JP6620807B2 - 複合体 - Google Patents
複合体 Download PDFInfo
- Publication number
- JP6620807B2 JP6620807B2 JP2017518722A JP2017518722A JP6620807B2 JP 6620807 B2 JP6620807 B2 JP 6620807B2 JP 2017518722 A JP2017518722 A JP 2017518722A JP 2017518722 A JP2017518722 A JP 2017518722A JP 6620807 B2 JP6620807 B2 JP 6620807B2
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- JP
- Japan
- Prior art keywords
- cermet
- intermediate layer
- metal
- phase
- composite
- 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.)
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- 239000011195 cermet Substances 0.000 claims description 344
- 229910052751 metal Inorganic materials 0.000 claims description 258
- 239000002184 metal Substances 0.000 claims description 256
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 116
- 239000002131 composite material Substances 0.000 claims description 112
- 239000000203 mixture Substances 0.000 claims description 47
- 229910000859 α-Fe Inorganic materials 0.000 claims description 40
- 229910052759 nickel Inorganic materials 0.000 claims description 31
- 229910052802 copper Inorganic materials 0.000 claims description 26
- 229910052596 spinel Inorganic materials 0.000 claims description 20
- 239000011029 spinel Substances 0.000 claims description 20
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 19
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 19
- 238000002844 melting Methods 0.000 claims description 17
- 230000008018 melting Effects 0.000 claims description 17
- 229910044991 metal oxide Inorganic materials 0.000 claims description 10
- 150000004706 metal oxides Chemical group 0.000 claims description 10
- 230000014509 gene expression Effects 0.000 claims description 6
- NQNBVCBUOCNRFZ-UHFFFAOYSA-N nickel ferrite Chemical compound [Ni]=O.O=[Fe]O[Fe]=O NQNBVCBUOCNRFZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910052804 chromium Inorganic materials 0.000 claims description 5
- 238000005520 cutting process Methods 0.000 claims description 3
- 229910052735 hafnium Inorganic materials 0.000 claims description 3
- 229910052748 manganese Inorganic materials 0.000 claims description 3
- 229910052758 niobium Inorganic materials 0.000 claims description 3
- 229910052715 tantalum Inorganic materials 0.000 claims description 3
- 229910052718 tin Inorganic materials 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 229910052720 vanadium Inorganic materials 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- 239000012071 phase Substances 0.000 description 205
- 239000000843 powder Substances 0.000 description 70
