TW202102554A - 陶瓷生片用樹脂組成物、陶瓷生片及積層陶瓷電容器 - Google Patents
陶瓷生片用樹脂組成物、陶瓷生片及積層陶瓷電容器 Download PDFInfo
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- TW202102554A TW202102554A TW109110654A TW109110654A TW202102554A TW 202102554 A TW202102554 A TW 202102554A TW 109110654 A TW109110654 A TW 109110654A TW 109110654 A TW109110654 A TW 109110654A TW 202102554 A TW202102554 A TW 202102554A
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- ceramic green
- resin
- resin composition
- green sheets
- polyvinyl acetal
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- 239000000919 ceramic Substances 0.000 title claims abstract description 120
- 239000011342 resin composition Substances 0.000 title claims abstract description 68
- 239000003985 ceramic capacitor Substances 0.000 title claims abstract description 12
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- 238000005481 NMR spectroscopy Methods 0.000 claims description 3
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- 230000007547 defect Effects 0.000 abstract 1
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- 229910052738 indium Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- YDZQQRWRVYGNER-UHFFFAOYSA-N iron;titanium;trihydrate Chemical group O.O.O.[Ti].[Fe] YDZQQRWRVYGNER-UHFFFAOYSA-N 0.000 description 1
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 229910052747 lanthanoid Inorganic materials 0.000 description 1
- 150000002602 lanthanoids Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 229940098779 methanesulfonic acid Drugs 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
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- 125000001421 myristyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 125000001400 nonyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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- 125000002958 pentadecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000001147 pentyl group Chemical group C(CCCC)* 0.000 description 1
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- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
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- 239000011029 spinel Substances 0.000 description 1
