TWI537998B - Laminated ceramic capacitors - Google Patents
Laminated ceramic capacitors Download PDFInfo
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- TWI537998B TWI537998B TW103107767A TW103107767A TWI537998B TW I537998 B TWI537998 B TW I537998B TW 103107767 A TW103107767 A TW 103107767A TW 103107767 A TW103107767 A TW 103107767A TW I537998 B TWI537998 B TW I537998B
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- 239000003985 ceramic capacitor Substances 0.000 title claims description 50
- 239000000919 ceramic Substances 0.000 claims description 85
- 239000003990 capacitor Substances 0.000 claims description 33
- 239000000203 mixture Substances 0.000 claims description 19
- 150000001875 compounds Chemical class 0.000 claims description 16
- 229910052702 rhenium Inorganic materials 0.000 claims description 7
- 229910052719 titanium Inorganic materials 0.000 claims description 6
- 229910052726 zirconium Inorganic materials 0.000 claims description 6
- 229910052788 barium Inorganic materials 0.000 claims description 4
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 3
- 229910052746 lanthanum Inorganic materials 0.000 claims description 3
- 229910052684 Cerium Inorganic materials 0.000 claims description 2
- 229910052779 Neodymium Inorganic materials 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 229910052789 astatine Inorganic materials 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 229910052748 manganese Inorganic materials 0.000 claims description 2
- 229910052712 strontium Inorganic materials 0.000 claims description 2
- 229910052720 vanadium Inorganic materials 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims 9
- JTCFNJXQEFODHE-UHFFFAOYSA-N [Ca].[Ti] Chemical compound [Ca].[Ti] JTCFNJXQEFODHE-UHFFFAOYSA-N 0.000 claims 1
- 229910052500 inorganic mineral Inorganic materials 0.000 claims 1
- 239000011707 mineral Substances 0.000 claims 1
- 239000000843 powder Substances 0.000 description 31
