TW202217015A - 陶瓷電子零件及其製造方法 - Google Patents
陶瓷電子零件及其製造方法 Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 32
- 238000004519 manufacturing process Methods 0.000 title claims description 18
- 229910052718 tin Inorganic materials 0.000 claims abstract description 17
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 15
- 229910052737 gold Inorganic materials 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims description 14
- 238000003475 lamination Methods 0.000 claims description 6
- 238000010030 laminating Methods 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 59
- 239000003985 ceramic capacitor Substances 0.000 description 25
- 230000000052 comparative effect Effects 0.000 description 18
- 235000012431 wafers Nutrition 0.000 description 14
- 238000009792 diffusion process Methods 0.000 description 12
- 239000012298 atmosphere Substances 0.000 description 9
- 229910002113 barium titanate Inorganic materials 0.000 description 8
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 7
- 229910010293 ceramic material Inorganic materials 0.000 description 7
- 238000010304 firing Methods 0.000 description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 238000010586 diagram Methods 0.000 description 6
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- 239000000654 additive Substances 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 5
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- 239000002184 metal Substances 0.000 description 4
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- -1 tetragonal compound Chemical class 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N Butyraldehyde Chemical compound CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 229910018731 Sn—Au Inorganic materials 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
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- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 2
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- 229910052796 boron Inorganic materials 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
