JP2012256851A - 強誘電体薄膜の製造方法 - Google Patents
強誘電体薄膜の製造方法 Download PDFInfo
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- JP2012256851A JP2012256851A JP2012073404A JP2012073404A JP2012256851A JP 2012256851 A JP2012256851 A JP 2012256851A JP 2012073404 A JP2012073404 A JP 2012073404A JP 2012073404 A JP2012073404 A JP 2012073404A JP 2012256851 A JP2012256851 A JP 2012256851A
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- thin film
- ferroelectric thin
- control layer
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- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 1
- 229940005605 valeric acid Drugs 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Abstract
【解決手段】結晶面が(111)軸方向に配向した下部電極を有する基板の下部電極上に、強誘電体薄膜形成用組成物を塗布し、加熱して結晶化させることにより下部電極上に強誘電体薄膜を製造する方法の改良であり、強誘電体薄膜が(110)面に優先的に結晶配向が制御された配向制御層により構成され、配向制御層を結晶化後の層厚を5nm〜30nmの範囲内にすることにより形成することを特徴とする。
【選択図】図1
Description
先ず、反応容器にチタニウムテトライソプロポキシドと安定化剤としてアセチルアセトンを添加し、窒素雰囲気下、150℃の温度で還流した。次いで、これに酢酸鉛3水和物と溶媒としてプロピレングリコールを添加し、窒素雰囲気下、150℃の温度で還流した。その後、150℃で減圧蒸留して副生成物を除去し、更に、希釈アルコールを添加することで、以下の表1に示す各濃度に調整された、酸化物換算で各金属比がPb/Ti=125/100の金属化合物を含有する結晶粒径制御層用組成物を得た。
基板として表面にスパッタリング法にてPt下部電極膜を形成した6インチシリコン基板を用意した。この基板のPt下部電極膜上に、スピンコート法により、500rpmで3秒間、その後2000rpmで20秒間の条件で、上記調製した5質量%濃度の配向制御層用組成物を塗布した。続いて、ホットプレートを用い、大気雰囲気中、180℃で5分間加熱して乾燥・仮焼成を行った後、昇温速度10℃/秒で酸素雰囲気中700℃、1分間加熱する本焼成を行って結晶化させ、層厚20nmの配向制御層を得た。これを実施例1の強誘電体薄膜とした。
実施例1と同様の基板を用意し、この基板のPt下部電極膜上に、スピンコート法により、500rpmで3秒間、その後2000rpmで20秒間の条件で、上記調製した5質量%濃度の配向制御層用組成物を塗布した。続いて、ホットプレートを用い、大気雰囲気中、200℃で5分間加熱して乾燥・仮焼成を行った後、昇温速度10℃/秒で酸素雰囲気中700℃、1分間加熱する本焼成を行って結晶化させ、層厚20nmの配向制御層を得た。次に、配向制御層上に、スピンコート法により、500rpmで3秒間、その後2000rpmで20秒間の条件で、上記調製した12質量%濃度の膜厚調整層用組成物を塗布した。続いて、ホットプレートを用い、大気雰囲気中、300℃で5分間加熱して乾燥・仮焼成を行った。この膜厚調整層用組成物の塗布、仮焼成の工程を4回繰り返した後、昇温速度10℃/秒で酸素雰囲気中700℃、1分間加熱する本焼成を行って結晶化させ、層厚300nmの膜厚調整層を得た。これを実施例2の強誘電体薄膜とした。