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- 238000003860 storage Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- 150000003505 terpenes Chemical class 0.000 description 1
- 235000007586 terpenes Nutrition 0.000 description 1
- 229940116411 terpineol Drugs 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229920002803 thermoplastic polyurethane Polymers 0.000 description 1
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- 150000003568 thioethers Chemical class 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 125000002889 tridecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 125000002948 undecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- HGBOYTHUEUWSSQ-UHFFFAOYSA-N valeric aldehyde Natural products CCCCC=O HGBOYTHUEUWSSQ-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Abstract
本發明提供一種陶瓷生片用樹脂組成物、及使用該陶瓷生片用樹脂組成物之陶瓷生片及積層陶瓷電容器,該陶瓷生片用樹脂組成物能夠製作即便於製成薄層時亦具有較高之機械強度、不易產生切斷後之外觀不良或乾燥後之尺寸變化之陶瓷生片。
本發明係一種陶瓷生片用樹脂組成物,其含有聚乙烯縮醛樹脂,陶瓷生片用樹脂組成物之tanδ之峰頂為1.25以上,且損失彈性模數E''為2.30×108
Pa以上。
Description
本發明係關於一種陶瓷生片用樹脂組成物、及使用該陶瓷生片用樹脂組成物之陶瓷生片及積層陶瓷電容器,該陶瓷生片用樹脂組成物能夠製作即便於製成薄層之情形時亦具有較高之機械強度、不易產生切斷後之外觀不良或乾燥後之尺寸變化之陶瓷生片。
近年來,搭載於各種電子機器之電子零件之小型化、積層化不斷發展,多層電路基板、積層線圈、積層陶瓷電容器等積層型電子零件被廣泛使用。
其中,積層陶瓷電容器通常經由如下步驟製造。
首先,於將聚乙烯縮丁醛樹脂或聚(甲基)丙烯酸酯系樹脂等黏合劑樹脂溶解於有機溶劑而成之溶液添加塑化劑、分散劑等後,添加陶瓷原料粉末,藉由珠磨機、球磨機等混合裝置均一地混合,獲得於消泡後具有一定黏度之陶瓷漿料組成物。使用刮刀、逆輥塗佈機等將該漿料組成物流延至經脫模處理之聚對苯二甲酸乙二酯膜、或SUS板等支撐體面,藉由對其加熱等而使溶劑等揮發成分被餾去後,自支撐體剝離而獲得陶瓷生片。
繼而,於所獲得之陶瓷生片上藉由網版印刷塗佈成為內部電極之導電膠,將所獲得者交替地重疊多片後,進行加熱壓接而製作積層體。其後,經由以下步驟獲得積層陶瓷電容器:進行使積層體中所包含之黏合劑樹脂成分等熱分解而去除之處理,即所謂之脫脂處理,於經過燒成所獲得之陶瓷燒結體之端面燒結外部電極。
又,伴隨電子機器之多功能化、小型化,對於積層陶瓷電容器要求大容量化小型化。與此對應,陶瓷生片使用更微細之粒徑(例如為0.5 μm以下)之陶瓷粉末,嘗試於剝離性之支撐體上塗佈成更薄之膜狀(例如為5 μm以下)。
然而,於陶瓷生片製作時之諸步驟中,薄膜狀之陶瓷生片受到拉伸或彎曲等應力。因此,要求具有能夠耐受該等應力之強度之陶瓷生片。
對此,於專利文獻1及2中記載有藉由將聚合度、乙醯基量、縮醛基量設為特定之範圍,可不添加過量之有機溶劑而獲得塗佈性優異之漿料組成物。
先前技術文獻
專利文獻
專利文獻1:日本專利第5462700號公報
專利文獻2:日本專利第5702311號公報
[發明所欲解決之課題]
然而,即便為如專利文獻1及2中記載之漿料組成物,亦存在所獲得之陶瓷生片之強度不充分,於自支撐體剝離時破損之問題。
又,於陶瓷生片製作時之切斷步驟中,存在切斷面變得不均一,產生外觀不良之問題。
進而,於乾燥步驟中,由於尺寸變化,亦引起產生切斷後之尺寸不良之問題。
鑒於上述現狀,本發明之目的在於:提供一種陶瓷生片用樹脂組成物、及使用該陶瓷生片用樹脂組成物之陶瓷生片及積層陶瓷電容器,該陶瓷生片用樹脂組成物能夠製作即便於製成薄層時亦具有較高之機械強度、不易產生切斷後之外觀不良或乾燥後之尺寸變化之陶瓷生片。
[解決課題之技術手段]
本發明係一種陶瓷生片用樹脂組成物,其含有聚乙烯縮醛樹脂,陶瓷生片用樹脂組成物之tanδ之峰頂為1.25以上,且損失彈性模數E''為2.30×108
Pa以上。
以下,對本發明進行詳述。