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- 239000010941 cobalt Substances 0.000 description 2
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- 238000007606 doctor blade method Methods 0.000 description 2
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- 239000011572 manganese Substances 0.000 description 2
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- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 238000010405 reoxidation reaction Methods 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- DJOYTAUERRJRAT-UHFFFAOYSA-N 2-(n-methyl-4-nitroanilino)acetonitrile Chemical compound N#CCN(C)C1=CC=C([N+]([O-])=O)C=C1 DJOYTAUERRJRAT-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- 229910052691 Erbium Inorganic materials 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 229910002367 SrTiO Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229910052769 Ytterbium Inorganic materials 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- AOWKSNWVBZGMTJ-UHFFFAOYSA-N calcium titanate Chemical compound [Ca+2].[O-][Ti]([O-])=O AOWKSNWVBZGMTJ-UHFFFAOYSA-N 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 1
- 239000002003 electrode paste Substances 0.000 description 1
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 description 1
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 1
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000000608 laser ablation Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- HGBOYTHUEUWSSQ-UHFFFAOYSA-N valeric aldehyde Natural products CCCCC=O HGBOYTHUEUWSSQ-UHFFFAOYSA-N 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
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Abstract
本發明提供一種可提昇壽命特性之陶瓷電子零件及其製造方法。
陶瓷電子零件之特徵在於具備積層晶片,該積層晶片積層有以陶瓷為主成分之複數個介電層、及複數個內部電極層,上述內部電極層包含Ni、Sn、Au。
Description
本發明係關於一種陶瓷電子零件及其製造方法。
積層陶瓷電容器等陶瓷電子零件之內部電極會用到Ni(鎳)。於燒成步驟中,為了防止Ni之氧化,大多使用還原氣氛。然而,若將燒成步驟之氣氛設為還原氣氛,則有介電層產生氧缺陷,導致可靠性變差之虞。因此,有文獻揭示出藉由使Ni之內部電極含Sn而提昇電容器之可靠性的技術(例如參照專利文獻1、2)。
[先前技術文獻]
[專利文獻]
[專利文獻1]國際公開第2014/024538號
[專利文獻2]日本專利特表2005-505695號公報
[發明所欲解決之問題]
然而,若將Ni用於內部電極,則陶瓷電子零件之壽命特性仍有改善之餘地。
本發明係鑒於上述問題而完成者,其目的在於提供一種可提昇壽命特性之陶瓷電子零件及其製造方法。