実施例1と同様の基板を用意し、この基板のPt下部電極膜上に、スピンコート法により、500rpmで3秒間、その後2000rpmで20秒間の条件で、上記調製した5質量%濃度の配向制御層用組成物を塗布した。続いて、ホットプレートを用い、大気雰囲気中、250℃で5分間加熱して乾燥・仮焼成を行った後、昇温速度10℃/秒で酸素雰囲気中700℃、1分間加熱する本焼成を行って結晶化させ、層厚20nmの配向制御層を得た。次に、配向制御層上に、スピンコート法により、500rpmで3秒間、その後2000rpmで20秒間の条件で、上記調製した12質量%濃度の膜厚調整層用組成物を塗布した。続いて、ホットプレートを用い、大気雰囲気中、300℃で5分間加熱して乾燥・仮焼成を行った。この膜厚調整層用組成物の塗布、仮焼成の工程を4回繰り返した後、昇温速度10℃/秒で酸素雰囲気中700℃、1分間加熱する本焼成を行って結晶化させ、層厚300nmの膜厚調整層を得た。これを実施例3の強誘電体薄膜とした。
実施例1と同様の基板を用意し、この基板のPt下部電極膜上に、スピンコート法により、500rpmで3秒間、その後2000rpmで20秒間の条件で、上記調製した5質量%濃度の配向制御層用組成物を塗布した。続いて、ホットプレートを用い、大気雰囲気中、300℃で5分間加熱して乾燥・仮焼成を行った後、昇温速度10℃/秒で酸素雰囲気中700℃、1分間加熱する本焼成を行って結晶化させ、層厚20nmの配向制御層を得た。次に、配向制御層上に、スピンコート法により、500rpmで3秒間、その後2000rpmで20秒間の条件で、上記調製した12質量%濃度の膜厚調整層用組成物を塗布した。続いて、ホットプレートを用い、大気雰囲気中、300℃で5分間加熱して乾燥・仮焼成を行った。この膜厚調整層用組成物の塗布、仮焼成の工程を4回繰り返した後、昇温速度10℃/秒で酸素雰囲気中700℃、1分間加熱する本焼成を行って結晶化させ、層厚300nmの膜厚調整層を得た。これを実施例4の強誘電体薄膜とした。
実施例1と同様の基板を用意し、この基板のPt下部電極膜上に、スピンコート法により、500rpmで3秒間、その後2000rpmで20秒間の条件で、上記調製した2質量%濃度の配向制御層用組成物を塗布した。続いて、ホットプレートを用い、大気雰囲気中、200℃で5分間加熱して乾燥・仮焼成を行った後、昇温速度10℃/秒で酸素雰囲気中700℃、1分間加熱する本焼成を行って結晶化させ、層厚5nmの配向制御層を得た。次に、配向制御層上に、スピンコート法により、500rpmで3秒間、その後2000rpmで20秒間の条件で、上記調製した12質量%濃度の膜厚調整層用組成物を塗布した。続いて、ホットプレートを用い、大気雰囲気中、350℃で5分間加熱して乾燥・仮焼成を行った。この膜厚調整層用組成物の塗布、仮焼成の工程を4回繰り返した後、昇温速度10℃/秒で酸素雰囲気中700℃、1分間加熱する本焼成を行って結晶化させ、層厚300nmの膜厚調整層を得た。これを実施例5の強誘電体薄膜とした。
実施例1と同様の基板を用意し、この基板のPt下部電極膜上に、スピンコート法により、500rpmで3秒間、その後2000rpmで20秒間の条件で、上記調製した7質量%濃度の配向制御層用組成物を塗布した。続いて、ホットプレートを用い、大気雰囲気中、200℃で5分間加熱して乾燥・仮焼成を行った後、昇温速度10℃/秒で酸素雰囲気中700℃、1分間加熱する本焼成を行って結晶化させ、層厚30nmの配向制御層を得た。次に、配向制御層上に、スピンコート法により、500rpmで3秒間、その後2000rpmで20秒間の条件で、上記調製した12質量%濃度の膜厚調整層用組成物を塗布した。続いて、ホットプレートを用い、大気雰囲気中、450℃で5分間加熱して乾燥・仮焼成を行った。この膜厚調整層用組成物の塗布、仮焼成の工程を4回繰り返した後、昇温速度10℃/秒で酸素雰囲気中700℃、1分間加熱する本焼成を行って結晶化させ、層厚300nmの膜厚調整層を得た。これを実施例6の強誘電体薄膜とした。
