｕＯ≦０．５重量％、ＺｒをＺｒＯ２換算で０．０５重量％≦ＺｒＯ２≦０．５重量％、ＦｅをＦｅ２Ｏ３換算で０重量％＜Ｆｅ２Ｏ３≦１．０重量％でることを特徴とする多結晶セラミック磁性体材料である。 The first invention, the table in the main component is represented by the general formula (Y 3.0-x-y- z Bi x Ca y Gd z) (Fe 5-α-β-γ In α Al β V γ) O 12 And the values of x, y, z are 0.5 ≦ x ≦ 0.9, 0.5 ≦ y ≦ 0.9, 0 ≦ z ≦ 0.4, and α, β, The value of γ is in the range of 0.05 ≦ α ≦ 0.4, 0 ≦ β ≦ 0.45, 0.25 ≦ γ ≦ 0.45, and contains Cu, Zr and Fe as subcomponents, The content of Cu is 0.1 wt% ≦ CuO ≦ 0.5 wt% in terms of CuO and Zr is 0.05 wt% ≦ ZrO 2 ≦ 0 in terms of ZrO 2 with respect to 100 parts by weight of the main component. A polycrystalline ceramic magnetic material characterized by 0.5 wt% and Fe in terms of Fe 2 O 3 0 wt% <Fe 2 O 3 ≦ 1.0 wt%.
本発明に係る多結晶セラミック磁性体材料は、飽和磁化４πＭｓが７０ｍＴ〜１１０ｍＴであり、その温度係数αｍが、−０．３５％／℃〜−０．２１％／℃であり、強磁性共鳴半値幅ΔＨが８０００Ａ／ｍ以下であることも特徴とする。 The polycrystalline ceramic magnetic material according to the present invention has a saturation magnetization 4πMs of 70 mT to 110 mT and a temperature coefficient αm of −0.35% / ° C. to −0.21% / ° C. It is also characterized in that the value width ΔH is 8000 A / m or less.
第２の発明は、第１の発明の多結晶セラミック磁性体材料と、Ａｇ、Ａｇ合金のいずれかを含む導体ペーストとを一体焼結してなるマイクロ波磁性体であって、前記マイクロ波磁性体の内部及び／又は表面に前記導体ペーストで形成された電極パターンを備えることを特徴とするマイクロ波磁性体である。 A second invention is a microwave magnetic body obtained by integrally sintering the polycrystalline ceramic magnetic material of the first invention and a conductor paste containing either Ag or an Ag alloy, and the microwave magnetism A microwave magnetic body comprising an electrode pattern formed of the conductive paste inside and / or on the surface of a body.
第３の発明は、第２の発明のマイクロ波磁性体に形成された電極パターンを中心導体とし、前記中心導体に接続するコンデンサと、前記マイクロ波磁性体に直流磁界を与えるフェライト磁石を備えたことを特徴とする非可逆回路素子である。 According to a third aspect of the present invention, there is provided a capacitor connected to the central conductor, the electrode pattern formed on the microwave magnetic body according to the second aspect of the invention, and a ferrite magnet that applies a DC magnetic field to the microwave magnetic body. This is a non-reciprocal circuit device.
前記フェライト磁石は、残留磁束密度Ｂｒが４２０ｍＴ以上であり、その温度係数が−０．１５％／℃〜−０．２５％／℃であることが好ましい。 The ferrite magnet preferably has a residual magnetic flux density Br of 420 mT or more and a temperature coefficient of −0.15% / ° C. to −0.25% / ° C.
本発明によれば、８６０℃以上９５０℃未満の低温で焼成することができ、銀や銅といった低抵抗の金属材料との同時焼成が可能で、Ｂｉ置換型においても異相の生成がなく、強磁性共鳴半値幅ΔＨおよび誘電損失ｔａｎδが小さい多結晶セラミック磁性体材料と、マイクロ波磁性体及びこれを用いた非可逆回路素子を提供することが出来る。 According to the present invention, firing can be performed at a low temperature of 860 ° C. or more and less than 950 ° C., and simultaneous firing with a low-resistance metal material such as silver or copper is possible. A polycrystalline ceramic magnetic material having a small magnetic resonance half width ΔH and a dielectric loss tan δ, a microwave magnetic material, and a nonreciprocal circuit device using the same can be provided.
