JP6897792B2 - セラミック部材 - Google Patents
セラミック部材 Download PDFInfo
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- JP6897792B2 JP6897792B2 JP2019557061A JP2019557061A JP6897792B2 JP 6897792 B2 JP6897792 B2 JP 6897792B2 JP 2019557061 A JP2019557061 A JP 2019557061A JP 2019557061 A JP2019557061 A JP 2019557061A JP 6897792 B2 JP6897792 B2 JP 6897792B2
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- 239000000919 ceramic Substances 0.000 title claims description 51
- 229910052788 barium Inorganic materials 0.000 claims description 52
- 229910052712 strontium Inorganic materials 0.000 claims description 51
- 229910052791 calcium Inorganic materials 0.000 claims description 37
- 239000013078 crystal Substances 0.000 claims description 30
- 239000002131 composite material Substances 0.000 claims description 24
- 238000000137 annealing Methods 0.000 claims description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 11
- 229910052760 oxygen Inorganic materials 0.000 claims description 11
- 239000001301 oxygen Substances 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 10
- 238000002441 X-ray diffraction Methods 0.000 claims description 8
- 238000010304 firing Methods 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 239000011575 calcium Substances 0.000 description 35
- 239000011572 manganese Substances 0.000 description 20
- 229910010293 ceramic material Inorganic materials 0.000 description 19
- 239000000463 material Substances 0.000 description 9
- 230000007423 decrease Effects 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- 229910052693 Europium Inorganic materials 0.000 description 4
- 229910052688 Gadolinium Inorganic materials 0.000 description 4
- 229910052772 Samarium Inorganic materials 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 3
- 239000002270 dispersing agent Substances 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 229910052692 Dysprosium Inorganic materials 0.000 description 2
- 229910052689 Holmium Inorganic materials 0.000 description 2
- 229910052771 Terbium Inorganic materials 0.000 description 2
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 238000007606 doctor blade method Methods 0.000 description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052727 yttrium Inorganic materials 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 229910052691 Erbium Inorganic materials 0.000 description 1