実施例1と同様の基板を用意し、この基板のPt下部電極膜上に、スピンコート法により、500rpmで3秒間、その後2000rpmで20秒間の条件で、上記調製した1質量%濃度の結晶粒径制御層用組成物を塗布した。続いて、ホットプレートを用い、大気雰囲気中、200℃で5分間加熱して乾燥・仮焼成を行い、層厚2nmの結晶粒径制御層を得た。次いで、結晶粒径制御層上に、スピンコート法により、500rpmで3秒間、その後2000rpmで20秒間の条件で、上記調製した5質量%濃度の配向制御層用組成物を塗布した。続いて、ホットプレートを用い、大気雰囲気中、200℃で5分間加熱して乾燥・仮焼成を行った後、昇温速度10℃/秒で酸素雰囲気中700℃、1分間加熱する本焼成を行って結晶化させ、層厚20nmの配向制御層を得た。次に、配向制御層上に、スピンコート法により、500rpmで3秒間、その後2000rpmで20秒間の条件で、上記調製した12質量%濃度の膜厚調整層用組成物を塗布した。続いて、ホットプレートを用い、大気雰囲気中、300℃で5分間加熱して乾燥・仮焼成を行った。この膜厚調整層用組成物の塗布、仮焼成の工程を4回繰り返した後、昇温速度10℃/秒で酸素雰囲気中700℃、1分間加熱する本焼成を行って結晶化させ、層厚300nmの膜厚調整層を得た。これを実施例7の強誘電体薄膜とした。
実施例1と同様の基板を用意し、この基板のPt下部電極膜上に、スピンコート法により、500rpmで3秒間、その後2000rpmで20秒間の条件で、上記調製した2質量%濃度の結晶粒径制御層用組成物を塗布した。続いて、ホットプレートを用い、大気雰囲気中、200℃で5分間加熱して乾燥・仮焼成を行い、層厚5nmの結晶粒径制御層を得た。次いで、結晶粒径制御層上に、スピンコート法により、500rpmで3秒間、その後2000rpmで20秒間の条件で、上記調製した7質量%濃度の配向制御層用組成物を塗布した。続いて、ホットプレートを用い、大気雰囲気中、200℃で5分間加熱して乾燥・仮焼成を行い、層厚30nmの配向制御層を得た。次に、配向制御層上に、スピンコート法により、500rpmで3秒間、その後2000rpmで20秒間の条件で、上記調製した12質量%濃度の膜厚調整層用組成物を塗布した。続いて、ホットプレートを用い、大気雰囲気中、300℃で5分間加熱して乾燥・仮焼成を行った。この膜厚調整層用組成物の塗布、仮焼成の工程を4回繰り返した後、昇温速度10℃/秒で酸素雰囲気中700℃、1分間加熱する本焼成を行って結晶化させ、層厚300nmの膜厚調整層を得た。これを実施例8の強誘電体薄膜とした。
実施例1と同様の基板を用意し、この基板のPt下部電極膜上に、スピンコート法により、500rpmで3秒間、その後2000rpmで20秒間の条件で、上記調製した10質量%濃度の配向制御層用組成物を塗布した。続いて、ホットプレートを用い、大気雰囲気中、200℃で5分間加熱して乾燥・仮焼成を行った後、昇温速度10℃/秒で酸素雰囲気中700℃、1分間加熱する本焼成を行って結晶化させ、層厚35nmの配向制御層を得た。次に、配向制御層上に、スピンコート法により、500rpmで3秒間、その後2000rpmで20秒間の条件で、上記調製した12質量%濃度の膜厚調整層用組成物を塗布した。続いて、ホットプレートを用い、大気雰囲気中、300℃で5分間加熱して乾燥・仮焼成を行った。この膜厚調整層用組成物の塗布、仮焼成の工程を4回繰り返した後、昇温速度10℃/秒で酸素雰囲気中700℃、1分間加熱する本焼成を行って結晶化させ、層厚300nmの膜厚調整層を得た。これを比較例1の強誘電体薄膜とした。
実施例1と同様の基板を用意し、この基板のPt下部電極膜上に、スピンコート法により、500rpmで3秒間、その後2000rpmで20秒間の条件で、上記調製した12質量%濃度の配向制御層用組成物を塗布した。続いて、ホットプレートを用い、大気雰囲気中、200℃で5分間加熱して乾燥・仮焼成を行った後、昇温速度10℃/秒で酸素雰囲気中700℃、1分間加熱する本焼成を行って結晶化させ、層厚75nmの配向制御層を得た。次に、配向制御層上に、スピンコート法により、500rpmで3秒間、その後2000rpmで20秒間の条件で、上記調製した12質量%濃度の膜厚調整層用組成物を塗布した。続いて、ホットプレートを用い、大気雰囲気中、300℃で5分間加熱して乾燥・仮焼成を行った。この膜厚調整層用組成物の塗布、仮焼成の工程を4回繰り返した後、昇温速度10℃/秒で酸素雰囲気中700℃、1分間加熱する本焼成を行って結晶化させ、層厚300nmの膜厚調整層を得た。これを比較例2の強誘電体薄膜とした。