本発明の多結晶セラミック磁性体材料は、主成分が、一般式（Ｙ３．０−ｘ−ｙ−ｚＢｉｘＣａｙＧｄｚ）（Ｆｅ５−α−β−γＩｎαＡｌβＶγ）Ｏ１２で表される組成を有し、ｘ、ｙ、ｚの値が、０．５≦ｘ≦０．９、０．５≦ｙ≦０．９、０≦ｚ≦０．４であり、α、β、γの値が、０．０５≦α≦０．４、０≦β≦０．４５、０．２５≦γ≦０．４５の範囲内にあって、副成分としてＣｕとＺｒとＦｅを含み、その含有量は、前記主成分１００重量部に対して、ＣｕをＣｕＯ換算で０．１重量％≦ＣｕＯ≦０．５重量％、ＺｒをＺｒＯ２換算で０．０５重量％≦ＺｒＯ２≦０．５重量％であり、ＦｅをＦｅ２Ｏ３換算で０重量％＜Ｆｅ２Ｏ３≦１．０重量％の範囲内にあって、ガーネット構造を有する相を主成分とし、８６０℃以上９５０℃以下の温度で焼結することを特徴とする多結晶セラミック磁性体材料である。 Polycrystalline ceramic magnetic material of the present invention, the main component is represented by the general formula (Y 3.0-x-y- z Bi x Ca y Gd z) (Fe 5-α-β-γ In α Al β V γ ) Having a composition represented by O 12 , and the values of x, y, and z are 0.5 ≦ x ≦ 0.9, 0.5 ≦ y ≦ 0.9, and 0 ≦ z ≦ 0.4 , Α, β, γ are in the range of 0.05 ≦ α ≦ 0.4, 0 ≦ β ≦ 0.45, 0.25 ≦ γ ≦ 0.45, and Cu and Zr as subcomponents And Fe, and the content of Cu is 0.1 wt% ≦ CuO ≦ 0.5 wt% in terms of CuO and Zr is 0.05 wt% in terms of ZrO 2 with respect to 100 parts by weight of the main component. ≦ ZrO a 2 ≦ 0.5% by weight, there the Fe 0 wt% in terms of Fe 2 O 3 <within the scope of the Fe 2 O 3 ≦ 1.0 wt%, the main component phase having a garnet structure , At 60 ° C. or higher 950 ° C. temperature below a polycrystalline ceramic magnetic material, characterized by sintering.
焼結温度、強磁性共鳴半値幅ΔＨ、誘電損失ｔａｎδ、飽和磁化４πＭｓ、飽和磁化４πＭｓの温度特性等は、多結晶セラミック磁性体材料の主成分組成により大きく影響され、主成分組成が上記の本発明の組成範囲から外れると以下のような不具合が生じる。 The temperature characteristics of the sintering temperature, the ferromagnetic resonance half width ΔH, the dielectric loss tan δ, the saturation magnetization 4πMs, the saturation magnetization 4πMs are greatly influenced by the main component composition of the polycrystalline ceramic magnetic material. If the composition falls outside the composition range of the invention, the following problems occur.
Ｂｉは低温焼結化に寄与する。ｘが、ｘ＜０．５であると、異相の生成は抑制されるが９５０℃未満での焼結が困難になる。また、ｘ＞０．９であると、８６０℃以上９５０℃未満での焼結は可能になるが、焼結体に異相が生じ易く誘電損失ｔａｎδがｔａｎδ＞１０×１０−４および強磁性共鳴半値幅ΔＨがΔＨ＞８０００（Ａ／ｍ）と著しく大きくなる。このため、ｘは０．５≦ｘ≦０．９であることが望ましい。好ましくは、０．５５≦ｘ≦０．７５である。 Bi contributes to low temperature sintering. When x is x <0.5, the formation of heterogeneous phases is suppressed, but sintering at less than 950 ° C. becomes difficult. Further, when x> 0.9, sintering at 860 ° C. or more and less than 950 ° C. is possible, but a heterogeneous phase is likely to occur in the sintered body, and dielectric loss tan δ is tan δ> 10 × 10 −4 and ferromagnetic resonance. The half-value width ΔH is remarkably increased as ΔH> 8000 (A / m). For this reason, x is preferably 0.5 ≦ x ≦ 0.9. Preferably, 0.55 ≦ x ≦ 0.75.
Ｃａは後述するＶとともに加えられ、焼結時に低融点のＶの蒸散を防ぐのに寄与する。このような効果を発揮させるには、ｙは０．５≦ｙ≦０．９とするのが好ましい。 Ca is added together with V described later, and contributes to preventing the low melting point V from evaporating during sintering. In order to exhibit such an effect, y is preferably set to 0.5 ≦ y ≦ 0.9.
Ｇｄは飽和磁化４πＭｓの温度係数αｍの調整に寄与する。ｚが、０．４を超えると、−２０から６０℃までの飽和磁化４πＭｓの温度係数αｍが、αｍ＜−０．２１（％／℃）となる場合があり、永久磁石との温度特性を補償することができない。また誘電損失ｔａｎδがｔａｎδ≧１０×１０−４、および、強磁性共鳴半値幅ΔＨがΔＨ＞８０００（Ａ／ｍ）と著しく大きくなる。このため、ｚは０≦ｚ≦０．４であることが望ましい。 Gd contributes to the adjustment of the temperature coefficient αm of the saturation magnetization 4πMs. If z exceeds 0.4, the temperature coefficient αm of saturation magnetization 4πMs from −20 to 60 ° C. may be αm <−0.21 (% / ° C.), and the temperature characteristics with the permanent magnet It cannot be compensated. Further, the dielectric loss tan δ is remarkably increased as tan δ ≧ 10 × 10 −4 and the ferromagnetic resonance half width ΔH is ΔH> 8000 (A / m). For this reason, z is preferably 0 ≦ z ≦ 0.4.