本發明者努力研究,結果發現:tanδ之峰頂、損失彈性模數E''為特定之範圍內之陶瓷生片用樹脂組成物能夠製作即便於製成薄層時亦具有較高之機械強度、不易產生切斷後之外觀不良或乾燥後之尺寸變化之陶瓷生片,從而完成本發明。
本發明之陶瓷生片用樹脂組成物之tanδ之峰頂為1.25以上。藉此,可賦予適度之柔軟性。上述tanδ之峰頂之較佳之下限為1.55,較佳之上限為3.00。
再者,上述tanδ之峰頂係例如使用DMA(IT計測公司製)於溫度範圍30℃~150℃、升溫速度6℃/分鐘、頻率1 Hz之條件下進行測定之情形時的於峰值溫度之tanδ之測定值。又,上述DMA測定較佳為將陶瓷生片用樹脂組成物成形為片狀後進行測定。
本發明之陶瓷生片用樹脂組成物之損失彈性模數E''為2.30×108
Pa以上。藉由設為上述範圍內,可賦予適度之柔軟性。上述損失彈性模數E''之較佳之下限為2.30×108
Pa,較佳之上限為2.80×108
Pa。
再者,上述損失彈性模數係例如使用DMA(IT計測公司製)於溫度範圍30℃~150℃、升溫速度6℃/分鐘、頻率1 Hz之條件下進行測定之情形時的於峰值溫度之損失彈性模數之測定值。又,上述DMA測定較佳為將陶瓷生片用樹脂組成物成形為片狀後進行測定。
本發明之陶瓷生片用樹脂組成物之tanδ之峰頂溫度與損失彈性模數E''之峰頂溫度之差(峰頂溫度差:[tanδ之峰頂溫度]-[損失彈性模數E''之峰頂溫度])較佳為8.0~15.0℃。藉由設為上述範圍內,可獲得強韌之膜強度。上述峰頂溫度差之更佳之下限為9.0℃,更佳之上限為14.0℃。
本發明之陶瓷生片用樹脂組成物含有聚乙烯縮醛樹脂。
上述聚乙烯縮醛樹脂具有:下述通式(1)所示之具有縮醛基之構成單位、下述通式(2)所示之具有羥基之構成單位、及下述通式(3)所示之具有乙醯基之構成單位。
上述式(1)中,R1
表示氫原子或碳數1~20之烷基。
上述式(1)中,於R1
為碳數1~20之烷基之情形時,作為該烷基,例如可列舉甲基、乙基、正丙基、異丙基、正丁基、異丁基、二級丁基、三級丁基等。又,可列舉戊基、己基、庚基、2-乙基己基、辛基、壬基、癸基、十一基、十二基、十三基、十四基、十五基、十八基等。其中,較佳為甲基、正丙基。
於上述聚乙烯縮醛樹脂中,上述通式(1)所示之具有縮醛基之構成單位之含量(以下,亦稱為「縮醛基量」)的較佳之下限為45莫耳%,較佳之上限為83莫耳%。
若上述縮醛基量為45莫耳%以上,則可提高對有機溶劑之溶解性。若上述縮醛基量為83莫耳%以下,則可製成強韌性優異之聚乙烯縮醛樹脂。
上述縮醛基量之更佳之下限為60莫耳%,進而較佳之下限為62莫耳%,尤佳之下限為65莫耳%,更佳之上限為80莫耳%,進而較佳之上限為78莫耳%。
再者,於本說明書中,作為縮醛基量之計算方法,由於聚乙烯縮醛樹脂之縮醛基係將聚乙烯醇樹脂之具有2個羥基之構成單位縮醛化而獲得者,因此,採用對縮醛化之具有2個羥基之構成單位進行計數之方法來計算縮醛基量。
於上述聚乙烯縮醛樹脂中,上述通式(2)所示之具有羥基之構成單位之含量(以下,亦稱為「羥基量」)的較佳之下限為18莫耳%,較佳之上限為45莫耳%。
若上述羥基量為18莫耳%以上,則可製成強韌性優異之聚乙烯縮醛樹脂。若上述羥基量為45莫耳%以下,則可使對有機溶劑之溶解性充分地提高。
上述羥基量之更佳之下限為20莫耳%,進而較佳之下限為22莫耳%,更佳之上限為40莫耳%,進而較佳之上限為37莫耳%。
於上述聚乙烯縮醛樹脂中,上述通式(3)所示之具有乙醯基之構成單位之含量(以下,亦稱為「乙醯基量」)的較佳之下限為0.5莫耳%,較佳之上限為20莫耳%。
若上述乙醯基量為0.5莫耳%以上,則可抑制因聚乙烯縮醛樹脂中之羥基之分子內及分子間之氫鍵而引起之高黏度化。若上述乙醯基量為20莫耳%以下,則聚乙烯縮醛樹脂之柔軟性不會過度提高,可提高處理性。
上述乙醯基量之更佳之下限為1.0莫耳%,更佳之上限為18莫耳%。
上述聚乙烯縮醛樹脂之平均聚合度較佳為1000~10000。
藉由使上述平均聚合度為1000以上,即便於製作如厚度20 μm以下之薄膜樹脂片之情形時,亦可賦予充分之機械強度。若上述平均聚合度為10000以下,則可使對有機溶劑之溶解性充分提高,可製成塗佈性、分散性優異者。又,藉由設為上述範圍內,可獲得具有較高之機械強度、不易產生切斷後之外觀不良或乾燥後之尺寸變化之陶瓷生片。
上述平均聚合度之更佳之下限為1050,進而較佳之下限為1100,更佳之上限為5000,進而較佳之上限為4900,最佳之上限為4800。
上述聚乙烯縮醛樹脂之藉由NMR測定及IR測定而定量之羥基之莫耳%換算半值寬較佳為0.01~0.15莫耳%/cm-1
。藉由設為上述範圍內,可獲得具有較高之機械強度、不易產生切斷後之外觀不良或乾燥後之尺寸變化之陶瓷生片。又,羥基之莫耳%換算半值寬更佳為0.01~0.145莫耳%/cm-1
。
再者,上述所謂IR測定係藉由紅外吸收光譜法而實施之吸收光譜之測定,例如可藉由IR測定計進行測定。
又,上述羥基之莫耳%換算半值寬能夠藉由以下方法算出:藉由IR測定,根據於3500 cm-1
附近出現之峰高之1/2處之峰寬測定羥基之半值寬,其後藉由NMR測定來測定羥基量,將羥基量除以羥基之半值寬。
上述聚乙烯縮醛樹脂通常能夠藉由將聚乙烯醇樹脂縮醛化而製造。