[解決問題之技術手段]
本發明之陶瓷電子零件之特徵在於具備積層晶片,該積層晶片積層有以陶瓷為主成分之複數個介電層、及複數個內部電極層,上述內部電極層包含Ni、Sn、Au。
於上述陶瓷電子零件之上述內部電極層中,相對於Ni而言,Sn含量與Au含量之合計可為0.01 at%以上95 at%以下。
於上述陶瓷電子零件之上述內部電極層中,相對於Ni而言,Sn含量與Au含量之合計可為0.2 at%以上10 at%以下。
於上述陶瓷電子零件之上述內部電極層中,Au含量可少於Sn含量。
於上述陶瓷電子零件之上述內部電極層中,與厚度方向之中心部相比,Sn之濃度在與上述介電層之界面附近更高。
於上述陶瓷電子零件之上述內部電極層中,與積層方向之中心部相比,Au之濃度在與上述介電層之界面附近更高。
本發明之陶瓷電子零件之製造方法之特徵在於包括如下步驟:藉由於介電坯片上形成包含Ni、Sn、Au之內部電極圖案而形成積層單元;藉由積層複數個上述積層單元而形成積層體;及燒成上述積層體。
於上述陶瓷電子零件之製造方法中,形成上述積層單元之步驟可為藉由真空成膜製程於上述介電坯片成膜上述內部電極圖案的步驟。
[發明之效果]
根據本發明,可提供一種可提昇壽命特性之陶瓷電子零件及其製造方法。
以下,參照附圖對實施方式進行說明。
(實施方式)
圖1係表示實施方式之積層陶瓷電容器100之局部剖視立體圖。圖2係圖1之A-A線剖視圖。圖3係圖1之B-B線剖視圖。如圖1~圖3所例示,積層陶瓷電容器100具備:積層晶片10,其具有大致長方體形狀;及外部電極20a、20b,其等設置於積層晶片10之任意對向之2端面。再者,積層晶片10之該2端面以外之4面之中,將積層方向之上表面及下表面以外之2面稱為側面。外部電極20a、20b於積層晶片10之積層方向之上表面、下表面及2側面延伸。但,外部電極20a、20b相互分開。再者,圖1中,X軸方向(第1方向)為積層晶片10之長度方向,其係積層晶片10之2端面對向之方向,且係外部電極20a與外部電極20b對向之方向。Y軸方向(第2方向)為內部電極層之寬度方向。Z軸方向為積層方向。X軸方向、Y軸方向、Z軸方向相互正交。
積層晶片10具有介電層11與內部電極層12交替積層之構成,介電層11包含作為介電體發揮功能之陶瓷材料,內部電極層12包含賤金屬材料。各內部電極層12之端緣於積層晶片10之設置有外部電極20a之端面與設置有外部電極20b之端面交替露出。藉此,各內部電極層12與外部電極20a及外部電極20b交替導通。其結果為,積層陶瓷電容器100具有介隔內部電極層12積層複數個介電層11之構成。又,於介電層11與內部電極層12之積層體中,於積層方向之最外層配置有內部電極層12,該積層體之上表面及下表面被覆蓋層13覆蓋。覆蓋層13以陶瓷材料為主成分。例如,覆蓋層13之材料與介電層11之陶瓷材料主成分相同。
積層陶瓷電容器100之尺寸例如為長度0.25 mm、寬度0.125 mm、高度0.125 mm,或長度0.4 mm、寬度0.2 mm、高度0.2 mm,或長度0.6 mm、寬度0.3 mm、高度0.3 mm,或長度1.0 mm、寬度0.5 mm、高度0.5 mm,或長度3.2 mm、寬度1.6 mm、高度1.6 mm,或長度4.5 mm、寬度3.2 mm、高度2.5 mm,但並不限定於該等尺寸。
介電層11例如以陶瓷材料為主成分,該陶瓷材料具有以通式ABO
3所示之鈣鈦礦構造。再者,該鈣鈦礦構造包含偏離化學計量組成之ABO
3-α。例如,可使用BaTiO
3(鈦酸鋇)、CaZrO
3(鋯酸鈣)、CaTiO
3(鈦酸鈣)、SrTiO
3(鈦酸鍶)、形成鈣鈦礦構造之Ba
1-x-yCa
xSr
yTi
1-zZr
zO
3(0≦x≦1,0≦y≦1,0≦z≦1)等作為該陶瓷材料。每層介電層11之厚度例如為0.05 μm以上5 μm以下,或0.1 μm以上3 μm以下,或0.2 μm以上1 μm以下。
如圖2所例示,連接於外部電極20a之內部電極層12與連接於外部電極20b之內部電極層12對向的區域係積層陶瓷電容器100中產生電容之區域。因此,將該產生電容之區域稱為電容區域14。即,電容區域14係連接於不同外部電極之鄰接內部電極層12彼此對向之區域。
連接於外部電極20a之內部電極層12彼此對向而未介隔連接於外部電極20b之內部電極層12的區域稱為端部邊緣15。又,連接於外部電極20b之內部電極層12彼此對向而未介隔連接於外部電極20a之內部電極層12的區域亦稱為端部邊緣15。即,端部邊緣15係連接於同一外部電極之內部電極層12對向而未介隔連接於不同外部電極之內部電極層12的區域。端部邊緣15係不產生電容之區域。
如圖3所例示,於積層晶片10中,將積層晶片10之2側面至內部電極層12之區域稱為側邊緣16。即,側邊緣16係上述積層構造中以覆蓋積層之複數個內部電極層12延伸至2側面側之端部之方式設置的區域。側邊緣16亦為不產生電容之區域。