Ｉｎ，Ａｌ，Ｖは飽和磁化４πＭｓの温度係数αｍの調整、低温焼結化に寄与する。α、β、γの値を、それぞれ０．０５≦α≦０．４、０≦β≦０．４５、０．２５≦γ≦０．４５の範囲内とするのが好ましい。Ｉｎ，Ａｌ，Ｖが上記範囲よりも少ないと９５０℃未満での焼結が困難になる。また前記範囲よりも少ないと、飽和磁化４πＭｓが４πＭｓ＞１１０（ｍＴ）となり、所定の形状による永久磁石の磁力が不足してしまう。また誘電損失ｔａｎδがｔａｎδ≧１０×１０−４、および、強磁性共鳴半値幅ΔＨがΔＨ＞８０００（Ａ／ｍ）と著しく大きくなる。また多い場合には、飽和磁化４πＭｓが４πＭｓ＜７０（ｍＴ）となり、永久磁石との温度特性を補償することができない。 In, Al, and V contribute to the adjustment of the temperature coefficient αm of the saturation magnetization 4πMs and the low-temperature sintering. The values of α, β, and γ are preferably set in the ranges of 0.05 ≦ α ≦ 0.4, 0 ≦ β ≦ 0.45, and 0.25 ≦ γ ≦ 0.45, respectively. When In, Al, and V are less than the above ranges, sintering at less than 950 ° C. becomes difficult. If the amount is less than the above range, the saturation magnetization 4πMs becomes 4πMs> 110 (mT), and the magnetic force of the permanent magnet having a predetermined shape is insufficient. Further, the dielectric loss tan δ is remarkably increased as tan δ ≧ 10 × 10 −4 and the ferromagnetic resonance half width ΔH is ΔH> 8000 (A / m). In many cases, the saturation magnetization 4πMs is 4πMs <70 (mT), and the temperature characteristics with the permanent magnet cannot be compensated.
また、本発明の多結晶セラミック磁性体材料における副成分は、異相の抑制、低温焼結化に寄与するが、組成が上記の本発明の組成範囲から外れると、以下のような不具合が生じる。 Further, the subcomponent in the polycrystalline ceramic magnetic material of the present invention contributes to the suppression of heterogeneous phase and low temperature sintering, but the following problems occur when the composition is out of the composition range of the present invention.
まず、ＣｕＯが主成分に対して０．５重量％より大きいと、低温での焼結は可能になるが誘電損失ｔａｎδがｔａｎδ≧１０×１０−４、および、強磁性共鳴半値幅ΔＨがΔＨ＞８０００（Ａ／ｍ）と著しく大きくなる。０重量％であると９５０℃未満での焼結が困難になる。このため、ＣｕＯは主成分に対して０．１重量％≦ＣｕＯ≦０．５重量％であることが望ましい。好ましくは、０．２重量％≦ＣｕＯ≦０．４重量％である。 First, when CuO is larger than 0.5% by weight with respect to the main component, sintering at low temperature becomes possible, but dielectric loss tan δ is tan δ ≧ 10 × 10 −4 , and ferromagnetic resonance half width ΔH is ΔH. > 8000 (A / m). If it is 0% by weight, sintering at less than 950 ° C. becomes difficult. For this reason, it is desirable that CuO is 0.1 wt% ≦ CuO ≦ 0.5 wt% with respect to the main component. Preferably, 0.2 wt% ≦ CuO ≦ 0.4 wt%.
また、ＺｒＯ２が主成分に対して０．５０重量％より大きいと、焼結体に異相を生じやすく強磁性共鳴半値幅ΔＨがΔＨ＞８０００（Ａ／ｍ）と著しく大きくなる。０重量％であると誘電損失ｔａｎδがｔａｎδ≧１０×１０−４、および、強磁性共鳴半値幅ΔＨがΔＨ＞８０００（Ａ／ｍ）と大きくなる。このため、ＺｒＯ２は主成分に対して０．０５重量％≦ＺｒＯ２≦０．５０重量％であることが望ましい。好ましくは、０．０７重量％≦ＺｒＯ２≦０．２０重量％である。 On the other hand, if ZrO 2 is larger than 0.50% by weight with respect to the main component, a heterogeneous phase is likely to be generated in the sintered body, and the ferromagnetic resonance half width ΔH becomes remarkably large as ΔH> 8000 (A / m). When the content is 0% by weight, the dielectric loss tan δ increases as tan δ ≧ 10 × 10 −4 , and the ferromagnetic resonance half width ΔH increases as ΔH> 8000 (A / m). For this reason, it is desirable that ZrO 2 is 0.05 wt% ≦ ZrO 2 ≦ 0.50 wt% with respect to the main component. Preferably, 0.07 wt% ≦ ZrO 2 ≦ 0.20 wt%.