実施例1と同様の基板を用意し、この基板のPt下部電極膜上に、スピンコート法により、500rpmで3秒間、その後3000rpmで20秒間の条件で、上記調製した10質量%濃度の配向制御層用組成物を塗布した。続いて、ホットプレートを用い、大気雰囲気中、200℃で5分間加熱して乾燥・仮焼成を行った。この配向制御層用組成物の塗布、仮焼成の工程を6回繰り返した後、昇温速度10℃/秒で酸素雰囲気中700℃、1分間加熱する本焼成を行って結晶化させ、層厚270nmの配向制御層を得た。これを比較例3の強誘電体薄膜とした。
実施例1〜8及び比較例1〜3で得られた強誘電体薄膜について、以下の手法により、各層の層厚、優先配向面、配向度、平均粒子径を求めた。その結果を次に表2にそれぞれ示す。また、実施例1、2、4、5、7のXRDパターンを図3に、比較例1〜3のXRDパターンを図4に、実施例2の表面SEM像(倍率10000倍)を図5に、実施例7の表面SEM像(倍率50000倍)を図6にそれぞれ示す。
(1) 層厚測定:各層の層厚は、強誘電体薄膜を分光エリプソメーター(J.A.Woollam社製:M−2000)により測定して、「結晶粒径制御層と配向制御層の合算の層厚」、「配向制御層の層厚」及び「膜厚調整層の層厚」をそれぞれ求めた。また「結晶粒径制御層の層厚」は、「結晶粒径制御層と配向制御層の合算の層厚」から「配向制御層の層厚」を減することにより算出した。
(2) 優先配向面:誘電体結晶の優先配向面は、強誘電体薄膜をX線回折装置(XRD;Bruker社製:MXP18HF)により測定し、得られた回折結果のうち、最も強度の高い配向面を優先配向面とした。
(3) 配向度:誘電体結晶の(110)面における配向度は、上記(2)で得られた回折結果から、(110)面の強度/((100)面の強度+(110)面の強度+(111)面の強度)を計算することにより算出した。
(4) 平均粒子径:誘電体結晶の平均粒子径は、強誘電体薄膜表面を走査型電子顕微鏡(SEM;HITACHI社製:S−900)により撮影し、電子顕微鏡写真(表面像)に写っている、任意の結晶粒子30個に対して、結晶粒子の粒径(最長径と最短径)をノギスを用いて測定し、これらの測定結果から平均粒子径を算出した。
11 下部電極
12 結晶粒径制御層
13 配向制御層(下地層)
14 膜厚調整層
Claims (9)
- 結晶面が(111)軸方向に配向した下部電極を有する基板の前記下部電極上に、強誘電体薄膜形成用組成物を塗布し、仮焼した後、焼成して結晶化させることにより前記下部電極上に強誘電体薄膜を製造する方法において、
前記強誘電体薄膜形成用組成物を前記下部電極上に塗布、仮焼、焼成して配向制御層を形成し、
前記強誘電体薄膜形成用組成物の塗布量を前記配向制御層の結晶化後の層厚が5nm〜30nmの範囲内になるように設定して前記配向制御層の優先的な結晶配向を(110)面にすることを特徴とする強誘電体薄膜の製造方法。 - 前記配向制御層を形成するための仮焼温度が180℃〜300℃の範囲内にある請求項1記載の強誘電体薄膜の製造方法。
- 前記配向制御層を形成する前に、前記下部電極上に結晶粒径制御層を形成し、前記結晶粒径制御層の上に前記配向制御層を形成する請求項1記載の強誘電体薄膜の製造方法。
- 前記強誘電体薄膜形成用組成物の一部を前記下部電極上に塗布、仮焼、焼成して配向制御層を形成した後に、前記強誘電体薄膜形成用組成物の残部を前記配向制御層上に塗布、仮焼、焼成して前記配向制御層の結晶配向と同じ結晶配向を有する膜厚調整層を形成する請求項1ないし3いずれか1項に記載の強誘電体薄膜の製造方法。
- 前記強誘電体薄膜形成用組成物の残部を塗布した後の前記膜厚調整層を形成するための仮焼温度が300℃〜450℃の範囲内にある請求項1記載の強誘電体薄膜の製造方法。