此種積層陶瓷電容器100中,若內部電極層12使用Ni,則有介電層11產生氧缺陷等,導致介電層11之可靠性變差之虞。例如,若於燒成步驟時將氣氛設為還原氣氛以抑制Ni之氧化,則介電層11容易產生氧缺陷。若將已經產生了氧缺陷之介電層11薄層化,施加高電場強度之電壓,則介電層11之耐久性會變得不足。於該情形時,擔心壽命特性變差,例如積層陶瓷電容器100之壽命變短、壽命產生偏差等。因此,本實施方式之積層陶瓷電容器100具有提昇壽命特性之構成。
首先,內部電極層12除包含Ni外,還包含Sn。藉由使內部電極層12包含Ni及Sn,可提昇積層陶瓷電容器100之壽命。例如,認為Ni與Sn之合金化使內部電極層12與介電層11之界面狀態發生了變化,積層陶瓷電容器100之壽命因此得到提昇。
其次,據觀察,若內部電極層12所含之Ni擴散至介電層11,則積層陶瓷電容器100有無法獲得充分壽命的傾向,但其機制尚不明確。因此,要求抑制Ni自內部電極層12擴散至介電層11。因此,本發明者等人就向內部電極層12添加之元素對Ni擴散產生之影響進行了調查。
首先,準備4種樣本。準備如下樣本作為第1樣本:於以鈦酸鋇為主成分之介電坯片上,藉由濺鍍形成由Ni構成之內部電極圖案(厚度200 nm)。準備如下樣本作為第2樣本:於以鈦酸鋇為主成分之介電坯片上印刷3.3 μg之Ni膏。準備如下樣本作為第3樣本:於以鈦酸鋇為主成分之介電坯片上,藉由濺鍍形成包含Ni及Sn之內部電極圖案(Sn為3.2 atm%,厚度200 nm)。準備如下樣本作為第4樣本:於以鈦酸鋇為主成分之介電坯片上,藉由濺鍍形成包含Ni及Au之內部電極圖案(Au為1.0 atm%,厚度200 nm)。
對於各樣本,於氧分壓10
-5atm~10
-8atm之還原氣氛中,於1100℃~1300℃進行燒成,製作樣本。使用La-ICP(laser ablation-Inductively Coupled Plasma,雷射剝蝕感應耦合電漿質量分析),測定介電層中之Ni濃度。由距內部電極層之距離與Ni濃度比即(Ni/Ti) atm%之關係進行測定。
圖4係表示結果之圖。如圖4所示,關於第1樣本~第3樣本,於遠離內部電極層之部位,Ni濃度亦升高了。認為其係燒成時Ni擴散所致。與此相對,關於第4樣本,於遠離內部電極層之部位,Ni濃度變低了。認為其原因在於燒成時Ni之擴散得到了抑制。根據該等結果可確認,藉由向內部電極層添加Au,可抑制Ni向介電層擴散。
因此,本實施方式之內部電極層12包含Ni及Sn,並且包含Au。藉由使內部電極層12進而包含Au,Au具有阻擋Ni擴散之功能,從而進一步抑制Ni向介電層11擴散。藉此,提昇介電層11對於施加高電場強度電壓之耐久性。其結果為,提昇積層陶瓷電容器100之壽命。藉由提昇壽命從而不再具有短壽命,亦抑制了壽命之偏差。因此,使積層陶瓷電容器100之壽命特性提昇。
內部電極層12之厚度例如為0.01 μm以上5 μm以下,或0.05 μm以上3 μm以下,或0.1 μm以上1 μm以下。
再者,若內部電極層12中Sn之含量較少,則有無法充分控制內部電極層12與介電層11之界面之狀態之虞。又,若Au之含量較少,則有無法充分抑制Ni擴散之虞。因此,較佳為對Sn含量與Au含量之合計設定下限。例如,內部電極層12中,相對於Ni而言,Sn含量與Au含量之合計較佳為0.01 at%以上,更佳為0.05 at%以上,進而較佳為0.1 at%以上,進而較佳為0.2 at%以上。
另一方面,若Sn含量與Au含量之合計較多,則有發生熔點降低、成本上升等不良情況之虞。因此,較佳為對Sn含量與Au含量之合計設置上限。例如,內部電極層12中,相對於Ni而言,Sn含量與Au含量之合計較佳為95 at%以下,更佳為50 at%以下,進而較佳為10 at%以下。
再者,若Sn含量與Au含量之合計為0.2 at%以上10 at%以下,則即便Au含量少於Sn含量,亦可控制內部電極層12與介電層11之界面之狀態,並抑制Ni之擴散。因此,從減少Au使用量以降低成本之觀點而言,較佳為Au含量少於Sn含量,只要Sn含量與Au含量之合計為0.2 at%以上10 at%以下即可。
再者,較佳為於內部電極層12之與介電層11之界面附近,Sn濃度變高。其原因在於:決定可靠性之因素並非內部電極層整體,而僅為介電層11與內部電極層12之界面附近。因此,如圖5(a)所例示,較佳為於內部電極層12中,形成如下濃度梯度:於厚度方向之中心部,Sn濃度較低,於與介電層11之界面附近,Sn濃度變高。又,如圖5(b)所例示,較佳為於內部電極層12之與介電層11之界面附近,Au濃度變高。其原因在於:Au濃度高係可有效率地抑制Ni向介電層11擴散之狀態。因此,較佳為於內部電極層12中,形成如下濃度梯度:於積層方向之中心部,Au濃度較低,於與介電層11之界面附近,Au濃度變高。
繼而,對積層陶瓷電容器100之製造方法進行說明。圖6係例示積層陶瓷電容器100之製造方法之流程之圖。
