JP6722684B2 - 極超短波用MOドープCo2Z型フェライト複合材料 - Google Patents
極超短波用MOドープCo2Z型フェライト複合材料 Download PDFInfo
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- JP6722684B2 JP6722684B2 JP2017540229A JP2017540229A JP6722684B2 JP 6722684 B2 JP6722684 B2 JP 6722684B2 JP 2017540229 A JP2017540229 A JP 2017540229A JP 2017540229 A JP2017540229 A JP 2017540229A JP 6722684 B2 JP6722684 B2 JP 6722684B2
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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- C—CHEMISTRY; METALLURGY
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Description
1. 鉄、コバルト、バリウムおよびストロンチウムの一方または両方、ならびにモリブデンを含むヘキサフェライト組成物であって、式
(BazSr(3−z))Co(2+x)MoxFe(y−2x)O41
(式中、
x=0.01〜0.20であり;
y=20〜24であり、
z=0〜3である)
を有する、Z型ヘキサフェライト相を備える、ヘキサフェライト組成物。
3. x=0.10〜0.12である、項目1または2に記載のヘキサフェライト組成物。
5. 0.1〜3.0GHzの周波数範囲にわたって少なくとも7.0の実数透磁率を有する、項目1〜4のいずれかに記載のヘキサフェライト組成物。
7. z=1.2〜3.0であり、かつヘキサフェライト組成物が、約0.1GHz〜少なくとも1.0GHzの周波数範囲にわたって8.0〜12.0の範囲の実数透磁率を有する、項目1〜6のいずれかに記載のヘキサフェライト組成物。
10. 0.1〜3.0GHzの周波数範囲にわたって少なくとも8.0の実数誘電率を有する、項目1〜9のいずれかに記載のヘキサフェライト組成物。
12. ヘキサフェライト組成物の実数誘電率が、10%以内でヘキサフェライト組成物の実数透磁率に等しい、項目1〜11のいずれかに記載のヘキサフェライト組成物。
14. 0.1〜0.8GHzの周波数で0.02未満の誘電損失正接tanδεを有する、項目1〜13のいずれかに記載のヘキサフェライト組成物。
16. 0.4GHzでおおよそ0.1の磁気損失正接tanδμを有する、項目1〜15のいずれかに記載のヘキサフェライト組成物。
る、項目1〜16のいずれかに記載のヘキサフェライト組成物。
18. 0.1〜3.5GHzの周波数で0.95未満の磁気損失正接tanδμを有する、項目1〜17のいずれかに記載のヘキサフェライト組成物。
21. 0.8GHzの周波数で0.03未満の磁気損失係数tanδμ/μ’を有する、項目1〜20のいずれかに記載のヘキサフェライト組成物。
23. アンテナ、フィルタ、インダクタ、サーキュレータ、または位相シフタである、項目22に記載の物品。
25. 0.1GHz以上の周波数で動作可能なアンテナである、項目24に記載の物品。
27. 0.1〜1.5GHzで動作可能なアンテナである、項目24に記載の物品。
29. 式
(BazSr(3−z))Co(2+x)MoxFe(y−2x)O41
(式中、
x=0.01〜0.20であり;
y=20〜24であり;
z=0〜3である)
を有するZ型ヘキサフェライト相を備える第2のヘキサフェライト組成物をさらに備え、
ここで、ヘキサフェライト組成物および第2のヘキサフェライト組成物中のBaの量およびSrの量が異なる、項目22〜28のいずれかに記載の物品。
31. ヘキサフェライト組成物が、約0.1GHz〜少なくとも1.0GHzの周波数範囲にわたって8.0〜12.0の範囲の実数透磁率を有し、かつ第2のヘキサフェライト組成物が、約0.1GHz〜約3.0GHzの周波数範囲にわたって2.0〜4.0の範囲の実数透磁率を有する、項目29または30に記載の物品。
33.