- 239000002994 raw material Substances 0.000 description 28
- 238000007747 plating Methods 0.000 description 13
- 238000000034 method Methods 0.000 description 9
- 238000009616 inductively coupled plasma Methods 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 7
- 239000004020 conductor Substances 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 5
- 238000010183 spectrum analysis Methods 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 4
- 230000005684 electric field Effects 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 229910000881 Cu alloy Inorganic materials 0.000 description 3
- 229910000990 Ni alloy Inorganic materials 0.000 description 3
- -1 and Sm) Inorganic materials 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 238000000295 emission spectrum Methods 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229910000679 solder Inorganic materials 0.000 description 2
- 229910001233 yttria-stabilized zirconia Inorganic materials 0.000 description 2
- 229910001316 Ag alloy Inorganic materials 0.000 description 1
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 229910020203 CeO Inorganic materials 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
- 229910052689 Holmium Inorganic materials 0.000 description 1
- 229910021193 La 2 O 3 Inorganic materials 0.000 description 1
- 101100513612 Microdochium nivale MnCO gene Proteins 0.000 description 1
- 229910017493 Nd 2 O 3 Inorganic materials 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- 229910052775 Thulium Inorganic materials 0.000 description 1
- 229910052769 Ytterbium Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 238000000992 sputter etching Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
- H01G4/06—Solid dielectrics
- H01G4/08—Inorganic dielectrics
- H01G4/12—Ceramic dielectrics
- H01G4/1209—Ceramic dielectrics characterised by the ceramic dielectric material
- H01G4/1236—Ceramic dielectrics characterised by the ceramic dielectric material based on zirconium oxides or zirconates