作為上述縮醛化之方法,並無特別限定,可使用先前公知之方法,例如可列舉在酸觸媒之存在下於聚乙烯醇樹脂之水溶液、醇溶液、水/醇混合溶液、二甲基亞碸(DMSO)溶液中添加各種醛之方法等。
作為上述醛,例如可列舉碳數1~19之直鏈狀、支鏈狀、環狀飽和、環狀不飽和、或芳香族之醛等。具體而言,例如可列舉:甲醛、乙醛、丙醛、正丁醛、異丁醛、三級丁醛、苯甲醛、環己醛等。上述醛可單獨使用,亦可併用2種以上。又,上述醛化合物除甲醛以外,亦可為1個以上之氫原子被鹵素等取代而成者。
作為上述聚乙烯醇樹脂,例如可使用藉由利用鹼、酸、氨水等對聚乙酸乙烯酯進行皂化而製造之樹脂等先前公知之聚乙烯醇樹脂。
上述聚乙烯醇樹脂可完全皂化,但只要於主鏈之至少一處相對於內消旋、外消旋位具有雙聯羥基之單元最低為1個單元,則無需完全皂化,亦可為部分皂化聚乙烯醇系樹脂。又,作為上述聚乙烯醇樹脂,亦可使用乙烯-乙烯醇共聚物樹脂、部分皂化乙烯-乙烯醇共聚物樹脂等可與乙烯醇共聚的單體與乙烯醇之共聚物。
上述聚乙酸乙烯酯系樹脂例如可列舉乙烯-乙酸乙烯酯共聚物等。
構成本發明之陶瓷生片用樹脂組成物之聚乙烯縮醛樹脂較佳為皂化度為75莫耳%以上之聚乙烯醇樹脂之縮醛化物。構成本發明之陶瓷生片用樹脂組成物之聚乙烯縮醛樹脂尤佳為藉由IR測定而定量之羥基之半值寬為300~400 cm-1
之聚乙烯醇樹脂之縮醛化物。尤佳為使用藉由IR測定而定量之羥基之半值寬為340~400 cm-1
之聚乙烯醇樹脂之縮醛化物。藉此,能夠將本發明之陶瓷生片用樹脂組成物之tanδ之峰頂、及損失彈性模數E''設為特定之範圍內。
上述聚乙烯醇樹脂通常含有皂化時產生之鹼性成分即羧酸鹽,因此,較佳為將其洗淨去除或中和後使用。藉由將羧酸鹽洗淨去除或進行中和,可有效地抑制於鹼性條件下受到觸媒作用之醛之縮合反應,因此,可進一步抑制樹脂之著色。
作為上述洗淨步驟中之洗淨方法,例如可列舉:藉由溶劑萃取鹼性成分之方法、或使樹脂溶解於良溶劑後投入不良溶劑僅使樹脂再沉澱之方法、或於含有聚乙烯醇系樹脂之溶液中添加吸附劑而吸附去除鹼性成分之方法等。
作為上述中和步驟中使用之中和劑,例如可列舉:鹽酸、硫酸、硝酸、磷酸等礦酸;或碳酸等無機酸;或甲酸、乙酸、丙酸、丁酸、己酸等羧酸;或甲磺酸、乙磺酸等脂肪族磺酸;或苯磺酸等芳香族磺酸;苯酚等酚類等。
本發明之陶瓷生片用樹脂組成物亦可含有塑化劑。藉由添加塑化劑,可使所獲得之陶瓷生片之機械強度、及柔軟性大幅度提高。
作為上述塑化劑,例如可列舉:鄰苯二甲酸二辛酯(DOP)、鄰苯二甲酸二丁酯(DBP)等鄰苯二甲酸二酯;己二酸二辛酯等己二酸二酯等;三乙二醇二-2-乙基己酸酯、四乙二醇二-2-乙基己酸酯等烷二醇二酯等。又,可列舉三乙二醇二-2-乙基丁酸酯、四乙二醇二-2-乙基丁酸酯、四乙二醇二-庚酸酯、三乙二醇二-庚酸酯等烷二醇二酯等。
於本發明之陶瓷生片用樹脂組成物中,上述塑化劑之含量相對於聚乙烯縮醛樹脂100重量份之較佳之下限為7重量份,更佳之下限為8.5重量份,較佳之上限為25重量份,更佳之上限為15重量份,進而較佳之上限為11.5重量份。
本發明之陶瓷生片用樹脂組成物亦可含有有機溶劑。
作為上述有機溶劑,並無特別限定,例如只要為可溶解上述聚乙烯縮醛樹脂者則無特別限定,例如可列舉:丙酮、甲基乙基酮、二丙基酮、二異丁基酮等酮類。又,可列舉:甲醇、乙醇、異丙醇、丁醇等醇類;甲苯、二甲苯等芳香族烴類等。進而,可列舉:丙酸甲酯、丙酸乙酯、丙酸丁酯、丁酸甲酯、丁酸乙酯、丁酸丁酯、戊酸甲酯、戊酸乙酯、戊酸丁酯、己酸甲酯、己酸乙酯、己酸丁酯、乙酸2-乙基己酯、丁酸2-乙基己酯等酯類等。又,可列舉:甲基賽珞蘇、乙基賽珞蘇、丁基賽珞蘇、萜品醇、二氫萜品醇、乙酸丁基賽珞蘇、丁基卡必醇乙酸酯、萜品醇乙酸酯、二氫萜品醇乙酸酯等。尤其就塗佈性、乾燥性之方面而言,較佳為醇類、酮類、芳香族烴類及該等之混合溶劑。其中,較佳為乙醇與甲苯之混合溶劑或甲基乙基酮與甲苯之混合溶劑。
本發明之陶瓷生片用樹脂組成物於不損害本發明之效果之範圍內,亦可含有上述聚乙烯縮醛樹脂以外之聚乙烯縮醛樹脂、或丙烯酸樹脂、乙基纖維素等其他樹脂。於此情形時,上述聚乙烯縮醛樹脂相對於全部黏合劑樹脂之含量較佳為50重量%以上。
於本發明之陶瓷生片用樹脂組成物中,視需要可適當添加無機粉末、分散劑、抗氧化劑、紫外線吸收劑、界面活性劑、填充劑等,視情況亦可添加少量丙烯酸樹脂或胺酯(urethane)樹脂等其他樹脂。
作為上述無機粉末,可列舉金屬或非金屬之氧化物或者非氧化物之粉末、陶瓷粉末。又,該等粉末之組成可為單一組成,亦可為化合物之狀態,可單獨使用或混合使用。再者,金屬之氧化物或非氧化物之構成元素可與陽離子或陰離子一併由單元素或多種元素構成,亦可進一步含有為了改良氧化物或非氧化物之特性而添加之添加物。具體而言,可列舉Li、K、Mg、B、Al、Si、Cu、Ca、Sr、Ba、Zn、Cd、Ga、In、Y、鑭系元素、錒系元素、Ti、Zr、Hf、Bi、V、Nb、Ta、W、Mn、Fe、Co、Ni等氧化物、碳化物、氮化物、硼化物、硫化物等。
又,若根據結晶結構對通常被稱為複合氧化物之含有多種金屬元素之具體的氧化物粉末進行分類,則作為採用鈣鈦礦型結構者,可列舉NaNbO3
、SrZrO3
、PbZrO3