(原料粉末製作步驟)
首先,準備用以形成介電層11之介電體材料。介電層11所包含之A位元素及B位元素通常以ABO
3粒子之燒結體之形式包含於介電層11中。例如,BaTiO
3係具有鈣鈦礦構造之正方晶化合物,表現出高介電常數。一般藉由使二氧化鈦等鈦原料與碳酸鋇等鋇原料發生反應合成鈦酸鋇而可獲得該BaTiO
3。作為介電層11之主成分陶瓷之合成方法,先前已知有各種方法,例如已知固相法、溶膠-凝膠法、水熱法等。於本實施方式中,可採用該等方法中之任一種。
視目的於所得之陶瓷粉末中添加特定之添加化合物。作為添加化合物,可例舉鎂(Mg)、錳(Mn)、釩(V)、鉻(Cr)、稀土類元素(釔(Y)、釤(Sm)、銪(Eu)、釓(Gd)、鋱(Tb)、鏑(Dy)、鈥(Ho)、鉺(Er)、銩(Tm)及鐿(Yb))之氧化物;或包含鈷(Co)、鎳、鋰(Li)、硼(B)、鈉(Na)、鉀(K)或者矽(Si)之氧化物;或包含鈷、鎳、鋰、硼、鈉、鉀或矽之玻璃。
例如將陶瓷原料粉末中包含添加化合物之化合物濕式混合,進行乾燥及粉碎,製備陶瓷材料。例如,亦可視需要對於以上述方式獲得之陶瓷材料進行粉碎處理來調節粒徑,或藉由與分級處理進行組合而調整粒徑。藉由以上步驟,獲得介電體材料。
(積層步驟)
其次,對所得之介電體材料加入聚乙烯醇縮丁醛(PVB)樹脂等黏合劑、乙醇、甲苯等有機溶劑、塑化劑,進行濕式混合。使用所得之漿料,例如藉由模嘴塗佈機法或刮刀法,於基材51上塗佈例如厚度0.5 μm以上1.0 μm以下之介電坯片52並使其乾燥。基材51例如為PET(Polyethylene Terephthalate,聚對苯二甲酸乙二酯)膜。
其次,如圖7(a)所例示,於介電坯片52上成膜內部電極圖案53。圖7(a)中,作為一例,於介電坯片52上隔開特定間隔成膜4層內部電極圖案53。成膜方法並無特別限定,例如可採用:使用包含Ni-Sn-Au之混合物之電極膏;於Ni金屬粉膏中混合包含Au、Sn之成分;使用合金靶進行濺鍍等真空成膜;使用單獨之靶進行同時濺鍍;等等。將成膜有內部電極圖案53之介電坯片52設為積層單元。
其次,將介電坯片52自基材51剝離,並如圖7(b)所例示,將積層單元積層。
其次,於藉由將積層單元積層所得之積層體之上下,積層特定數量(例如2~10層)之覆蓋片材進行熱壓接,切割為特定晶片尺寸(例如1.0 mm×0.5 mm)。圖7(b)之例中,沿虛線切割。覆蓋片材可與介電坯片52為相同成分,亦可添加不同之添加化合物。
(燒成步驟)
於N
2氣氛中對以此種方式所得之陶瓷積層體進行脫黏合劑處理後,以浸漬法塗佈作為外部電極20a、20b之基底層之金屬膏,於氧分壓10
-5~10
-8atm之還原氣氛中,於1100~1300℃燒成10分鐘~2小時。如此,獲得積層陶瓷電容器100。
(再氧化處理步驟)
其後,亦可於N
2氣體氣氛中於600℃~1000℃進行再氧化處理。
(鍍覆處理步驟)
其後,亦可藉由鍍覆處理,於外部電極20a、20b塗覆Cu、Ni、Sn等金屬。
根據本實施方式之製造方法,內部電極層12包含Ni及Sn,還包含Au。藉此,使所得之積層陶瓷電容器100之壽命提昇。藉由提昇壽命,使其不再具有短壽命,亦抑制了壽命之偏差。因此,使積層陶瓷電容器100壽命特性提昇。
再者,於上述各實施方式中,作為陶瓷電子零件之一例,對積層陶瓷電容器進行了說明,但並不限定於此。例如亦可使用變阻器、熱敏電阻等其他電子零件。
[實施例]
以下,製作實施方式之積層陶瓷電容器,對特性進行調查。
(實施例1)
對鈦酸鋇粉末加入添加物,用球磨機充分進行濕式混合粉碎,獲得介電體材料。於介電體材料中加入作為有機黏合劑之丁醛系樹脂、作為溶劑之甲苯、以及乙醇,用刮刀法於PET之基材上塗佈介電坯片。介電坯片之厚度設為1.0 μm。
其次,使用包含Ni-Sn-Au合金之膏,於介電坯片上成膜內部電極圖案。以原子比計,Ni/Sn/Au比設為96/2/2。
其次,將介電坯片自基材剝離,並將積層單元積層。積層時之溫度設為80℃。將積層單元積層後,施加4 MPa之壓力進行加壓。加壓時間設為5秒。其次,於藉由將積層單元積層所得之積層體之上下積層特定數量之覆蓋片材,以均壓進行熱壓接。均壓之壓力設為120 MPa,溫度設為100℃,加壓時間設為25秒。其後,切割為特定晶片尺寸(1.0 mm×0.5 mm×0.5 mm)。
於N
2氣氛中對以此種方式所得之陶瓷積層體進行脫黏合劑處理後,以浸漬法塗佈作為外部電極之基底層之金屬膏,於還原氣氛下進行燒成。
(實施例2)
將Ni/Sn/Au之原子比改為99.6/0.2/0.2,除此以外,於與實施例1相同之製造條件下製作積層陶瓷電容器。
(實施例3)
將Ni/Sn/Au之原子比改為80/10/10,除此以外,於與實施例1相同之製造條件下製作積層陶瓷電容器。
(比較例1)
未於內部電極層中添加Sn或Au。其他製造條件與實施例1相同。
(比較例2)