また、Ｆｅ２Ｏ３が主成分に対して１．０重量％より大きいと、低温での焼結は可能になるが強磁性共鳴半値幅ΔＨがΔＨ＞８０００（Ａ／ｍ）と著しく大きくなる。またイットリウム（Ｙ）サイトのＢｉによる異相の生成は抑制されるが、鉄（Ｆｅ）サイトの異相が発生しやすくΔＨ＞８０００（Ａ／ｍ）と著しく大きくなる。 On the other hand, if Fe 2 O 3 is larger than 1.0% by weight with respect to the main component, sintering at a low temperature becomes possible, but the ferromagnetic resonance half width ΔH becomes remarkably large as ΔH> 8000 (A / m). . Further, although the generation of a heterogeneous phase due to Bi at the yttrium (Y) site is suppressed, the heterogeneous phase at the iron (Fe) site is likely to occur, and ΔH> 8000 (A / m) is significantly increased.
上記の成分組成により、８６０℃以上９５０℃以下の低温で焼結することができ、飽和磁化４πＭｓが７０ｍＴ〜１１０ｍＴであり、その温度係数αｍが、−０．３５％／℃〜−０．２１％／℃であり、強磁性共鳴半値幅ΔＨが８０００Ａ／ｍ以下の多結晶セラミック磁性体材料を得ることができる。
従って、本発明の多結晶セラミック磁性体材料は、銀や銅といった高い導電率を有する金属材料を内部電極として用い、一体焼結を行うことができる。よって、磁性体材料の有する高いＱ値と、内部電極の電気抵抗による損失を抑え、極めて損失の小さいマイクロ波磁性体を構成することができる。これにより、アイソレータ、サーキュレータなどのマイクロ波非可逆回路素子に応用して、優れたマイクロ波特性と低損失を実現することができる。
With the above component composition, sintering can be performed at a low temperature of 860 ° C. or more and 950 ° C. or less, the saturation magnetization 4πMs is 70 mT to 110 mT, and the temperature coefficient αm is −0.35% / ° C. to −0.21. % / ° C., and a polycrystalline ceramic magnetic material having a ferromagnetic resonance half width ΔH of 8000 A / m or less can be obtained.
Therefore, the polycrystalline ceramic magnetic material of the present invention can be integrally sintered using a metal material having a high conductivity such as silver or copper as an internal electrode. Therefore, it is possible to suppress a loss due to the high Q value of the magnetic material and the electric resistance of the internal electrode, and to construct a microwave magnetic body with extremely small loss. As a result, it can be applied to microwave nonreciprocal circuit elements such as isolators and circulators to achieve excellent microwave characteristics and low loss.
以下、実施例について詳細に説明する。
出発原料として純度９９．０％以上の酸化ガドリニウム（Ｇｄ２Ｏ３）、酸化イットリウム（Ｙ２Ｏ３）、炭酸カルシウム（ＣａＣＯ３）、酸化ビスマス（Ｂｉ２Ｏ３）、酸化鉄（Ｆｅ２Ｏ３）、酸化インジウム（Ｉｎ２Ｏ３）、酸化バナジウム（Ｖ２Ｏ５）および酸化アルミニウム（Ａｌ２Ｏ３）を用意し、これらを表１に示す組成比率になるように秤量し、スラリー濃度４０％となるようにイオン交換水を加え、ボールミルにて２５時間から４５時間湿式混合し、その後、乾燥した。この乾燥した粉末に対して８００℃から８７５℃の温度で１．５時間から２時間保持して仮焼を行った。なお仮焼は、後工程である焼結工程での焼結温度よりも４０℃〜７０℃低温に設定される。
Hereinafter, examples will be described in detail.
Starting materials of gadolinium oxide (Gd 2 O 3 ), yttrium oxide (Y 2 O 3 ), calcium carbonate (CaCO 3 ), bismuth oxide (Bi 2 O 3 ), iron oxide (Fe 2 O) having a purity of 99.0% or more 3 ), indium oxide (In 2 O 3 ), vanadium oxide (V 2 O 5 ), and aluminum oxide (Al 2 O 3 ) were prepared and weighed so that the composition ratios shown in Table 1 were obtained, and the slurry concentration Ion exchange water was added so that it might become 40%, and it wet-mixed with the ball mill for 25 to 45 hours, and dried after that. The dried powder was calcined by holding at a temperature of 800 ° C. to 875 ° C. for 1.5 hours to 2 hours. In addition, calcination is set to 40 to 70 degreeC low temperature rather than the sintering temperature in the sintering process which is a post process.