、SrTiO3
、BaZrO3
、PbTiO3
、BaTiO3
等。作為採用尖晶石型結構者,可列舉MgAl2
O4
、ZnAl2
O4
、CoAl2
O4
、NiAl2
O4
、MgFe2
O4
等。作為採用鈦鐵礦型結構者,可列舉MgTiO3
、MnTiO3
、FeTiO3
等。作為採用石榴石型結構者,可列舉GdGa5
O12
、Y6
Fe5
O12
等。其中,本發明之改質聚乙烯縮醛樹脂相對於與BaTiO3
之粉末混合之陶瓷生片顯示出較高之特性。
上述無機粉末之平均粒徑並無特別限定,例如作為薄層陶瓷生片(厚度5 μm以下)之製作用,較佳為0.05~0.5 μm以下。
於本發明之陶瓷生片用樹脂組成物含有無機粉末之情形時,相對於無機粉末100重量份,上述聚乙烯縮醛樹脂之含量之較佳之下限為0.1重量份,較佳之上限為20重量份。藉由將上述聚乙烯縮醛樹脂之含量設為0.1重量份以上,無機粉末之分散性變得充分,藉由設為20重量份以下,黏度變為適度之範圍,可提高操作性。上述含量之更佳之下限為0.6重量份,進而較佳之上限為15重量份。尤其是藉由將上述含量設為0.6重量份以上,可使聚乙烯縮醛樹脂充分地吸附至無機粉末之表面,因此,可使無機粉末更微細地分散。
於本發明之陶瓷生片用樹脂組成物含有無機粉末之情形時,相對於無機粉末100重量份,上述有機溶劑之含量之較佳之下限為20重量份,較佳之上限為60重量份。藉由將上述有機溶劑之含量設為20重量份以上,能夠使黏度為適度之範圍,不限制無機粉末之移動而獲得充分之分散性,藉由設為60重量份以下,無機粉末濃度不會變得過低,能夠減少無機粉末彼此之碰撞次數而獲得充分之分散性。
作為製造本發明之陶瓷生片用樹脂組成物之方法,並無特別限定,例如可列舉以下方法:使用球磨機、攪拌磨機、三輥研磨機等各種混合機混合上述聚乙烯縮醛樹脂、有機溶劑及視需要添加之各種添加劑無機粉末。再者,上述無機粉末亦可於另外製備無機分散液後添加。
於塗佈本發明之陶瓷生片用樹脂組成物後,進行加熱使其乾燥,藉此獲得樹脂片。
作為塗佈本發明之陶瓷生片用樹脂組成物時之方法,並無特別限定,例如可列舉輥式塗佈機、模嘴塗佈機、簾塗佈機等方法。再者,關於其他具體方法,可使用先前公知之方法。
含有陶瓷粉末之樹脂片能夠用作陶瓷生片。此種陶瓷生片亦為本發明之一。
使用上述陶瓷生片能夠製造陶瓷電子零件。例如可藉由進行以下步驟而製造陶瓷電子零件:於陶瓷生片之表面塗佈電極層用漿料之步驟;將形成有電極層之陶瓷生片積層並進行加熱壓接而獲得積層體,對該積層體進行脫脂、燒成之步驟。
作為上述陶瓷電子零件,並無特別限定,例如可列舉:積層陶瓷電容器、積層陶瓷電感器、電容器、壓電致動器、積層變阻器、積層熱阻器、EMI濾波器、氮化鋁多層基板、氧化鋁多層基板等。此種陶瓷電子零件亦為本發明之一。
於上述陶瓷電子零件之製造方法中,進行於上述陶瓷生片之表面塗佈電極層用漿料之步驟。
作為電極層用漿料,例如可藉由將聚乙烯縮醛樹脂或乙基纖維素、丙烯酸樹脂等作為黏合劑樹脂而溶解於有機溶劑,使導電粉末等分散而獲得。該等樹脂可單獨使用,亦可混合2種以上使用。含有聚乙烯縮醛樹脂之電極層用漿料於加熱壓接步驟中對陶瓷生片顯示出優異之接著性,故而較佳。
於上述陶瓷電子零件之製造方法中,於製作上述形成有電極層之陶瓷生片後,將以相同之方式製作之形成有電極層之陶瓷生片積層並進行加熱壓接而獲得積層體,對該積層體進行脫脂、燒成,藉此可獲得片侵蝕(sheet attack)或龜裂等問題得以解決之積層陶瓷電子零件。
再者,關於上述加熱壓接步驟、對積層體進行脫脂、燒成之步驟並無特別限定,可使用先前公知之方法。
[發明之效果]
根據本發明,能夠提供一種陶瓷生片用樹脂組成物、及使用該陶瓷生片用樹脂組成物之陶瓷生片及積層陶瓷電容器,該陶瓷生片用樹脂組成物能夠製作即便於製成薄層時亦具有較高之機械強度、不易產生切斷後之外觀不良或乾燥後之尺寸變化之陶瓷生片。
以下,列舉實施例更詳細地說明本發明,但本發明並不僅限定於該等實施例。
(實施例1)
(聚乙烯縮醛樹脂之製作)
於平均聚合度1000、皂化度98.5莫耳%、羥基半值寬350 cm-1
之聚乙烯醇樹脂250 g添加純水2700 g,於90℃攪拌約2小時使其溶解。將該溶液冷卻至40℃,於其中添加濃度35重量%之鹽酸100 g與正丁醛115 g,進行縮醛化反應,使反應產物析出。其後,於40℃使縮醛化反應完成,藉由常規方法進行中和、水洗及乾燥,獲得聚乙烯縮醛樹脂之白色粉末。
將所獲得之聚乙烯縮醛樹脂以10重量%之濃度溶解於DMSO-d6
,使用13
C-NMR,測定縮醛基量、羥基量、乙醯基量。再者,聚乙烯醇樹脂之羥基之半值寬使用HORIBA FT-720(堀場製作所公司製)測定。
(陶瓷生片用樹脂組成物之製作)
將所獲得之聚乙烯縮醛樹脂10.0重量份、及作為塑化劑之DOP 1.0重量份添加至乙醇/甲苯混合溶劑(重量比1:1)45.0重量份,進行攪拌溶解,獲得陶瓷生片用樹脂組成物。
(樹脂片之製作)
使用塗佈機,以乾燥後之厚度成為15 μm之方式將所獲得之陶瓷生片用樹脂組成物塗佈於經脫模處理之PET膜上後,於70℃加熱120分鐘使其乾燥,藉此製作樹脂片。
(實施例2)
(聚乙烯縮醛樹脂之製作)
除使用聚合度1700、皂化度98.5莫耳%、羥基半值寬350 cm-1