(a)Fe、Ba、Co、およびMoを含むヘキサフェライト相前駆体化合物を準備する工程と、
(b)ヘキサフェライト相前駆体化合物を空気中で焼成して、Z型ヘキサフェライト相
を含む材料を形成する工程と
を備える、ヘキサフェライト組成物を製造する方法。
35. ヘキサフェライト相前駆体化合物が、MoO2、BaCO3、Co3O4、およびFe2O3を含む、項目33または34に記載の方法。
38.
(c)工程(b)で形成された材料を破砕して、粉末混合物を形成する工程と、
(d)粉末混合物を焼結する工程と
をさらに含む、項目33〜37のいずれかに記載の方法。
40. 粉末混合物が、4〜20時間焼結される、項目38または39に記載の方法。
41. 粉末混合物が、酸素雰囲気で焼結される、項目38〜40のいずれかに記載の方法。
43. 粉末混合物に結合剤を添加する工程をさらに備える、項目38〜42のいずれかに記載の方法。
46.
(e)工程(d)で形成された材料を破砕して、粉末混合物を形成する工程と、
(f)工程(e)で形成された粉末混合物をアニールする工程と
をさらに備える、項目38〜45のいずれかに記載の方法。
48. 粉末混合物が、9〜20時間アニールされる、項目46または47に記載の方法。
本ヘキサフェライト組成物は、高周波数用途、特に極超短波(UHF)およびマイクロ波の用途ならびにデバイス、例えば、極超短波およびマイクロ波の範囲で動作可能なアンテナ、フィルタ、インダクタ、およびサーキュレータでの動作に適する。極超短波(UHF)範囲は、0.3GHz〜3GHzである。
(BazSr(3−z))Co(2+x)MoxFe(y−2x)O41
(式中、
x=0.01〜0.20であり;
y=20〜24であり;
z=0〜3である)
を有する。
一部の実施形態において、本組成物は、高周波数で高い実数透磁率μ’を示す:
f=0.1〜1GHzでの透磁率: μ’>8;
f=0.1〜0.8GHzでの透磁率: μ’>10。
f=0.1〜0.8GHzでの損失: tanδμ<0.3およびtanδε<0.01.
f=0.8GHzでの損失係数: tanδμ/μ’<0.03およびtanδε/ε’<0.001。
組成物は、z=3である、MoドープBaCo2Zヘキサフェライトである。一部の実施形態において、MoドープBaCo2Zヘキサフェライトは、約0.1GHz〜約1.0GHzの周波数で8.0〜12.0の範囲の実数透磁率を有し得る。一部の実施形態において、この材料は、0.08<x<0.15のMo含有量で、f=0.3GHzで0.08〜0.15の範囲の磁気損失正接およびf=0.8GHzで0.3〜0.75の範囲の磁気損失正接を有し得る。一部の実施形態において、この材料は、0.01<x<0.20のMo含有量でf=0.1〜10.0GHzの範囲にわたって8〜13の範囲の実数透磁率を有し得る。一部の実施形態において、誘電損失正接は、0.01<x<0.12のMo含有量についてf=0.1〜10.0GHzで0.02未満でもよい。
3GHzまたはそれ超の周波数で約2.0〜約12.0の範囲の実数透磁率μ’を有する。一部の実施形態では0.1GHz〜少なくとも3.0GHzの範囲の周波数で、および一部の実施形態ではより高い周波数で、実数誘電率が、少なくとも3.0、少なくとも5.0、少なくとも7.0、少なくとも8.0、少なくとも9.0、少なくとも10.0、少なくとも11.0、少なくとも12.0である。
δεを有する。
2)1200℃±100℃で300分±60分間保持する;
3)炉を、周囲まで、例えば、240分±60分間かけて冷却させる。
1)周囲温度(例えば、約20℃)で出発し、800℃±100℃まで180分±60分間かけて昇温させる;
2)1200℃±100℃まで180分±60分間かけて昇温させる;
3)1200℃±100℃で240分±60分間保持する;
4)炉を、周囲温度まで、例えば、480分±60分間かけて冷却させる。