- H01G4/1245—Ceramic dielectrics characterised by the ceramic dielectric material based on zirconium oxides or zirconates containing also titanates
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
- C04B35/49—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates
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- H01G4/00—Fixed capacitors; Processes of their manufacture
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- H—ELECTRICITY
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- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
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- H01G4/1218—Ceramic dielectrics characterised by the ceramic dielectric material based on titanium oxides or titanates
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- H01G4/1236—Ceramic dielectrics characterised by the ceramic dielectric material based on zirconium oxides or zirconates
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- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/228—Terminals
- H01G4/248—Terminals the terminals embracing or surrounding the capacitive element, e.g. caps
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- H01G4/30—Stacked capacitors
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Description
本發明係關於一種於例如車載用之高溫環境下使用之積層陶瓷電容。
積層陶瓷電容之高溫側之保證溫度係基於絕緣性及高溫負荷可靠性(高溫負荷試驗中之壽命)決定。一般而言，該保證溫度於一般民生用中設為85℃，於必需高可靠性之產業機械用中設為125℃。
另一方面，近年來，於產業機械用之中，亦對車載用等之高溫環境下所使用之積層陶瓷電容要求150~175℃之更高溫度下之高溫負荷可靠性。
適用於滿足此種要求之積層陶瓷電容之介電陶瓷組合物例如記載於日本專利特開2011-207630號公報(專利文獻1)。專利文獻1中所記載之介電陶瓷組合物係以組成式：100(Ba1-xCax)TiO3+aR2O3+bV2O5+cZrO2+dMnO(其中，R為選自Y、La、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm及Yb中之至少1種金屬元素，a、b、c及d表示莫耳比)表示，並且滿足0.03≦x≦0.20、0.05≦a≦3.50、0.22≦b≦2.50、0.05≦c≦3.0、及0.01≦d≦0.30之各條件。
使用上述介電陶瓷組合物之積層陶瓷電容於在溫度175℃下施加電場強度20V/μm之直流電壓之高溫負荷試驗中，確認到具有MTTF(Mean Time To Failure：故障前平均時間)為50小時以上之優異之高溫負荷可靠性。
[專利文獻1]日本專利特開2011-207630號公報
假定將車載用積層陶瓷電容用作始終為高溫環境之引擎室內所搭載之電氣機器之零件。例如，搭載於引擎之氣缸頭附近之ECU(Electronic Control Unit：電子控制裝置)等所使用之積層陶瓷電容尤其存在暴露於高溫下之可能性。關於此種積層陶瓷電容，存在要求200℃以上之更高之保證溫度之情形。