之聚乙烯醇樹脂250 g以外,以與實施例1相同之方式製作聚乙烯縮醛樹脂、陶瓷生片用樹脂組成物、樹脂片。
(實施例3)
(聚乙烯縮醛樹脂之製作)
除使用聚合度3300、皂化度98.5莫耳%、羥基半值寬350 cm-1
之聚乙烯醇樹脂250 g以外,以與實施例1相同之方式製作聚乙烯縮醛樹脂、陶瓷生片用樹脂組成物、樹脂片。
(實施例4)
(聚乙烯縮醛樹脂之製作)
除使用聚合度4900、皂化度98.5莫耳%、羥基半值寬350 cm-1
之聚乙烯醇樹脂250 g以外,以與實施例1相同之方式製作聚乙烯縮醛樹脂、陶瓷生片用樹脂組成物、樹脂片。
(實施例5)
(聚乙烯縮醛樹脂之製作)
除使用聚合度1700、皂化度98.5莫耳%、羥基半值寬350 cm-1
之聚乙烯醇樹脂250 g以外,以與實施例1相同之方式製作聚乙烯縮醛樹脂、陶瓷生片用樹脂組成物、樹脂片。
(實施例6)
(聚乙烯縮醛樹脂之製作)
除使用聚合度1700、皂化度98.5莫耳%、羥基半值寬350 cm-1
之聚乙烯醇樹脂250 g以外,以與實施例1相同之方式製作聚乙烯縮醛樹脂、陶瓷生片用樹脂組成物、樹脂片。
(實施例7)
(聚乙烯縮醛樹脂之製作)
除使用聚合度1700、皂化度98.5莫耳%、羥基半值寬350 cm-1
之聚乙烯醇樹脂250 g以外,以與實施例1相同之方式製作聚乙烯縮醛樹脂、陶瓷生片用樹脂組成物、樹脂片。
(實施例8)
(聚乙烯縮醛樹脂之製作)
除使用聚合度5000、皂化度98.5莫耳%、羥基半值寬350 cm-1
之聚乙烯醇樹脂250 g以外,以與實施例1相同之方式製作聚乙烯縮醛樹脂、陶瓷生片用樹脂組成物、樹脂片。
(實施例9)
(聚乙烯縮醛樹脂之製作)
除使用聚合度9200、皂化度98.5莫耳%、羥基半值寬350 cm-1
之聚乙烯醇樹脂250 g以外,以與實施例1相同之方式製作聚乙烯縮醛樹脂、陶瓷生片用樹脂組成物、樹脂片。
(實施例10)
(聚乙烯縮醛樹脂之製作)
除使用聚合度8000、皂化度98.5莫耳%、羥基半值寬350 cm-1
之聚乙烯醇樹脂250 g以外,以與實施例1相同之方式製作聚乙烯縮醛樹脂、陶瓷生片用樹脂組成物、樹脂片。
(實施例11)
(聚乙烯縮醛樹脂之製作)
除使用聚合度1700、皂化度98.5莫耳%、羥基半值寬350 cm-1
之聚乙烯醇樹脂250 g以外,以與實施例1相同之方式製作聚乙烯縮醛樹脂、陶瓷生片用樹脂組成物、樹脂片。
(比較例1)
除使用聚合度600、皂化度98.5莫耳%、羥基半值寬335 cm-1
之聚乙烯醇樹脂250 g以外,以與實施例1相同之方式製作聚乙烯縮醛樹脂、陶瓷生片用樹脂組成物、樹脂片。
(比較例2)
除使用聚合度4900、皂化度98.5莫耳%、羥基半值寬335 cm-1
之聚乙烯醇樹脂250 g以外,以與實施例1相同之方式製作聚乙烯縮醛樹脂、陶瓷生片用樹脂組成物、樹脂片。
(比較例3)
除使用聚合度1700、皂化度98.5莫耳%、羥基半值寬335 cm-1
之聚乙烯醇樹脂250 g以外,以與實施例1相同之方式製作聚乙烯縮醛樹脂、陶瓷生片用樹脂組成物、樹脂片。
(比較例4)
除使用聚合度3300、皂化度98.5莫耳%、羥基半值寬335 cm-1
之聚乙烯醇樹脂250 g以外,以與實施例1相同之方式製作聚乙烯縮醛樹脂、陶瓷生片用樹脂組成物、樹脂片。
(比較例5)
除使用聚合度4900、皂化度98.5莫耳%、羥基半值寬335 cm-1
之聚乙烯醇樹脂250 g以外,以與實施例1相同之方式製作聚乙烯縮醛樹脂、陶瓷生片用樹脂組成物、樹脂片。
(比較例6)
除使用聚合度9000、皂化度98.5莫耳%、羥基半值寬335 cm-1
之聚乙烯醇樹脂250 g以外,以與實施例1相同之方式製作聚乙烯縮醛樹脂、陶瓷生片用樹脂組成物、樹脂片。
(比較例7)
除使用聚合度9000、皂化度98.5莫耳%、羥基半值寬335 cm-1
之聚乙烯醇樹脂250 g以外,以與實施例1相同之方式製作聚乙烯縮醛樹脂、陶瓷生片用樹脂組成物、樹脂片。
(評價)
對於實施例及比較例中所獲得之聚乙烯縮醛樹脂、陶瓷生片用樹脂組成物及樹脂片,進行了以下評價。將結果示於表1。
(1)莫耳%換算半值寬之確認
關於實施例及比較例中所獲得之聚乙烯縮醛樹脂,使用HORIBA FT-720(堀場製作所公司製)藉由IR測定而測定羥基之半值寬。由藉由IR測定所測得之羥基之半值寬、及藉由13
C-NMR所測得之羥基量,針對聚乙烯縮醛樹脂求出羥基之莫耳%換算半值寬。
(2)tanδ及損失彈性模數E''
將所獲得之樹脂片切為0.5 cm×2.0 cm而製作試片後,使用DMA(IT計測公司製),於下述條件下測定動態黏彈性。
再者,tanδ(損耗正切)係使用於峰頂溫度之數值。又,對於儲存模數E'及損失彈性模數E''亦同樣地測定於峰頂溫度之數值。又,算出tanδ之峰頂溫度與損失彈性模數E''之峰頂溫度之差(峰頂溫度差:[tanδ之峰頂溫度]-[損失彈性模數E''之峰頂溫度])。
(測定條件)
測定模式:拉伸模式
強制振動頻率:1 Hz
溫度範圍:30℃~150℃
升溫速度:6℃/分鐘
(3)拉伸彈性模數、斷裂伸長率及斷裂應力
(陶瓷生片之製作)