1)周囲温度(例えば、約20℃)で出発し、400℃±100℃まで80分±10分間かけて昇温させる;
2)900℃±100℃まで200分±10分間かけて昇温させる;
3)900℃±100℃で240分±100分間保持する;
4)炉を、例えば、360分±100分間にわたって周囲に冷却させる。
本明細書に記載されるCO2Zヘキサフェライトの透磁率、誘電率、および共鳴周波数は、Mo、Sr、およびBaイオンによる置換によって調整され得る。したがって、これらのMoドープCo2Zヘキサフェライトは、0.3〜10GHzで動作するマイクロ波磁気誘電基板材料の望ましい候補である。組成物は、高い動作周波数(0.1〜1GHzおよびそれ超)にわたって高い透磁率(μ’>8)を示し得る。透磁率および誘電率の等しいまたは実質的に等しい値は、μ’およびε’の両方ともが、f=0.8GHzで7超、または一部の実施形態では8超で実現され、インピーダンスの一致をもたらすことができる。本組成物は、例えば、f=0.8GHzでtanδμ/μ’=0.03およびtanδε/ε’=0.001の低い磁気および誘電損失係数を有し得る。材料コストは、例えば、Irドープヘキサフェライトと比較して低い。
ヘキサフェライト組成物は、スピントロニクス用途、例えば、ディスクドライブ読取りヘッドならびに他のデータ記憶およびメモリデバイスで、ならびに磁気センサなどで使用される巨大磁気抵抗(GMR)デバイスおよび巨大トンネル磁気抵抗(TMR)デバイスで使用され得る。他のスピントロニクス用途には、半導体デバイス、例えば、スピントランジスタおよびスピン発光ダイオードが含まれる。
結晶学的構造は、CuKα線を使用してθ−2θジオメトリで室温でのX線回折(XRD、Philips X’pert PRO)測定によって決定した。複素誘電率および透磁率スペクトルは、f=0.05〜1.0GHzでトロイド試料のために、7mm HP85050C精密エアラインを備えたAgilent E864A 45MHz〜50Ghz PNAシリーズベクタネットワークアナライザ(VNA)およびAgilent
インピーダンスアナライザ(IA)を使用することによって、0.3〜10GHzの周波数範囲にわたって測定した。形態観察は、走査電子顕微鏡法(SEM)によって走査した。
1.Co2Zヘキサフェライトについての透磁率スペクトルのMo依存性
Co2Zヘキサフェライトの様々なMo(Mo4+イオン)含有量(x)による実数透磁率の変化を図1Aに表す。この図は、モリブデン含有量が増加するにつれて(x>0.10)、低周波数での透磁率が低下することを示す。カットオフ周波数(共鳴周波数)は、図1Bに示すとおりに、xが0.10を超えて増加するにつれて、1.0GHzを超えて増加する。
実数誘電率は、図4Aに示すとおりに、0.1〜10.0GHzの周波数範囲にわたってモリブデン含有量によってε’=約7.5〜>12の範囲に調整することができる。最低磁気損失を有する、試料ZM6は、図4Bに示すとおりに、約8の小さい誘電率を示す。
試料ZM5および試料ZM6の透磁率、誘電率ならびに磁気および誘電損失正接の周波数依存性を図7Aおよび図7Bに表す。f<0.5GHzで、磁気損失正接は0.15未満である一方で、透磁率は10〜11程度に高い。最低磁気損失正接は、試料ZM6についてf=0.8GHzで0.27未満である。インピーダンスの一致は、等しいかまたは実質的に等しい透磁率および誘電率(ε’=9(または8)、μ’=10)に関して得ることができる。
試料ZM5および試料ZM6の磁気スペクトルを、図8に示すとおりに、0.1〜1GHzの周波数範囲にわたってインピーダンスアナライザにより測定した。結果は、VNAにより測定されたものとよく一致しており、0.8GHzにおいて、8〜11の透磁率および0.3未満の磁気損失正接を示す。
5.SEM形態観察
図9は、MoドープCo2ZヘキサフェライトのSEM形態観察を示し、8〜5:1の大きなアスペクト比の形状の小板であるようにみえる結晶粒の等方性結晶粒配向および一様な結晶粒分布を示す。平均結晶粒サイズは、長軸に沿ってほぼ60〜80μmであると推定される。