於內部電極層中添加與實施例1相同濃度之Au,但未添加Sn。其他製造條件與實施例1相同。
(比較例3)
於內部電極層中添加與實施例1相同濃度之Sn,但未添加Au。其他製造條件與實施例1相同。
(壽命試驗)
對於實施例1~3及比較例1~3,分別測定複數個樣本發生故障時所經過之時間。測定方法為測定於150℃/18 V/μm之直流電場下,洩漏電流成為最小洩漏電流之10倍時所經過之時間。
圖8係針對實施例1~3及比較例1~3,分別表示發生故障時所經過之時間與累計故障率之關係的魏普圖。表1表示圖8之魏普圖之斜率。又,表1對於實施例1~3及比較例1~3,分別表示樣本個數之50%發生故障之時間。
[表1]
比較例1 | 比較例2 | 比較例3 | 實施例1 | 實施例2 | 實施例3 | |
斜率 | 0.81 | 3.00 | 4.88 | 5.73 | 5.44 | 6.26 |
50%故障時間 (min) | 530 | 6159 | 4511 | 17163 | 15387 | 18314 |
如圖8及表1所示,比較例1中,魏普圖之斜率平緩,短壽命之樣本較多。又,樣本間壽命差異較大。認為其原因在於:內部電極層未包含Sn或Au。比較例2與比較例1相比雖然壽命更長,但未獲得充分之壽命。認為其原因在於:僅於內部電極層之Ni中添加了Sn而未添加Au,故未能充分抑制Ni之擴散。比較例3與比較例1相比雖然壽命更長,但未充分獲得充分之壽命。認為其原因在於:僅於內部電極層之Ni中添加了Au而未添加Sn,故未能充分控制內部電極層與介電層之界面。
與此相對,實施例1~3中,每個樣本之壽命均足夠長。又,魏普圖之斜率較大,壽命之偏差亦得到了抑制。認為其原因在於:內部電極層不僅包含Ni,還同時包含Sn及Au。
對於實施例1及比較例2、3,使用La-ICP測定介電層中之Ni濃度。圖9(a)係表示比較例3之結果之圖。圖9(b)係表示比較例2之結果之圖。圖9(c)係表示實施例1之結果之圖。如圖9(a)所示,於未對內部電極層添加Au之情形時,大量Ni擴散至介電層中。與此相對,如圖9(b)所示,於對內部電極層添加Au來代替Sn時,Ni向介電層擴散之量得到了抑制。進而,如圖9(c)所示,可知當對內部電極層中添加Sn與Au兩者時,Ni向介電層擴散之量進一步得到了抑制。如此可知,藉由使內部電極層包含Sn及Au兩者,可進一步抑制Ni向介電層擴散。認為該等結果係得到表1之結果之原因。
以上,對本發明之實施例進行了詳細敍述,但本發明並不限定於該特定實施例,可於申請專利範圍所記載之本發明之主旨之範圍內進行各種變化、變更。
10:積層晶片
11:介電層
12:內部電極層
13:覆蓋層
14:電容區域
15:端部邊緣
16:側邊緣
20a:外部電極
20b:外部電極
51:基材
52:介電坯片
53:內部電極圖案
100:積層陶瓷電容器
圖1係積層陶瓷電容器之局部剖視立體圖。
圖2係圖1之A-A線剖視圖。
圖3係圖1之B-B線剖視圖。
圖4係表示向內部電極層添加之元素對Ni之擴散產生之影響的圖。
圖5(a)係例示內部電極層中之Sn濃度之圖,(b)係例示內部電極層中之Au濃度之圖。
圖6係例示積層陶瓷電容器之製造方法之流程的圖。
圖7(a)及(b)係例示積層步驟之圖。
圖8係針對實施例及比較例,表示至發生故障時所經過之時間與累計故障率之關係的魏普圖。
圖9(a)~(c)係表示介電層中之Ni濃度之圖。
10:積層晶片
11:介電層
12:內部電極層
13:覆蓋層
20a:外部電極
20b:外部電極
100:積層陶瓷電容器
Claims (8)
- 一種陶瓷電子零件,其特徵在於具備積層晶片,該積層晶片積層有以陶瓷為主成分之複數個介電層、及複數個內部電極層, 上述內部電極層包含Ni、Sn、Au。
- 如請求項1之陶瓷電子零件,其中於上述內部電極層中,相對於Ni而言,Sn含量與Au含量之合計為0.01 at%以上95 at%以下。
- 如請求項2之陶瓷電子零件,其中於上述內部電極層中,相對於Ni而言,Sn含量與Au含量之合計為0.2 at%以上10 at%以下。
- 如請求項1至3中任一項之陶瓷電子零件,其中於上述內部電極層中,Au含量少於Sn含量。
- 如請求項1至3中任一項之陶瓷電子零件,其中於上述內部電極層中,與厚度方向之中心部相比,Sn之濃度在與上述介電層之界面附近更高。
- 如請求項1至3中任一項之陶瓷電子零件,其中於上述內部電極層中,與積層方向之中心部相比,Au之濃度在與上述介電層之界面附近更高。
- 一種陶瓷電子零件之製造方法,其特徵在於包括如下步驟:藉由於介電坯片上形成包含Ni、Sn、Au之內部電極圖案而形成積層單元; 藉由積層複數個上述積層單元而形成積層體;及 燒成上述積層體。
- 如請求項7之陶瓷電子零件之製造方法,其中形成上述積層單元之步驟係藉由真空成膜製程於上述介電坯片成膜上述內部電極圖案的步驟。
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