然而，使用專利文獻1中記載之介電陶瓷組合物之積層陶瓷電容於上述高溫下之高溫負荷可靠性尚未得到證實。
因此，本發明之目的在於欲提供一種即便於例如車載用之高溫環境下使用之情形時，高溫負荷可靠性亦優異之積層陶瓷電容。
為了解決上述問題，本發明之積層陶瓷電容謀求對用於介電陶瓷層之介電陶瓷組合物進行改良。
本發明之積層陶瓷電容包含電容本體及複數個外部電極。電容本體係包含經積層之複數個介電陶瓷層、及沿著介電陶瓷層間之界面形成之複數個內部電極而構成。複數個外部電極形成於電容本體之外表面上之彼此不同之位置，且電性連接於內部電極。
並且，介電陶瓷層包含作為元素之Ba、Re(其中，Re為選自La、Ce、Pr、Nd及Sm中之至少1種元素)、Ti、Zr、M(其中，M為選自Mg、Al、Mn及V中之至少1種元素)、Si、及任意之Sr。
並且，介電陶瓷層包含作為化合物之鈣鈦礦型化合物，該鈣鈦礦型化合物在構成上係包含Ba、Re、Ti、Zr、及任意之Sr。
進而，以莫耳份表示介電陶瓷層中所含之元素之量之情形時，將Ti之量及Zr之量之合計設為100時，Sr之量a滿足0≦a≦20.0之條件、Re之量b滿足0.5≦b≦10.0之條件、Zr之量c滿足46≦c≦90之條件、M之量d滿足0.5≦d≦10.0之條件、Si之量e滿足0.5≦e≦5.0之條件、且Ba之量及Sr之量及Re之量之合計相對於Ti之量及Zr之量之合計的比m滿足0.990≦m≦1.050之條件(以下稱為第1條件)。
上述積層陶瓷電容於進行在溫度200℃下施加電場強度為15V/μm之直流電壓之高溫負荷試驗之情形時，具有MTTF為100小時以上之優異之高溫負荷可靠性。又，介電陶瓷之相對介電常數(εr)為70以上。
又，關於本發明之積層陶瓷電容，以莫耳份表示介電陶瓷層中所含之元素之量之情形時，將Ti之量及Zr之量之合計設為100時，亦可使Sr之量a滿足0≦a≦20.0之條件、Re之量b滿足0.5≦b≦5.0之條件、Zr之量c滿足46≦c≦80之條件、M之量d滿足0.5≦d≦5.0之條件、Si之量e滿足1.0≦e≦3.0之條件、且Ba之量及Sr之量及Re之量之合計相對於Ti之量及Zr之量之合計的比m滿足0.990≦m≦1.050之條件(以下稱為第2條件)。
上述積層陶瓷電容具有上述優異之高溫負荷可靠性，進而介電陶瓷之εr為100以上。
又，關於本發明之積層陶瓷電容，以莫耳份表示介電陶瓷層中所含之元素之量之情形時，將Ti之量及Zr之量之合計設為100時，亦可使Sr之量a滿足0≦a≦20.0之條件、Re之量b滿足1.0≦b≦5.0之條件、Zr之量c滿足60≦c≦80之條件、M之量d滿足1.0≦d≦5.0之條件、Si之量e滿足1.0≦e≦3.0之條件、且Ba之量及Re之量及Sr之量之合計相對於Ti之量及Zr之量之合計的比m滿足1.010≦m≦1.040之條件(以下稱為第3條件)。
上述積層陶瓷電容於進行上述條件下之高溫負荷試驗之情形時，具有MTTF為150小時以上之更優異之高溫負荷可靠性，介電陶瓷之εr為100以上。
本發明之積層陶瓷電容於進行在溫度200℃下施加電場強度為15V/μm之直流電壓之高溫負荷試驗之情形時，具有MTTF為100小時以上之優異之高溫負荷可靠性。又，介電陶瓷之εr為70以上。
1‧‧‧積層陶瓷電容
2‧‧‧電容本體
3‧‧‧介電陶瓷層
4、5‧‧‧內部電極
6、7‧‧‧電容本體之兩端面
8、9‧‧‧外部電極
OL‧‧‧與介電陶瓷層正交之線(正交線)
圖1係表示本發明之實施形態之積層陶瓷電容1之外觀之立體圖。
圖2係圖1所示之積層陶瓷電容1之正面剖面圖。
圖3係用以說明圖1所示之積層陶瓷電容1之介電陶瓷層3的厚度之測定方法之圖。
-實施形態-
以下展示本發明之實施形態，進而詳細地說明本發明之特徵之處。
<積層陶瓷電容之構造>
積層陶瓷電容1包含電容本體2。電容本體2係包含經積層之複數個介電陶瓷層3、及沿著複數個介電陶瓷層3之間的複數個界面分別形成之複數個內部電極4及5。
內部電極4及5係以到達電容本體2之外表面之方式形成。於本發明之實施形態中，內部電極4係以到達電容本體2之一端之端面6之方式形成，內部電極5係以到達另一端之端面7之方式形成。又，內部電極4及內部電極5交替地配置於電容本體2之內部。
於電容本體2之外表面上且為端面6及7上分別形成有外部電極8
及9。視需要亦可於外部電極8及9上分別形成包含Ni、Cu等之第1鍍敷層。亦可進而於其上分別形成包含焊料、Sn等之第2鍍敷層。
於此種積層陶瓷電容1中，介電陶瓷層3中所含之元素之種類及化合物、元素之量滿足本發明中所規定之各條件。