表4は、既存のIrドープCo2Zヘキサフェライトと、0.8GHzでMoドープおよびIrドープCo2Zヘキサフェライトについてのε’、μ’、tanδεおよびtanδμの比較を提示する。MoドープCo2Zヘキサフェライトは、試料ZM5および試料ZM6である。
要約すると、公称組成物Ba3Co2+xMoxFe24−2xO41(ここで、x=0〜0.20である)の多結晶ヘキサフェライト組成物を、セラミックプロセスにより調製した。結果は、MoドープCo2Z多結晶ヘキサフェライトが、0.1〜5.0GHzの広い周波数範囲にわたって既存のIrドープCo2Zヘキサフェライトのものより優れている透磁率、誘電率ならびに磁気および誘電損失を有することを示す。測定されたマイクロ波誘電および磁気特性は、損失tanδεおよび損失tanδμが、x=0.10〜0.15を有するモリブデンの添加によって0.8GHzで、それぞれ、75%および60%だけ低下したが、透磁率は、0.8GHzで、10.1に増加し、IrドープCo2Zヘキサフェライトと比較して、25%だけ増強したことを示した。さらに、MoドープCo2Zヘキサフェライトはまた、0.1〜1.0GHzの周波数範囲にわたって実数誘電率および透磁率の実質的に等しい値(8〜9)を実証して、特性インピーダンスを自由空間インピーダンスのものと同じ特性インピーダンスにする。注目すべきことに、MoドープCo2Zヘキサフェライトは、前に報告されたものの中でも最低損失係数(tanδε/ε’<0.00075およびtanδμ/μ’<0.029)を生じさせるだけでなく、低い材料コストも有する。MoドープCo2Zヘキサフェライトの材料コストは、IrドープCo2Zヘキサフェライトのものの3分の1であることができる。これらの特性は、これらのヘキサフェライトを極超短波(UHF)でのマイクロ波デバイス、例えば、小型アンテナにおける用途に適したものにする。
製造プロセスは、以下の原材料およびそれらの純度:BaCO3(99.95%)、SrCO3(99.95%)、Co3O4(99.7%)、MoO2(99%)およびFe2O3(99.95%)によって始めた。それぞれの比は、目標公称組成と一致するよう
に選択した。例えば、ヘキサフェライト相前駆体化合物は、0〜0.96重量%のMoO2、22.10〜22.18重量%のBaCO3、6.02〜6.59重量%のCo3O4、および70.35〜71.8重量%のFe2O3を含み得る。
最良の試料は、ZSF4であった。それは、1.0GHzで高い透磁率、ε’=8.67、および低い損失正接、tanδμ=0.091、ならびに高いカットオフ周波数、fr=2.40GHzを示した。
1.磁気透磁率スペクトルおよび磁気損失
透磁率スペクトルを0.1〜10.0GHzの周波数にわたって測定した。透磁率は、図16に見られるとおりに、x=0.10のMo含有量を除いて、Mo含有量によって低周波数(0.1GHz)で3.8から3.3への低下を示す。Mo含有量は、図17に見られるとおりに、5.0GHzを超えるより高い周波数への損失正接ピークのシフトをもたらす。Mo含有量x=0.10は、図17に見られるとおりに、0.4〜1.5GHzの周波数範囲で最小の損失正接をもたらす。すなわち、x=0.20についての損失正接
は、0.4GHzで約0.1および1.5GHzで0.4であり、これは、MoドープSrCo2Zフェライトの中で最低の損失である。
誘電率は、図19に見られるとおりに、基本的にSrCo2Zヘキサフェライト中のMo含有量に比例し、x=0.02についてわずかに低下する。誘電損失正接は、図20に見られるとおりに、Mo含有量の増加(x=0からx=0.20)とともに、0.03から0.08に増加する。
3.磁気および誘電損失