次に、副成分として酸化銅（ＣｕＯ）、酸化ジルコニウム（ＺｒＯ２）、酸化鉄（Ｆｅ２Ｏ３）を用意し、上記のようにして得た母材粉末に対して、これらを表１に示す組成比率になるように秤量し加え、スラリー濃度４０％となるようにイオン交換水を加え、ボールミルにて２０から３０時間湿式粉砕し、その後、乾燥して磁性体磁器組成物を得た。なお上記のようにして得られた粉末の平均粒径は０．２５μｍから１．５μｍとなるように調整した。副成分の添加は、主成分秤量時に添加しても同様の効果が得られた。 Next, copper oxide (CuO), zirconium oxide (ZrO 2 ), and iron oxide (Fe 2 O 3 ) are prepared as subcomponents, and these are shown in Table 1 for the base material powder obtained as described above. Weighed and added to the composition ratio shown, added ion-exchanged water to a slurry concentration of 40%, wet crushed with a ball mill for 20 to 30 hours, and then dried to obtain a magnetic ceramic composition. The average particle size of the powder obtained as described above was adjusted to 0.25 μm to 1.5 μm. Even when the auxiliary component was added at the time of weighing the main component, the same effect was obtained.
次に、上記のようにして得られた磁性体磁器組成物にバインダー水溶液を添加混錬して得た造粒粉末を、１ｔｏｎ／ｃｍ２から２ｔｏｎ／ｃｍ２の圧力で加圧して成形体とした。これを空気中において表１に示す焼成温度で５時間焼成し、焼結体を得た。 Then, the granulated powder obtained by adding and kneading a binder solution in the magnetic ceramic composition obtained as described above, the molded body under pressure at a pressure from 1 ton / cm 2 of 2 ton / cm 2 did. This was fired in air at the firing temperature shown in Table 1 for 5 hours to obtain a sintered body.
次に、得られた焼結体を用いて誘電体円柱共振器を作製し、ハッキ・コールマン法により、誘電損失ｔａｎδを測定した。また、評価用試料の飽和磁化Ｍｓは振動型磁力計を用いて測定した。さらに得られた焼結体を０．１５ｍｍから０．２５ｍｍの厚さに薄円板状に加工し、短絡同軸線路法により強磁性共鳴半値幅ΔＨを測定した。この結果を表１に示す。なお焼成温度は焼結体が緻密化した温度であって、焼結体密度と焼成温度との関係において、焼結体密度が焼成温度に対して実質的に変化を示さなくなる温度である。 Next, a dielectric cylindrical resonator was fabricated using the obtained sintered body, and dielectric loss tan δ was measured by the Hack-Coleman method. Moreover, the saturation magnetization Ms of the sample for evaluation was measured using a vibration type magnetometer. Further, the obtained sintered body was processed into a thin disc shape with a thickness of 0.15 mm to 0.25 mm, and the ferromagnetic resonance half width ΔH was measured by a short-circuited coaxial line method. The results are shown in Table 1. The firing temperature is a temperature at which the sintered body is densified, and is a temperature at which the sintered body density does not substantially change with respect to the firing temperature in the relationship between the sintered body density and the firing temperature.
表１に示される＊印はこの発明範囲外の比較例であり、それ以外はすべてこの発明範囲内の実施例である。表１に示すとおり、試料Ｎｏ．１では異相の生成は抑制されたが０．５≦ｘ≦０．９０の範囲から外れるために９５０℃未満の焼成温度では、緻密な焼結体を得ることができなかった。試料Ｎｏ．２、３、４では、副成分であるＣｕとＺｒとＦｅがそれぞれＣｕをＣｕＯ換算で０．１重量％≦ＣｕＯ≦０．５重量％、ＺｒをＺｒＯ２換算で０．０５重量％≦ＺｒＯ２≦０．５重量％、ＦｅをＦｅ２Ｏ３換算で０重量％＜Ｆｅ２Ｏ３≦１．０重量％の範囲から外れるために、イットリウム（Ｙ）サイトのＢｉによる異相が生成され、誘電損失ｔａｎδが１０×１０−４を超えるとともに、磁性共鳴半値幅ΔＨが８０００Ａ／ｍを超えた。試料Ｎｏ．８、１２では、副成分であるＦｅがＦｅ２Ｏ３換算で０重量％＜Ｆｅ２Ｏ３≦１．０重量％の範囲から外れるために、鉄（Ｆｅ）サイトの異相が発生し、磁性共鳴半値幅ΔＨが８０００Ａ／ｍを超えた。
The asterisks shown in Table 1 are comparative examples outside the scope of the invention, and all other examples are examples within the scope of the invention. As shown in Table 1, Sample No. In Example 1, the generation of heterogeneous phases was suppressed, but out of the range of 0.5 ≦ x ≦ 0.90, so that a dense sintered body could not be obtained at a firing temperature of less than 950 ° C. Sample No. In 2, 3, and 4, the subcomponents Cu, Zr and Fe are each 0.1% by weight ≦ CuO ≦ 0.5% by weight in terms of CuO and Zr is 0.05% by weight ≦ ZrO in terms of ZrO 2. 2 ≦ 0.5 wt%, 0 wt% of Fe in terms of Fe 2 O 3 <to deviate from Fe 2 O 3 ≦ 1.0 wt% range, different phase by Bi yttrium (Y) sites is generated, The dielectric loss tan δ exceeded 10 × 10 −4 and the magnetic resonance half width ΔH exceeded 8000 A / m. Sample No. In 8, 12 to a by-component Fe is out of Fe 2 O 3 0% by weight in terms of <Fe 2 O 3 ≦ 1.0 wt% range, different phase is generated iron (Fe) site, magnetic The resonance half width ΔH exceeded 8000 A / m.