將聚乙烯縮醛樹脂(積水化學工業公司製,BL-1)1重量份添加至甲苯20重量份與乙醇20重量份之混合溶劑並攪拌溶解。繼而,將100重量份之鈦酸鋇之粉末(堺化學工業公司製,BT01,平均粒徑0.1 μm)添加至所獲得之溶液,利用珠磨機(AIMEX公司製,Ready Mill)攪拌180分鐘,藉此製作無機分散液。
於所獲得之無機分散液添加陶瓷生片用樹脂組成物,使用珠磨機攪拌90分鐘後,使用塗佈機以乾燥後之厚度成為20 μm之方式塗佈於經脫模處理之PET膜上。其後,於40℃加熱30分鐘使其乾燥,將PET膜剝離,藉此製作陶瓷生片。
對於所獲得之陶瓷生片,依據JIS K 7113,使用拉力試驗機(島津製作所公司製,AUTOGRAPH AGS-J),於拉伸速度20 mm/分鐘之條件下進行拉伸彈性模數(MPa)、斷裂伸長率(%)及斷裂應力(MPa)之測定。
(4)切斷截面狀態
利用SEM觀察「(3)拉伸彈性模數、斷裂伸長率及斷裂應力」測定後之斷裂面,按照下述評價標準進行判定。
◎:斷裂面無缺口、裂痕、損傷
○:斷裂面無缺口、裂痕,但有損傷
△:斷裂面無缺口,但有裂痕
×:斷裂面有缺口
(5)尺寸變化率
以與「(3)拉伸彈性模數、斷裂伸長率及斷裂應力」相同之方法製作陶瓷生片。使所獲得之陶瓷生片於70℃乾燥3小時,算出70℃乾燥前後之尺寸變化率,根據以下標準進行評價。
◎:2%以下
○:超過2%且3%以下
△:超過3%且4%以下
×:超過4%
[表1]
[產業上之可利用性]
聚乙烯縮醛樹脂 | 評價 | |||||||||||||||
平均 聚合度 | 縮醛基量 (莫耳%) | 乙醯基量 (莫耳%) | 羥基量 (莫耳%) | 羥基 莫耳%換算 半值寬 (莫耳%/cm-1 ) | 聚乙烯縮醛樹脂 膜評價 | GS評價 | ||||||||||
tanδ | E'' [Pa] | tanδ-E'' 峰值溫度差 | 斷裂 應力[MPa] | 彈性 模數[MPa] | 斷裂伸長率[%] | 斷裂 應力[MPa] | 彈性 模數[MPa] | 斷裂伸長率 [%] | 切斷截面狀態 SEM觀察 | 尺寸 變化率 | ||||||
實施例1 | 1000 | 65.0 | 1.5 | 33.5 | 0.142 | 1.55 | 2.30×108 | 14.8 | 60 | 950 | 280 | 27 | 910 | 15 | ○ | ◎ |
實施例2 | 1700 | 65.0 | 1.5 | 33.5 | 0.137 | 1.97 | 2.33×108 | 13.1 | 75 | 900 | 410 | 32 | 1050 | 23 | ◎ | ◎ |
實施例3 | 3300 | 65.0 | 1.5 | 33.5 | 0.140 | 2.33 | 2.36×108 | 13.0 | 85 | 900 | 370 | 34 | 1080 | 23 | ○ | ○ |
實施例4 | 4900 | 65.0 | 1.5 | 33.5 | 0.138 | 2.39 | 2.38×108 | 12.6 | 85 | 955 | 280 | 38 | 1100 | 25 | ○ | ○ |
實施例5 | 1700 | 65.0 | 1.0 | 34.0 | 0.100 | 2.01 | 2.35×108 | 12.8 | 77 | 940 | 400 | 33 | 1080 | 24 | ◎ | ◎ |
實施例6 | 1700 | 65.0 | 2.2 | 32.8 | 0.148 | 1.88 | 2.30×108 | 13.5 | 74 | 890 | 420 | 31 | 1050 | 22 | ◎ | ○ |
實施例7 | 1700 | 78.0 | 1.5 | 21.5 | 0.140 | 1.80 | 2.30×108 | 14.0 | 70 | 880 | 435 | 33 | 1000 | 25 | ◎ | ○ |
實施例8 | 5000 | 65.0 | 1.5 | 33.5 | 0.145 | 2.40 | 2.32×108 | 12.2 | 88 | 910 | 410 | 38 | 1190 | 28 | ○ | ○ |
實施例9 | 9200 | 65.0 | 1.5 | 33.5 | 0.140 | 2.36 | 2.31×108 | 10.0 | 92 | 890 | 440 | 41 | 1190 | 30 | ○ | △ |
實施例10 | 8000 | 65.0 | 1.5 | 33.5 | 0.144 | 2.39 | 2.38×108 | 11.0 | 90 | 900 | 425 | 40 | 1200 | 30 | ○ | ○ |
實施例11 | 1700 | 50.5 | 1.5 | 48.0 | 0.148 | 1.30 | 2.36×108 | 14.7 | 77 | 1010 | 190 | 30 | 1000 | 17 | △ | ◎ |
比較例1 | 600 | 65.0 | 1.5 | 33.5 | 0.152 | 1.00 | 2.29×108 | 16.2 | 35 | 410 | 250 | 19 | 880 | 13 | × | ○ |