- 229910021193 La 2 O 3 Inorganic materials 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000007772 electroless plating Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000004993 emission spectroscopy Methods 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 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
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 230000004043 responsiveness Effects 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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- C01G45/12—Manganates manganites or permanganates
- C01G45/1221—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof
- C01G45/125—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type[MnO3]n-, e.g. Li2MnO3, Li2[MxMn1-xO3], (La,Sr)MnO3
- C01G45/1264—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type[MnO3]n-, e.g. Li2MnO3, Li2[MxMn1-xO3], (La,Sr)MnO3 containing rare earth, e.g. La1-xCaxMnO3, LaMnO3
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Description
(1)R1がNdからなり、R2がSm、EuおよびGdのうちの少なくとも1種からなるとき、xが0.05≦x≦1.0であり、
(2)R1がNdからなり、R2がTb、Dy、Ho、ErおよびYのうちの少なくとも1種からなるとき、xが0.05≦x≦0.8であり、
(3)R1がSm、EuおよびGdのうちの少なくとも1種からなり、R2がTb、Dy、HoおよびYのうちの少なくとも1種からなるとき、xが0≦x≦0.4であり、
(4)R1がSm、EuおよびGdのうちの少なくとも1種からなり、R2がSm、EuおよびGdのうちのR1として選ばれなかった残りの少なくとも1種からなるとき、xが0≦x≦1.0である
ことを特徴とするセラミック材料が提案されている(特許文献1)。
(i)Caであるか、あるいは
(ii)Caと、さらにSrおよびBaの少なくとも1種を含み、Ca、SrおよびBaの合計に対する、SrおよびBaの合計量が、5mol%以下であり、
その表面の結晶系が単斜晶系である、セラミック部材が提供される。
(i)Caであるか、あるいは
(ii)Caと、さらにSrおよびBaの少なくとも1種を含み、Ca、SrおよびBaの合計に対する、SrおよびBaの合計量が、5mol%以下であり、
CuKα線源を用いるX線回折解析において、2θ=32.5°および32.7°にピークを有する、セラミック部材が提供される。
La源、AE源(ここに、AEは、
(i)Caであるか、あるいは
(ii)Caと、さらにSrおよびBaの少なくとも1種を含み、Ca、SrおよびBaの合計に対する、SrおよびBaの合計量が、5mol%以下である)、およびMn源を焼成して焼結体を得る工程、
得られた焼結体の表面の少なくとも一部を除去する工程、
前記表面の少なくとも一部が除去された焼結体を、酸素存在下、900℃以上でアニール処理する工程
を含む、製造方法が提供される。
La1−x−yAEyMnO3
[式中:
AEは、(i)Caであるか、あるいは
(ii)Caと、さらにSrおよびBaの少なくとも1種を含み、Ca、SrおよびBaの合計に対する、SrおよびBaの合計量が、5mol%以下であり、
xは、0<x≦0.20を満たし、
yは、0<y≦0.10を満たす。]
で表される組成を有する複合酸化物である。
AEは、
(i)Caであるか、あるいは
(ii)Caと、さらにSrおよびBaの少なくとも1種を含み、Ca、SrおよびBaの合計に対する、SrおよびBaの合計量が、5mol%以下であり、
Laの含有モル部およびAEの含有モル部の合計が、Mn100モル部に対して、100モル部より小さく80モル部以上であり、
AEの含有モル部が、Mn100モル部に対して、0モル部よりも大きく10モル部以下である。
AEの含有モル部が、Mn100モル部に対して、3モル部よりも大きく10モル部未満である。
La源、AE源(ここに、AEは、
(i)Caであるか、あるいは
(ii)Caと、さらにSrおよびBaの少なくとも1種を含み、Ca、SrおよびBaの合計に対する、SrおよびBaの合計量が、5mol%以下である)、およびMn源を焼成して焼結体を得る工程、
得られた焼結体の表面の少なくとも一部を除去する工程、
表面の少なくとも一部が除去された焼結体を、酸素存在下、900℃以上でアニール処理する工程
を含む、製造方法を提供する。