本発明の範囲内の実施例においては、共に８６０℃以上９５０℃未満の温度で緻密な焼結体を得ることができ、かつ誘電損失ｔａｎδがｔａｎδ≦１０×１０−４および強磁性共鳴半値幅ΔＨがΔＨ＜８０００（Ａ／ｍ）となる。また、−２０から６０℃までの飽和磁化４πＭｓの温度係数αｍが、−０．３５％／℃〜−０．２１％／℃となり、永久磁石との温度特性を補償することができる。また、副成分としてＦｅがＦｅ２Ｏ３換算で０重量％＜Ｆｅ２Ｏ３≦１．０重量％添加されることで、イットリウム（Ｙ）サイトのＢｉによる異相の生成が抑制される。 In the examples within the scope of the present invention, a dense sintered body can be obtained at a temperature of 860 ° C. or more and less than 950 ° C., and the dielectric loss tan δ is tan δ ≦ 10 × 10 −4 and the ferromagnetic resonance half width. ΔH is ΔH <8000 (A / m). Further, the temperature coefficient αm of the saturation magnetization 4πMs from −20 to 60 ° C. becomes −0.35% / ° C. to −0.21% / ° C., and the temperature characteristics with the permanent magnet can be compensated. Further, the addition of 0% by weight <Fe 2 O 3 ≦ 1.0% by weight in terms of Fe 2 O 3 as an accessory component suppresses the generation of a heterogeneous phase due to Bi at the yttrium (Y) site.
本発明に係る多結晶セラミック磁性体材料からなるマイクロ波磁性体と、それを用いた非可逆回路素子について説明する。図１は、この発明の一実施例に用いたマイクロ波磁性体（中心導体組立体）の外観を示す斜視図である。図２は前記中心導体組立体の分解斜視図であり、図３は本発明の一実施例に係る非可逆回路素子の分解斜視図である。
この非可逆回路素子の基本構成としては、中心導体組立体４、中央部の透孔の中に前記中心導体組立体４を組み込むようになしたコンデンサ積層体５、このコンデンサ積層体５に組み入れられるチップあるいは抵抗膜で形成した抵抗体９０、中心導体組立体４に直流磁界を印加する永久磁石３、磁性ヨークを兼ねる金属製の上ケース１と同じく下ケース２とからなっている。コンデンサ積層体５と下ケース２との間に、実装基板との接続端子を備え、中心導体組立体４とコンデンサ積層体５を接続する接続電極を備えた樹脂ベース６を配置している。
A microwave magnetic material made of a polycrystalline ceramic magnetic material according to the present invention and a nonreciprocal circuit device using the same will be described. FIG. 1 is a perspective view showing the appearance of a microwave magnetic body (central conductor assembly) used in one embodiment of the present invention. FIG. 2 is an exploded perspective view of the central conductor assembly, and FIG. 3 is an exploded perspective view of a non-reciprocal circuit device according to an embodiment of the present invention.