<積層陶瓷電容之製造>
其次，按照製造步驟順序對上述積層陶瓷電容1之製造方法進行說明。
準備用於介電陶瓷組合物之原料粉末，使之漿料化，將該漿料成形為片狀，獲得用於介電陶瓷層3之生片。此處，作為介電陶瓷原料粉末，如以下詳細說明，使用用於本發明之介電陶瓷組合物之原料粉末。
關於該介電陶瓷之原料粉末之製造方法，若介電陶瓷層3中所含之元素之種類及化合物、元素之量滿足本發明中所規定之各條件，則可使用任意之方法。所使用之原材料亦可使用碳酸鹽、氧化物、氫氧化物、氯化物等各種形態者。
例如，作為鈣鈦礦型化合物粉末之製造方法(合成方法)，除了將包含碳酸鹽或氧化物之原材料混合並預燒合成之固相法，亦可使用水熱法等各種公知之方法。又，亦可以成為所需之鈣鈦礦型化合物之組成之方式，將藉由水熱法等製作之BaTiO3或BaZrO3與各種原材料混合後進行預燒，而製造鈣鈦礦型化合物粉末。
又，作為介電陶瓷之原料粉末，亦可為將藉由水熱法等製作之BaTiO3或BaZrO3與各種原材料混合而成者。並且，亦可於電容本體之煅燒時使其等進行反應，合成在構成上包含Ba、Re、Ti、Zr、及任意之Sr之鈣鈦礦型化合物。
於獲得之生片之特定者之各一主面形成內部電極4及5。構成內部電極4及5之導電性材料可使用Ni、Ni合金、Cu、及Cu合金等。通
常使用Ni或Ni合金。該等內部電極4及5通常係使用包含上述導電性材料粉末之導電膏，利用網版印刷法或轉印法形成。內部電極4及5並未限定於此，可利用任意之方法形成。
將形成有內部電極4或5之用於介電陶瓷層3之生片積層必需之數量，並且使該等生片成為夾於未形成內部電極之適當數量之生片間的狀態。藉由對其進行熱壓接合，獲得生電容本體。
將該生電容本體於特定之還原性氣氛中，以特定之溫度進行煅燒，獲得燒結後之電容本體2。
於燒結後之電容本體2之兩端面6及7上，以分別與內部電極4及5電性連接之方式形成外部電極8及9。構成該等外部電極8及9之導電性材料可使用Ni、Ni合金、Cu、Cu合金、Ag或Ag合金等。通常使用Cu或Cu合金。外部電極8及9通常藉由將於導電性材料粉末中添加玻璃料而獲得之導電膏塗佈於電容本體2之兩端面6及7上，並將其燒接而形成。
再者，亦可預先將應成為外部電極8及9之導電膏塗佈於煅燒前之生電容本體，與用以獲得電容本體2之煅燒同時進行燒接。
其次，於外部電極8及9上，視需要實施Ni、Cu等之鍍敷，形成第1鍍敷層。又，於該等第1鍍敷層上實施Sn、焊料等之鍍敷，形成第2鍍敷層。如上，完成積層陶瓷電容1。
-實驗例-
其次，基於實驗例對本發明進行更具體之說明。該等實驗例亦為用以提供規定本發明之積層陶瓷電容之介電陶瓷層中所含之元素之量之條件、或元素之量之較佳條件的根據者。實驗例中，製作如圖1及圖2所示之積層陶瓷電容作為試樣。
<介電陶瓷原料粉末之製造>
準備構成介電陶瓷層中所含之鈣鈦礦型化合物之各粉末，即，
作為Ba之原材料之BaCO3，作為Sr之原材料之SrCO3，作為Re之原材料之La2O3、CeO2、Pr6O11、Nd2O3及Sm2O3，作為Ti之原材料之TiO2，及作為Zr之原材料之ZrO2。各粉末使用純度99重量%以上者。
將該等各粉末以如下方式進行稱量、調製，即，以莫耳份表示各元素之量之情形時，Ba之量及Sr之量及Re之量之合計相對於Ti之量及Zr之量之合計的比m、Sr之量a、Re之量b、Zr之量c、Ba之量、及Ti之量成為表1及表2所示之值。調製時，根據各粉末之純度進行調製量之修正。
將該等調製原料粉末使用球磨機進行濕式混合，使之均勻地分散後進行乾燥，並實施壓碎處理而獲得調整粉末。將獲得之調整粉末於1050℃下進行預燒，獲得鈣鈦礦型化合物粉末。
另一方面，準備MgCO3、Al2O3、MnCO3、及V2O5之各粉末作為介電陶瓷層中所含之M之原材料。又，準備SiO2之粉末作為Si之原材料。各粉末使用純度99重量%以上者。
其次，將該等各粉末及上述鈣鈦礦型化合物粉末以如下方式進行稱量、調製，即，以莫耳份表示各元素之量之情形時，將Ti之量及Zr之量之合計設為100時，M之量d、及Si之量e成為表1及表2所示之值。調製時，根據各粉末之純度進行調製量之修正。
再者，為了調整鈣鈦礦型化合物中之Ba之量及Sr之量及Re之量之合計相對於Ti之量及Zr之量之合計的比m，亦可於將鈣鈦礦型化合物粉末及M之原材料及Si之原材料進行混合之階段添加BaCO3、SrCO3、TiO2、及ZrO2等原材料。
將該等調製原料粉末使用球磨機進行濕式混合，均勻地分散後進行乾燥，並實施壓碎處理而獲得介電陶瓷之原料粉末。
又，於上述濕式混合之過程中，將YSZ(Yttria Stabilized Zirconia：氧化釔穩定化氧化鋯)球用作介質之情形等時，存在自稱量