- 238000010438 heat treatment Methods 0.000 description 60
- 230000000052 comparative effect Effects 0.000 description 36
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 31
- 238000000034 method Methods 0.000 description 31
- 239000011812 mixed powder Substances 0.000 description 24
- 238000004458 analytical method Methods 0.000 description 23
- 238000005259 measurement Methods 0.000 description 22
- 238000009792 diffusion process Methods 0.000 description 19
- 229910045601 alloy Inorganic materials 0.000 description 17
- 239000000956 alloy Substances 0.000 description 17
- 238000005868 electrolysis reaction Methods 0.000 description 16
- 238000002156 mixing Methods 0.000 description 16
- 238000010304 firing Methods 0.000 description 15
- 238000000465 moulding Methods 0.000 description 15
- 150000003839 salts Chemical class 0.000 description 15
- 238000004519 manufacturing process Methods 0.000 description 14
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- 239000011800 void material Substances 0.000 description 12
- 238000013001 point bending Methods 0.000 description 11
- 238000010586 diagram Methods 0.000 description 9
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 8
- 229910002091 carbon monoxide Inorganic materials 0.000 description 8
- 229910052742 iron Inorganic materials 0.000 description 8
- 239000007789 gas Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 5
- 239000011230 binding agent Substances 0.000 description 5
- 230000007423 decrease Effects 0.000 description 5
- 229910001873 dinitrogen Inorganic materials 0.000 description 5
- 239000007791 liquid phase Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 4
- 239000011261 inert gas Substances 0.000 description 4
- 239000000155 melt Substances 0.000 description 4
- 239000002905 metal composite material Substances 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 230000000630 rising effect Effects 0.000 description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 3
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 description 3
- 238000005275 alloying Methods 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 238000007493 shaping process Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 238000013507 mapping Methods 0.000 description 2
- 239000011164 primary particle Substances 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
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- 239000010935 stainless steel Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 229910003271 Ni-Fe Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