比較例2 | 4900 | 65.0 | 1.5 | 33.5 | 0.137 | 2.40 | 2.28×108 | 14.5 | 56 | 800 | 245 | 29 | 995 | 26 | △ | △ |
比較例3 | 1700 | 65.0 | 1.5 | 33.5 | 0.153 | 2.28 | 2.19×108 | 15.2 | 70 | 720 | 300 | 25 | 900 | 15 | △ | △ |
比較例4 | 3300 | 65.0 | 1.5 | 33.5 | 0.165 | 1.23 | 2.22×108 | 15.0 | 75 | 750 | 330 | 26 | 1000 | 23 | △ | △ |
比較例5 | 4900 | 65.0 | 1.5 | 33.5 | 0.159 | 1.22 | 2.21×108 | 14.9 | 78 | 780 | 350 | 28 | 900 | 25 | △ | × |
比較例6 | 9000 | 76.5 | 1.5 | 22.0 | 0.165 | 1.20 | 2.28×108 | 14.3 | 80 | 820 | 375 | 30 | 900 | 23 | △ | × |
比較例7 | 9000 | 58.0 | 1.5 | 40.5 | 0.170 | 1.21 | 2.22×108 | 14.1 | 77 | 800 | 310 | 31 | 1000 | 20 | △ | × |
根據本發明,能夠提供一種陶瓷生片用樹脂組成物、及使用該陶瓷生片用樹脂組成物之陶瓷生片及積層陶瓷電容器,該陶瓷生片用樹脂組成物能夠製作即便於製成薄層時亦具有較高之機械強度、不易產生切斷後之外觀不良或乾燥後之尺寸變化之陶瓷生片。
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Claims (8)
- 一種陶瓷生片用樹脂組成物,其含有聚乙烯縮醛樹脂, 陶瓷生片用樹脂組成物之tanδ之峰頂為1.25以上,且 損失彈性模數E''為2.30×108 Pa以上。
- 如請求項1之陶瓷生片用樹脂組成物,其中,聚乙烯縮醛樹脂之藉由NMR測定及IR測定而定量之羥基之莫耳%換算半值寬為0.01~0.15莫耳%/cm-1 。
- 如請求項1或2之陶瓷生片用樹脂組成物,其中,相對於聚乙烯縮醛樹脂100重量份,塑化劑之含量為25重量份以下。
- 2或3之陶瓷生片用樹脂組成物,其中,聚乙烯縮醛樹脂係皂化度為75莫耳%以上之聚乙烯醇系樹脂之縮醛化物。
- 2、3或4之陶瓷生片用樹脂組成物,其中,聚乙烯縮醛樹脂之縮醛基量為45~83莫耳%。
- 2、3、4或5之陶瓷生片用樹脂組成物,其中,聚乙烯縮醛樹脂之平均聚合度為1000~10000。
- 一種陶瓷生片,其係使用請求項1、2、3、4、5或6之陶瓷生片用樹脂組成物而成。
- 一種積層陶瓷電容器,其具有請求項7之陶瓷生片。
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EP (1) | EP3950829A4 (zh) |
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CN (1) | CN113646380A (zh) |
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JPS55141192A (en) | 1979-04-21 | 1980-11-04 | Miyarisan Kk | Continuous cultivation of spore forming fungi |
JPS581766A (ja) * | 1981-06-25 | 1983-01-07 | Sekisui Chem Co Ltd | 接着剤組成物 |
JP3831748B2 (ja) * | 2003-01-29 | 2006-10-11 | Tdk株式会社 | グリーンシート用塗料、グリーンシート、グリーンシート用塗料の製造方法、グリーンシートの製造方法および電子部品の製造方法 |
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JP4603623B2 (ja) * | 2008-11-13 | 2010-12-22 | 積水化学工業株式会社 | ポリビニルアセタール樹脂組成物 |
CN102822117A (zh) * | 2010-01-26 | 2012-12-12 | 可乐丽股份有限公司 | 陶瓷生片用浆料组合物、陶瓷生片以及层叠陶瓷电容器 |
JP5462700B2 (ja) * | 2010-05-10 | 2014-04-02 | 株式会社クラレ | セラミックグリーンシート用ポリビニルアセタール樹脂、スラリー組成物、セラミックグリーンシート及び積層セラミックコンデンサ |
CN105175590B (zh) * | 2010-08-19 | 2017-10-03 | 株式会社可乐丽 | 聚乙烯醇缩醛树脂 |
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