之原材料以外混入ZrO2之情況。於該情形時，以包括混入量在內成為表1及表2之組成之方式調整ZrO2粉末之調製量。
於該等介電陶瓷之原料粉末中，有可能包含作為不可避免之雜質之Ca及Hf，利用其他途徑確認對本發明之效果不產生影響。
將獲得之介電陶瓷之原料粉末藉由酸進行溶解，並進行ICP發射光譜分析。所謂「ICP發射光譜分析」，為Inductively Coupled Plasma(高頻電感耦合電漿)發射光譜分析之略稱。
其結果，確認到介電陶瓷之原料粉末具有與表1及表2所示之組成實質上相同之組成。
<積層陶瓷電容之製造>
於該等介電陶瓷原料粉末中添加聚乙烯丁醛系黏合劑、塑化劑及乙醇等有機溶劑，利用球磨機進行濕式混合，獲得包含介電陶瓷組合物之漿料。將該等漿料於包含聚對苯二甲酸乙二酯之承載膜上成形為片狀，獲得包含介電陶瓷組合物之生片。
使用將Ni作為導電性材料之導電膏，於獲得之生片上印刷內部電極圖案。將該等生片相互對向，以構成複數個靜電電容之方式堆積，進而於其上下表面堆積適當數量之未形成內部電極圖案之陶瓷生片並熱壓接合，獲得生電容本體。
將獲得之生電容本體於大氣中以溫度290℃保持3小時，使黏合劑燃燒。將使黏合劑燃燒後之電容本體於還原性氣氛中以溫度1150~1250℃保持2小時並煅燒，獲得經燒結之電容本體。於還原性氣氛中使用N2-H2-H2O之混合氣體。將氧分壓PO2設定為於上述溫度下內部電極中所含之Ni不會氧化之10-12~10-9MPa。
將Cu作為導電性材料，於經燒結之電容本體之兩端面塗佈含有B2O3-SiO2-BaO系玻璃料之導電膏，於N2氣氛中，以溫度800℃進行燒接，藉此形成與內部電極電性連接之外部電極。
其後，藉由滾筒鍍敷(barrel plating)，於外部電極之表面形成Ni鍍敷層(第1鍍敷層)，進而於Ni鍍敷層上形成Sn鍍敷層(第2鍍敷層)。
藉由以上之步驟，獲得試樣編號1~68之試樣之積層陶瓷電容。
以此方式所獲得之各試樣之積層陶瓷電容之外形尺寸係寬度為1.0mm，長度為2.0mm，及厚度為1.0mm。又，與取得靜電電容相關之介電陶瓷層之數量為85，每層之對向電極面積為1.6mm2。
又，將除去所獲得之各試樣之積層陶瓷電容之外部電極後之電容本體藉由酸進行溶解，並進行ICP發射光譜分析。再者，將電容本體進行溶解處理而製成溶液之方法並無特別制約。
於上述方法中，由於將介電陶瓷層及內部電極同時溶解，故於分析時，除了介電陶瓷層中所含之元素以外，亦檢測出內部電極中所含之元素。因此，根據上述ICP發射光譜分析之結果，將除去既知之內部電極中所含之元素而得者視作對將介電陶瓷層溶解處理而成之溶液進行ICP發射光譜分析之結果。又，其結果，將以莫耳份表示所檢測出之元素者視作介電陶瓷層中所含之元素之量。
其結果，確認到介電陶瓷層具有與表1及表2所示之調製組成實質上相同之組成。
因而，本發明之積層陶瓷電容之介電陶瓷層中所含之元素之種類、及元素之量之條件或元素之量之較佳條件係基於表1及表2所示之組成而規定。
<介電陶瓷層之厚度之測定>
將如上所述製作之試樣編號1~68之試樣之積層陶瓷電容各試樣各準備3個。
以寬度(W)方向沿著垂直方向之狀態保持各試樣之3個積層陶瓷電容，以樹脂加固試樣之周圍，使根據試樣之長度(L)及厚度(T)而規定之LT面自樹脂露出。其後，利用研磨機，研磨各試樣之LT面，進
行研磨直至達到各試樣之寬度(W)方向之1/2程度之深度。並且，為了去除由研磨引起之內部電極之延伸，藉由離子研磨(ion milling)加工研磨表面。
對於獲得之研磨後之試樣，如圖3所示，於LT剖面之L方向之1/2程度之位置拉出與介電陶瓷層3正交之線(正交線)OL。將積層有與取得靜電電容相關之介電陶瓷層3之區域於厚度(T)方向分割為3等分，分為上部區域、中央區域、下部區域之3個區域。
繼而，除掉各區域之最外之介電陶瓷層3、及由於內部電極缺損而關連觀察到2層以上之介電陶瓷層3之部分，於各區域中央部，將上述正交線OL上之介電陶瓷層之厚度分別各測定10層並求平均值。即，由於對3個試樣之3個區域之10層進行測定，故而用以求出平均值之資料數為90。其結果，於試樣編號1~68之各試樣中，介電陶瓷層之厚度為10.0μm。再者，介電陶瓷層之厚度係使用掃描型電子顯微鏡而測定。
<介電陶瓷之εr之測定>
將如上所述製作之試樣編號1~68之試樣之積層陶瓷電容各試樣各準備20個。
使用阻抗分析儀(Agilent Technologies公司製造：HP4194A)，於溫度25±2℃下施加電壓為1Vrms、頻率為1kHz之交流電壓而測定各試樣之20個之積層陶瓷電容之靜電電容(C)，求出平均值。由獲得之C之平均值、內部電極面積、及上述獲得之介電陶瓷層之厚度算出介電陶瓷之εr。