突入電流抑制素子を下記の方法で作製した。
素体原料としてそれぞれ99.9%以上の酸化マンガン(Mn3O4)、炭酸カルシウム(CaCO3)の粉末を用いた。これら原料を焼成後に下記式の組成になるように秤量した。
(La1−x−yAEy)MnO3±δ (AE=Ca、x=0.11、y=0.03)
・IV特性評価
上記のようにして作製した試料(La0.86Ca0.03)MnO3±δについて、下記の通り電気特性を評価した。
上記で得られた試料について、X線回折(XRD)により、結晶構造を解析した。結果を図2および表1に示す。尚、X線回折解析は、RINT−K(株式会社リガク製)を用いて行った。線源はCuKα線であり、粉末ではなく、素体の表面を測定した。
NTC特性の評価としてB定数を測定した。B定数は、ナノボルトメータ(アジレント34420A)を用いて液相中で抵抗測定を行い、下記式にて算出した。結果を表1に示す。尚、測定温度は25℃と100℃とし、測定中は温度が設定温度に対して±0.1℃内に収まるようにした。
B=ln(R100/R25)/(1/(273.15+100)−1/(273.15+25)
[R100:100℃における素子抵抗、R25:25℃における素子抵抗]
Claims (14)
- La、AEおよびMnの複合酸化物から構成されるセラミック部材であって、AEは、
(i)Caであるか、あるいは
(ii)Caと、さらにSrおよびBaの少なくとも1種を含み、Ca、SrおよびBaの合計に対する、SrおよびBaの合計量が、5mol%以下であり、
その表面の結晶系が単斜晶系である、セラミック部材。 - 前記複合酸化物が、以下の式(I):
La1−x−yAEyMnO3
[式中:
AEは、
(i)Caであるか、あるいは
(ii)Caと、さらにSrおよびBaの少なくとも1種を含み、Ca、SrおよびBaの合計に対する、SrおよびBaの合計量が、5mol%以下であり、
xは、0<x≦0.20を満たし、
yは、0<y≦0.10を満たす。]
で表される組成を有する、請求項1に記載のセラミック部材。 - 前記複合酸化物が、La、AEおよびMnの複合酸化物であって、
AEは、
(i)Caであるか、あるいは
(ii)Caと、さらにSrおよびBaの少なくとも1種を含み、Ca、SrおよびBaの合計に対する、SrおよびBaの合計量が、5mol%以下であり、
Laの含有モル部およびAEの含有モル部の合計が、Mn100モル部に対して、100モル部より小さく80モル部以上であり、
AEの含有モル部が、Mn100モル部に対して、0モル部よりも大きく10モル部以下である、
請求項1に記載のセラミック部材。 - La、AEおよびMnの複合酸化物から構成されるセラミック部材であって、AEは、
(i)Caであるか、あるいは
(ii)Caと、さらにSrおよびBaの少なくとも1種を含み、Ca、SrおよびBaの合計に対する、SrおよびBaの合計量が、5mol%以下であり、
CuKα線源を用いるX線回折解析において、2θ=32.5°および32.7°にピークを有する、セラミック部材。 - 前記複合酸化物が、以下の式(I):
La1−x−yAEyMnO3
[式中:
AEは、
(i)Caであるか、あるいは
(ii)Caと、さらにSrおよびBaの少なくとも1種を含み、Ca、SrおよびBaの合計に対する、SrおよびBaの合計量が、5mol%以下であり、
xは、0<x≦0.20を満たし、
yは、0<y≦0.10を満たす。]
で表される組成を有する、請求項4に記載のセラミック部材。 - 前記複合酸化物が、La、AEおよびMnの複合酸化物であって、
AEは、
(i)Caであるか、あるいは
(ii)Caと、さらにSrおよびBaの少なくとも1種を含み、Ca、SrおよびBaの合計に対する、SrおよびBaの合計量が、5mol%以下であり、
Laの含有モル部およびAEの含有モル部の合計が、Mn100モル部に対して、100モル部よりも小さく80モル部以上であり、
AEの含有モル部が、Mn100モル部に対して、0モル部よりも大きく10モル部以下である、
請求項5に記載のセラミック部材。 - 2θ=32.5°のピーク強度に対する、2θ=32.7°のピーク強度の比が、1より大きい、請求項4〜6のいずれか1項に記載のセラミック部材。
- 表面の結晶系と中央部の結晶系が異なる、請求項1〜7のいずれか1項に記載のセラミック部材。
- 表面の結晶系が単斜晶系であり、中央部の結晶系が斜方晶系である、請求項8に記載のセラミック部材。
- 電子部品の素体である、請求項1〜9のいずれか1項に記載のセラミック部材。
- 請求項10に記載の素体と、該素体の表面に形成された電極を有して成る、電子素子。
- IV特性相関係数rの二乗が、0.9995以上である、請求項11に記載の電子素子。
- 突入電流を抑制するためのサーミスタ素子として用いられる、請求項11または12に記載の電子素子。
- La、AEおよびMnの複合酸化物から構成されるセラミック部材の製造方法であって、
La源、AE源(ここに、AEは、
(i)Caであるか、あるいは
(ii)Caと、さらにSrおよびBaの少なくとも1種を含み、Ca、SrおよびBaの合計に対する、SrおよびBaの合計量が、5mol%以下である)、およびMn源を焼成して焼結体を得る工程、
得られた焼結体の表面の少なくとも一部を除去する工程、
前記表面の少なくとも一部が除去された焼結体を、酸素存在下、900℃以上でアニール処理する工程
を含む、製造方法。
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