As the basic configuration of the nonreciprocal circuit element, a
前記中心導体組立体４は、相対向する第１および第２の主面と当該主面間を連結する側面を備えた矩形状のマイクロ波磁性体に中心導体を積層配置するものである。
この中心導体組立体４の作製工程は次の通りである。まず、Ｂｉ２Ｏ３、Ｙ２Ｏ３、ＣａＣＯ３、Ｆｅ２Ｏ３、Ｉｎ２Ｏ３、Ｖ２Ｏ５を出発原料として、主成分が一般式（Ｙ１．５３Ｂｉ０．６５Ｃａ０．８２）（Ｆｅ４．０３Ｉｎ０．２６Ａｌ０．３０Ｖ０．４１）Ｏ１２（原子％）（試料Ｎｏ．９）となるように秤量し、前記出発原料をボールミルにて湿式混合し、得られたスラリーを乾燥した後、８５０℃の温度で仮焼し、ボールミルにて湿式粉砕した。
次に、副成分として酸化銅（ＣｕＯ）、酸化ジルコニウム（ＺｒＯ２）、酸化鉄（Ｆｅ２Ｏ３）を用意し、上記のようにして得た母材粉末１００重量部に対して、ＣｕＯ ０．２０重量％、ＺｒＯ２ ０．１０重量％、Ｆｅ２Ｏ３ ０．３０重量％になるように秤量し加え、スラリー濃度４０％となるようにイオン交換水を加え、ボールミルにて２０から３０時間湿式粉砕し、その後、乾燥して多結晶セラミック磁性体材料を得た。なお上記のようにして得られた粉末の平均粒径は０．２５μｍから１．５μｍとなるように調整した。
この磁性材料粉末と有機バインダー、可塑材、および、有機溶剤をボールミルにて混合し粘度を調整した後、ドクターブレード法にて４０μｍ〜１５０μｍの磁性体セラミックグリーンシートを作製した。
The
The manufacturing process of the
Next, copper oxide (CuO), zirconium oxide (ZrO 2 ), and iron oxide (Fe 2 O 3 ) were prepared as subcomponents, and CuO 0 with respect to 100 parts by weight of the base material powder obtained as described above. 20% by weight, ZrO 2 0.10% by weight, Fe 2 O 3 0.30% by weight, and ion-exchanged water was added so that the slurry concentration was 40%. Wet milled for a period of time and then dried to obtain a polycrystalline ceramic magnetic material. The average particle size of the powder obtained as described above was adjusted to 0.25 μm to 1.5 μm.
The magnetic material powder, an organic binder, a plasticizer, and an organic solvent were mixed by a ball mill to adjust the viscosity, and then a magnetic ceramic green sheet having a thickness of 40 μm to 150 μm was prepared by a doctor blade method.
得られたセラミックグリーンシートに、φ０．１〜φ０．４のビアホール（図中、黒丸で表示）をレーザ加工にて形成し、中心導体となる導電性ペーストを印刷し、さらにグリーンシートを重ねて８０℃に加熱して１２ＭＰａの圧力で熱圧着して積層体とした後、所定の大きさ、形状となるように、例えばダイシングソーや鋼刃で前記積層体を切断した後、９２０℃で、８時間焼成した。前記ビアホールには、Ａｇ導体が充填されており、各中心導体４４ａ〜４４ｃとグランド電極Ｇｎｄ、入出力電極Ｉｎ、Ｏｕｔ、Ｌｏａｄを接続している。このようにして、中心導体４４ａ〜４４ｃが互いに絶縁を保って等角度で交差し、第２の主面４３ｆにグランド電極ＧＮＤと入出力電極Ｉｎ、Ｏｕｔ、ＬｏａｄをＬＧＡ（Ｌａｎｄ Ｇｒｉｄ Ａｒｒａｙ）として備える中心導体組立体４を得た。
Via holes of φ0.1 to φ0.4 (indicated by black circles in the figure) are formed by laser processing on the obtained ceramic green sheet, and a conductive paste serving as a central conductor is printed, and the green sheets are further stacked. After heating to 80 ° C. and thermocompression bonding at a pressure of 12 MPa to form a laminate, after cutting the laminate with, for example, a dicing saw or steel blade so as to have a predetermined size and shape, at 920 ° C., Baked for 8 hours. The via hole is filled with an Ag conductor, and the
前記コンデンサ積層体５は、その上面および積層体内部には整合容量を形成するための入力容量電極Ｃ１、出力容量電極Ｃ２、ロード容量電極Ｃ３と、終端抵抗９０が配置されるグランド電極Ｇｎｄが形成されている。また、コンデンサ積層体５の裏面には樹脂ベース６に対して電気的に接続するための入出力電極Ｉｎ、Ｏｕｔ、Ｌｏａｄ、グランド電極Ｇｎｄがそれぞれ設けられている。
The capacitor laminate 5 has an input capacitance electrode C1, an output capacitance electrode C2, a load capacitance electrode C3 for forming a matching capacitance, and a ground electrode Gnd on which a
前記樹脂ベース６は、例えば０．１ｍｍ厚さの銅板を用い、射出成形によりこの銅板と液晶ポリマーを一体成形して製造される。この樹脂ベース６の上面、すなわちコンデンサ積層体５との接続面側には、接続電極Ｉｎ、Ｏｕｔ、Ｌｏａｄ、ＧＮＤが導体板で形成され、樹脂部分を含めて平面状に構成されている。しかも、接続電極Ｉｎ、Ｏｕｔ、Ｌｏａｄ、ＧＮＤは同一平面上に形成され、接続電極ＧＮＤ、Ｌｏａｄと端子Ｇ、接続電極Ｉｎ、Ｏｕｔは端子電極Ｐ１、Ｐ２と、それぞれ同一の導体板で構成され、電気的に接続している。 The resin base 6 is manufactured by, for example, using a copper plate having a thickness of 0.1 mm and integrally molding the copper plate and the liquid crystal polymer by injection molding. On the upper surface of the resin base 6, that is, on the connection surface side with the capacitor laminate 5, connection electrodes In, Out, Load, and GND are formed of a conductor plate, and are configured in a planar shape including the resin portion. In addition, the connection electrodes In, Out, Load, GND are formed on the same plane, the connection electrodes GND, Load and the terminal G, and the connection electrodes In, Out are configured by the same conductor plate, respectively, as the terminal electrodes P1, P2. Electrically connected.