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- 150000002739 metals Chemical class 0.000 description 1
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- 230000008023 solidification Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Images
Classifications
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Description
サーメット部材と金属部材と中間層とを有する複合体であって、
前記サーメット部材はサーメット酸化物相とサーメット金属相とを含み、
前記サーメット酸化物相はNiを含む酸化物またはFeを含む酸化物を含み、
前記サーメット金属相はNiを含み、
前記中間層はCuを含み、
前記サーメット部材と前記中間層との界面から前記サーメット部材側に10、50、100、1000μm離れた点における前記金属相中のCuの質量比率をC10、C50、C100、C1000(mass%)とし、
前記界面から前記サーメット部材側に10、100μm離れた点における前記酸化物相中のCuの質量比率をM10、M100(mass%)としたときに、下記式1、式2を同時に満たすことを特徴とする。
C10>C50>C100>C1000(mass%):(式1)
5>M10―M100>−5(mass%):(式2)
前記中間層は少なくとも第1の中間層および第2の中間層を有し、
前記第1の中間層は、前記サーメット部材と接合しており、
前記第1の中間層は少なくとも第1金属Cuを含み、
前記第2の中間層は少なくとも第2金属M2を含み、
前記第1金属Cuの融点が前記第2金属M2の融点よりも低く、
前記第1の中間層におけるCuの質量濃度が前記第2の中間層におけるCuの質量濃度よりも高く、
前記第2の中間層におけるM2の質量濃度が前記第1の中間層におけるM2の質量濃度よりも高くてもよい。
40/60≦Cu/M2≦90/10:(式3)
前記第3の中間層は、前記金属部材と接合してもよい。
前記第3の中間層におけるM2の質量濃度が前記第2の中間層におけるM2の質量濃度よりも低いことが好ましい。
前記中間酸化物相は少なくとも一種以上の金属の酸化物を含むことが好ましい。
60/40≦So/Sm≦90/10:(式4)
組成式NixFeyMzO4(x+y+z=3、x≠0、y≠0、MはAl、Co、Cr、Mn、Ti、Zr、Sn、V、Nb、Ta、Hfからなる群から選択される少なくとも1種以上)で表されるスピネルフェライト相と、
組成式Nix’Fe1−x’O(x’≠0)で表される酸化ニッケル相と、を有し、
前記サーメット酸化物相と前記サーメット金属相とを含む前記サーメット部材全体を100質量%とする場合において、
前記スピネルフェライト相の含有率が40〜80質量%であり、
前記酸化ニッケル相の含有率が0〜10質量%(0質量%を含む)であり、
前記サーメット金属相の含有率が15〜45質量%であることが好ましい。
60/40≦So/Sm≦90/10を満たすこと好ましい。So/Smが上記の範囲内であることが好ましいのは、サーメット部材3中のサーメット金属相6をサーメット酸化物相5で覆うことでサーメット金属相5の溶融塩(特にフッ化物)への溶解を防ぐとともにサーメット部材3の導電性を向上することができるためである。
5>M10−M100>−5(mass%):式2
次に、本実施形態に係る複合体の好適な製造方法について説明するが、以下の記載により本発明に係る複合体の製造方法は限定されない。
(実施例1〜45および比較例1〜24)
市販のNiO粉末とFe2O3粉末とを、NiOとFe2O3のモル比率が70:30となるように配合し、ボールミルを用いて混合した。混合により得られた混合粉を、大気中、温度1000℃で3時間保持して仮焼を行った。仮焼により得られた仮焼粉をボールミルで粉砕し、フェライト酸化物粉末を調製した。
(実施例50〜75)
実験例2では、実験例1とは異なり、NiO粉末とFe2O3粉末との混合比率を、NiOとFe2O3のモル比率が50:50になるようにした。また、接合時間も変化させた。さらに、表2に示す材質の中間部材(実施例50では第1中間部材のみ、実施例51〜69では第1中間部材および第2中間部材、実施例70〜75では第1中間部材、第2中間部材に加えて第3中間部材)を準備した。各中間部材の厚みは0.02cmとした。
(実施例80〜92)
実験例3では、実験例2と同様に、NiO粉末とFe2O3粉末との混合比率を、NiOとFe2O3のモル比率が50:50になるようにした。さらに、中間部材として以下に示す製法により作製した混合成形体を用いた。上記した点および表5に記載のある条件以外は、実験例2の実施例50と同様にして表5に示す実施例81〜92を得た。そして、表5および表6に示す各種特性を測定した。全ての実施例でクラックは発生せず、中間部材におけるボイド比率が5%未満であった。
2・・・中間部材
3・・・サーメット部材
4・・・中間層
5・・・サーメット酸化物相
5a・・・スピネルフェライト相
5b・・・酸化ニッケル相
6・・・サーメット金属相
8・・・サーメット金属相(C10測定)
9・・・サーメット金属相(C50測定)
10・・・サーメット金属相(C100測定)
11・・・サーメット金属相(C1000測定)
12・・・サーメット酸化物相(M10測定)
13・・・サーメット酸化物相(M100測定)
41・・・第1の中間層
42・・・第2の中間層
43・・・第3の中間層
46・・・中間金属相
48・・・中間酸化物相
D1、D2、D3・・・サーメット部材の寸法
D4、D5、D6・・・金属部材の寸法
Claims (21)
- サーメット部材と金属部材と中間層とを有する複合体であって、