MoドープSrCo2Zヘキサフェライトの最低の磁気および誘電損失は、x=0.10のMo含有量で示された。このMo含有量で、f=1.0GHzにおいて:
μ’=3.7
tanδμ=0.24
ε’=14.2;および
tanδε=0.03
である。
本明細書で使用される場合、「から本質的になる(consiting essentially of)」は、特許請求の範囲の基本的および新規な特性に著しく影響を与えない材料または工程の包含を可能にする。特に組成物の成分の記載またはデバイスの素子の記載において、用語「含む(comprising)」の本明細書でのいずれの記述も、「から本質的になる」または「からなる(consiting of)」と交換され得る。
、2015年1月30日に出願された米国仮出願第62/110,025号の35§119(e)の下での優先権を主張し、この開示は、本明細書に援用される。
Claims (10)
- 鉄、コバルト、バリウムおよびストロンチウムの一方または両方、ならびにモリブデンを含むヘキサフェライト組成物であって、式
(BazSr(3−z))Co(2+x)MoxFe(y−2x)O41
(式中、
x=0.01〜0.20であり;
y=20〜24であり;
z=0〜3である)
を有する、Z型ヘキサフェライト相を備える、ヘキサフェライト組成物。 - x=0.08〜0.15である、請求項1に記載のヘキサフェライト組成物。
- 0.1〜1.0GHzの周波数範囲にわたって少なくとも3.0の実数透磁率を有する、または、0.1〜1.0GHzの周波数範囲にわたって7.0〜12.0範囲の実数透磁率を有する、請求項1に記載のヘキサフェライト組成物。
- 0.1〜3.0GHzの周波数範囲にわたって少なくとも6.0の実数誘電率を有する、または、0.1〜10.0GHzの周波数範囲にわたって6.0〜18.0の実数誘電率を有する、請求項1に記載のヘキサフェライト組成物。
- 3%以内で自由空間のインピーダンスに一致する特性インピーダンス、0.1〜0.8GHzの周波数で0.02未満の誘電損失正接tanδε、0.1〜1.0GHzの周波数で0.16未満の誘電損失正接tanδε、0.4GHzで0.1の磁気損失正接tanδμ、0.1〜0.8GHzの周波数で0.3未満の磁気損失正接tanδμ、0.1〜3.5GHzの周波数で0.95未満の磁気損失正接tanδμ、0.1〜1.0GHzの周波数範囲にわたって0.1〜1.0の範囲の磁気損失正接tanδμ、0.8GHzの周波数で0.001未満の誘電損失係数tanδε/ε’、および、0.8GHzの周波数で0.03未満の磁気損失係数tanδμ/μ’のうちの少なくとも1つを有する、請求項1に記載のヘキサフェライト組成物。
- 請求項1に記載のヘキサフェライト組成物を備える、物品。
- アンテナ、フィルタ、インダクタ、サーキュレータ、または位相シフタである、請求項6に記載の物品。
- 式
(BazSr(3−z))Co(2+x)MoxFe(y−2x)O41
(式中、
x=0.01〜0.20であり;
y=20〜24であり;
z=0〜3である)
を有するZ型ヘキサフェライト相を備える第2のヘキサフェライト組成物をさらに備え、
前記ヘキサフェライト組成物および前記第2のヘキサフェライト組成物中のBaの量およびSrの量が異なる、請求項7に記載の物品。 - 請求項1に記載のヘキサフェライト組成物を製造する方法であって、
(a)Fe、Ba、Co、およびMoを含むヘキサフェライト相前駆体化合物を準備する工程と、
(b)前記ヘキサフェライト相前駆体化合物を空気中で焼成して、Z型ヘキサフェライト相を含む材料を形成する工程と
を備える、方法。 - 前記ヘキサフェライト相前駆体化合物が、0〜0.96重量%のMoO2、22.10〜22.18重量%のBaCO3、6.02〜6.59重量%のCo3O4、および70.35〜71.8重量%のFe2O3を含む、請求項9に記載の方法。
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