<積層陶瓷電容之高溫負荷可靠性之測定>
將如上所述製作之試樣編號1~68之試樣之積層陶瓷電容各試樣各準備100個。
關於各試樣之100個積層陶瓷電容，假定將其用於搭載於引擎之
氣缸頭附近之ECU，進行於溫度200℃下施加電壓為150V之直流電壓之高溫負荷試驗，測定其等之電阻值之經時變化。施加於介電陶瓷層之電場強度由上述所得之介電陶瓷層之厚度及施加電壓計算為15kV/mm。關於各試樣之100個積層陶瓷電容，以電阻值成為1MΩ以下之時間為故障時間，根據故障時間之維伯分析(Weibull Analysis)求出各試樣之MTTF。
將煅燒後之介電陶瓷層中所含之元素之種類及元素之量、εr、及高溫負荷試驗中之MTTF之測定結果匯總示於表1及表2。
於表1及表2中，試樣編號附帶有＊者為不符合本發明之積層陶瓷電容之介電陶瓷層中所含之元素之量之條件之試樣。
如表1及表2所示，介電陶瓷層中所含之元素之量滿足第1條件之各試樣於上述條件下進行高溫負荷試驗之情形時，確認到具有MTTF為100小時以上之優異之高溫負荷可靠性，介電陶瓷之εr為70以上。
又，介電陶瓷層中所含之元素之量滿足第2條件之各試樣具有上述優異之高溫負荷可靠性，進而介電陶瓷之εr為100以上，故而較佳。
又，介電陶瓷層中所含之元素之量滿足第3條件之各試樣於上述條件下進行高溫負荷試驗之情形時，具有MTTF為150小時以上之更優異之高溫負荷可靠性，且介電陶瓷之εr為100以上，故而更佳。
與此相對，於介電陶瓷層中所含之元素之量未滿足第1條件至第3條件之任一條件之試樣中，確認到高溫負荷可靠性或εr之至少任一者為欠佳之結果。
於上述實驗例中，為了進行介電陶瓷層中所含之元素之量之分析，將除去各試樣之積層陶瓷電容之外部電極後之電容本體藉由酸進行溶解，並除去既知之內部電極中所含之元素，將由此所得者視作對將介電陶瓷層溶解處理而成之溶液進行ICP發射光譜分析之結果。
亦可代替上述方法，例如藉由自電容本體剝離介電陶瓷層等方法，將介電陶瓷層與內部電極分離而取出後，藉由酸進行溶解，並進行ICP發射光譜分析。
再者，本發明並非限定於上述實施形態者，關於構成電容本體之介電陶瓷層或內部電極之層數、介電陶瓷之組成等，可於本發明之範圍內添加各種應用、變化。
1‧‧‧積層陶瓷電容
2‧‧‧電容本體
3‧‧‧介電陶瓷層
4‧‧‧內部電極
5‧‧‧內部電極
6‧‧‧電容本體之兩端面
7‧‧‧電容本體之兩端面
8‧‧‧外部電極
9‧‧‧外部電極
Claims (3)
- 一種積層陶瓷電容，其包含：電容本體，其係包含經積層之複數個介電陶瓷層、及沿著上述介電陶瓷層間之界面形成之複數個內部電極，以及複數個外部電極，其形成於上述電容本體之外表面上之彼此不同之位置，且電性連接於上述內部電極，且上述介電陶瓷層包含作為元素之Ba、Re(其中，Re為選自La、Ce、Pr、Nd及Sm中之至少1種元素)、Ti、Zr、M(其中，M為選自Mg、Al、Mn及V中之至少1種元素)、Si、及任意之Sr，且包含作為化合物之鈣鈦礦型化合物，該鈣鈦礦型化合物在構成上係包含Ba、Re、Ti、Zr、及任意之Sr，以莫耳份表示上述介電陶瓷層中所含之元素之量之情形時，將Ti之量及Zr之量之合計設為100時，Sr之量a滿足0≦a≦20.0之條件、Re之量b滿足0.5≦b≦10.0之條件、Zr之量c滿足46≦c≦90之條件、M之量d滿足0.5≦d≦10.0之條件、Si之量e滿足0.5≦e≦5.0之條件、且Ba之量及Sr之量及Re之量之合計相對於Ti之量及Zr之量之合計的比m滿足0.990≦m≦1.050之條件。
- 如請求項1之積層陶瓷電容，其中以莫耳份表示上述介電陶瓷層中所含之元素之量之情形時，將Ti之量及Zr之量之合計設為100時，Sr之量a滿足0≦a≦20.0之條件、Re之量b滿足0.5≦b≦5.0之條件、 Zr之量c滿足46≦c≦80之條件、M之量d滿足0.5≦d≦5.0之條件、Si之量e滿足1.0≦e≦3.0之條件、且Ba之量及Sr之量及Re之量之合計相對於Ti之量及Zr之量之合計的比m滿足0.990≦m≦1.050之條件。
- 如請求項2之積層陶瓷電容，其中以莫耳份表示上述介電陶瓷層本體中所含之元素之量之情形時，將Ti之量與Zr之量之合計設為100時，Sr之量a滿足0≦a≦20.0之條件、Re之量b滿足1.0≦b≦5.0之條件、Zr之量c滿足60≦c≦80之條件、M之量d滿足1.0≦d≦5.0之條件、Si之量e滿足1.0≦e≦3.0之條件、且Ba之量及Sr之量及Re之量之合計相對於Ti之量及Zr之量之合計的比m滿足1.010≦m≦1.040之條件。
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