永久磁石は、日立金属株式会社製のＬａ−Ｃｏ置換フェライト磁石ＹＢＭ−９ＢＥを方形に形成したものを用いた。この永久磁石は、残留磁束が４３０ｍＴから４５０ｍＴであり、残留磁束密度の温度係数が−０．２０％〜−０．１８％である。なお、永久磁石の形状については。円盤状、六角形など任意の形状のものを採用し得る。このことは、ガーネットの形状についても同様である。 As the permanent magnet, a La-Co substituted ferrite magnet YBM-9BE manufactured by Hitachi Metals, Ltd., which was formed in a square shape was used. This permanent magnet has a residual magnetic flux of 430 mT to 450 mT, and a temperature coefficient of the residual magnetic flux density of −0.20% to −0.18%. About the shape of the permanent magnet. Arbitrary shapes such as a disk shape and a hexagonal shape can be adopted. The same applies to the shape of the garnet.
得られた中心導体組立体４をコンデンサ積層体５の透孔内に配置した後、樹脂ベース６の接続電極を介して接続し、中心導体組立体４の上側に永久磁石３を配置し、これらを上ケース１と下ケース２で覆って非可逆回路素子とした。本発明の非可逆回路素子の挿入損失について温度特性を評価したが、温度変化にともなう挿入損失が最小となる周波数の変動が小さく、優れた温度特性を備えた非可逆回路素子が得られた。
After the obtained
本発明によれば、８６０℃以上９５０℃未満の低温で焼成することができ、銀や銅といった低抵抗の金属材料との同時焼成が可能で、Ｂｉ置換型においても異相の生成がなく強磁性共鳴半値幅ΔＨおよび誘電損失ｔａｎδが小さい多結晶セラミック磁性体材料と、マイクロ波磁性体及びこれを用いた非可逆回路素子を提供することが出来る。これにより、サーキュレータ、アイソレータなどのマイクロ波非可逆回路素子に応用して、優れたマイクロ波特性と低損失を実現することができる。 According to the present invention, firing can be performed at a low temperature of 860 ° C. or more and less than 950 ° C., and simultaneous firing with a low-resistance metal material such as silver or copper is possible. A polycrystalline ceramic magnetic material having a small resonance half width ΔH and dielectric loss tan δ, a microwave magnetic material, and a nonreciprocal circuit device using the same can be provided. As a result, it can be applied to microwave nonreciprocal circuit elements such as circulators and isolators to realize excellent microwave characteristics and low loss.
１ 上ケース
２ 下ケース
３ 永久磁石
４ 中心導体組立体
５ コンデンサ積層体
６ 樹脂ベース
４４ａ〜４４ｃ 中心導体
DESCRIPTION OF SYMBOLS 1 Upper case 2
Claims (5)
ｘ、ｙ、ｚの値が、０．５≦ｘ≦０．９、０．５≦ｙ≦０．９、０≦ｚ≦０．４であり、
α、β、γの値が、０．０５≦α≦０．４、０≦β≦０．４５、０．２５≦γ≦０．４５の範囲内にあって、副成分としてＣｕとＺｒとＦｅを含み、その含有量は、前記主成分１００重量部に対して、ＣｕをＣｕＯ換算で０．１重量％≦ＣｕＯ≦０．５重量％、ＺｒをＺｒＯ２換算で０．０５重量％≦ＺｒＯ２≦０．５重量％、ＦｅをＦｅ２Ｏ３換算で０重量％＜Ｆｅ２Ｏ３≦１．０重量％であることを特徴とする多結晶セラミック磁性体材料。 Main component, the general formula (Y 3.0-x-y- z Bi x Ca y Gd z) (Fe 5-α-β-γ In α Al β V γ) has a composition represented by O 12 ,
the values of x, y, z are 0.5 ≦ x ≦ 0.9, 0.5 ≦ y ≦ 0.9, 0 ≦ z ≦ 0.4,
The values of α, β, and γ are in the range of 0.05 ≦ α ≦ 0.4, 0 ≦ β ≦ 0.45, 0.25 ≦ γ ≦ 0.45, and Cu and Zr as subcomponents Fe is included, and the content thereof is 0.1 wt% ≦ CuO ≦ 0.5 wt% in terms of CuO, and 0.05 wt% ≦ Zr in terms of ZrO 2 with respect to 100 parts by weight of the main component. polycrystalline ceramic magnetic material, characterized in that ZrO 2 ≦ 0.5 wt%, 0 wt% of Fe in terms of Fe 2 O 3 <Fe 2 O 3 ≦ 1.0% by weight.
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