前記サーメット部材はサーメット酸化物相とサーメット金属相とを含み、
前記サーメット酸化物相はNiを含む酸化物またはFeを含む酸化物を含み、
前記サーメット金属相はNiを含み、
前記中間層はCuを含み、
前記サーメット部材と前記中間層との界面から前記サーメット部材側に10、50、100、1000μm離れた点における前記金属相中のCuの質量比率をC10、C50、C100、C1000(mass%)とし、
前記界面から前記サーメット部材側に10、100μm離れた点における前記酸化物相中のCuの質量比率をM10、M100(mass%)としたときに、下記式1、式2を 同時に満たすことを特徴とする複合体。
C10>C50>C100>C1000(mass%):(式1)
5>M10―M100>−5(mass%):(式2)
- 請求項1に記載の複合体であって、前記金属部材は少なくともNiを含むことを特徴とする複合体。
- 請求項1または請求項2に記載の複合体であって、前記中間層の、NiとCuの質量比率を百分率で表したときに、Niが10<Ni<70(mass%)、Cuが30<Cu<90(mass%)であることを特徴とする複合体。
- 請求項1〜3のいずれかに記載の複合体であって、
前記中間層は少なくとも第1の中間層および第2の中間層を有し、
前記第1の中間層は、前記サーメット部材と接合しており、
前記第1の中間層は少なくとも第1金属Cuを含み、
前記第2の中間層は少なくとも第2金属M2を含み、
前記第1金属Cuの融点が前記第2金属M2の融点よりも低く、
前記第1の中間層におけるCuの質量濃度が前記第2の中間層におけるCuの質量濃度よりも高く、
前記第2の中間層におけるM2の質量濃度が前記第1の中間層におけるM2の質量濃度よりも高いことを特徴とする複合体。 - 請求項4に記載の複合体であって、
前記第1の中間層が、前記第2の中間層とも接合している複合体。 - 請求項4または請求項5に記載の複合体であって、前記第2の中間層が、前記金属部材と接合している複合体。
- 請求項4〜6のいずれかに記載の複合体であって、
前記第1の中間層におけるCuとM2との質量比(Cu/M2)が下記の式3の範囲内である複合体。
40/60≦Cu/M2≦90/10:(式3)
- 請求項4〜7のいずれかに記載の複合体であってM2がNiである複合体。
- 請求項4、5、7、8のいずれかに記載の複合体であって、
前記中間層は、前記第1の中間層、前記第2の中間層に加えて第3の中間層を有し、
前記第3の中間層は、前記金属部材と接合している複合体。 - 請求項9に記載の複合体であって、
前記第3の中間層におけるCuの質量濃度が前記第2の中間層におけるCuの質量濃度より高く、
前記第3の中間層におけるM2の質量濃度が前記第2の中間層におけるM2の質量濃度よりも低い複合体。 - 請求項9または請求項10に記載の複合体であって、前記第2の中間層が、前記第1の中間層および前記第3の中間層と接合している複合体。
- 請求項1〜11のいずれかに記載の複合体であって、前記サーメット部材に含まれる前記サーメット酸化物相は、少なくともNiの酸化物を含む複合体。
- 請求項1〜12のいずれかに記載の複合体であって、前記サーメット部材に含まれる前記サーメット酸化物相のうち少なくとも一部はニッケルフェライトからなる複合体。
- 請求項1〜3のいずれかに記載の複合体であって、
前記中間層は中間酸化物相と中間金属相とを含み、
前記中間酸化物相は少なくとも一種以上の金属の酸化物を含む複合体。 - 請求項14に記載の複合体であって、前記少なくとも一種以上の金属の酸化物はサーメット酸化物相に含まれる金属の酸化物から選択される複合体。
- 請求項14または請求項15に記載の複合体であって、前記サーメット部材と前記中間層との界面に対して垂直に前記複合体を切断した切断面において、前記中間酸化物相が存在する領域における前記中間酸化物相が占める面積と前記中間金属相が占める面積との合計を100%とする場合に、前記中間酸化物相が占める面積比率が、10%〜50%である複合体。
- 請求項14〜16のいずれかに記載の複合体であって、前記中間層全体に占めるボイドの面積比率が30%以下である複合体。
- 請求項1〜17のいずれかに記載の複合体であって、前記サーメット部材の断面における前記サーメット酸化物相の面積をSo、前記サーメット金属相の面積をSmとし、前記サーメット酸化物相と前記サーメット金属相との面積比をSo/Smとする場合に、So/Smが下記の式4を満たす複合体。
60/40≦So/Sm≦90/10:(式4)
- 請求項1〜18のいずれかに記載の複合体であって、
前記サーメット酸化物相が、
組成式NixFeyMzO4(x+y+z=3、x≠0、y≠0、MはAl、Co、Cr、Mn、Ti、Zr、Sn、V、Nb、Ta、Hfからなる群から選択される少なくとも1種以上)で表されるスピネルフェライト相と、
組成式Nix’Fe1−x’O(x’≠0)で表される酸化ニッケル相と、を有し、
前記サーメット酸化物相と前記サーメット金属相とを含む前記サーメット部材全体を100質量%とする場合において、
前記スピネルフェライト相の含有率が40〜80質量%であり、
前記酸化ニッケル相の含有率が0〜10質量%(0質量%を含む)であり、
前記サーメット金属相の含有率が15〜45質量%である複合体。 - 請求項19に記載の複合体であって、前記サーメット部材に含まれる前記スピネルフェライト相の平均組成が組成式Nix1Fey1Mz1O4(0.60≦x1≦0.90、1.90≦y1≦2.40、0.00≦z1≦0.20)で表される複合体。
- 請求項19または請求項20に記載の複合体であって、前記サーメット部材に前記酸化ニッケル相が含まれ、前記酸化ニッケル相の平均組成が組成式Nix’1Fe1−x’1O(0.70≦x’1≦1.00)で表される複合体。
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