- 前記強誘電体薄膜がPb含有ペロブスカイト型酸化物であり、前記強誘電体薄膜形成用組成物がβ−ジケトン類及び多価アルコール類を含んでいる請求項1記載の強誘電体薄膜の製造方法。
- 前記β−ジケトン類がアセチルアセトンであり、前記多価アルコール類がプロピレングリコールである請求項4記載の強誘電体薄膜の製造方法。
- 請求項1ないし7いずれか1項に記載の方法により製造された(110)面に優先的に結晶配向した強誘電体薄膜。
- 請求項8記載の強誘電体薄膜を有する薄膜コンデンサ、キャパシタ、IPD、DRAMメモリ用コンデンサ、積層コンデンサ、トランジスタのゲート絶縁体、不揮発性メモリ、焦電型赤外線検出素子、圧電素子、電気光学素子、アクチュエータ、共振子、超音波モータ、又はLCノイズフィルタ素子の複合電子部品。
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US (2) | US8951603B2 (ja) |
EP (1) | EP2525393B1 (ja) |
JP (1) | JP5828293B2 (ja) |
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WO2015030064A1 (ja) * | 2013-08-27 | 2015-03-05 | 三菱マテリアル株式会社 | PNbZT薄膜の製造方法 |
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US10411183B2 (en) | 2014-03-27 | 2019-09-10 | Mitsubishi Materials Corporation | Composition for forming Mn-doped PZT-based piezoelectric film and Mn-doped PZT-based piezoelectric film |
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JP2017228760A (ja) * | 2016-06-17 | 2017-12-28 | キヤノン株式会社 | 圧電体基板及びその製造方法、ならびに液体吐出ヘッド |
JP2019220638A (ja) * | 2018-06-22 | 2019-12-26 | 三菱マテリアル株式会社 | Knn膜形成用液組成物及びこの液組成物を用いたknn膜の形成方法 |
WO2019244673A1 (ja) * | 2018-06-22 | 2019-12-26 | 三菱マテリアル株式会社 | Knn膜形成用液組成物及びこの液組成物を用いたknn膜の形成方法 |
JP7192262B2 (ja) | 2018-06-22 | 2022-12-20 | 三菱マテリアル株式会社 | Knn膜形成用液組成物及びこの液組成物を用いたknn膜の形成方法 |
JP2020057713A (ja) * | 2018-10-03 | 2020-04-09 | キヤノン株式会社 | 配向性圧電体膜およびその製造方法、圧電体素子、並びに、液体吐出ヘッド |
JP7166866B2 (ja) | 2018-10-03 | 2022-11-08 | キヤノン株式会社 | 配向性圧電体膜およびその製造方法、圧電体素子、並びに、液体吐出ヘッド |
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Publication number | Publication date |
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CN102787356B (zh) | 2016-10-05 |
EP2525393A2 (en) | 2012-11-21 |
JP5828293B2 (ja) | 2015-12-02 |
US20150104637A1 (en) | 2015-04-16 |
TWI613725B (zh) | 2018-02-01 |
KR20120128567A (ko) | 2012-11-27 |
US20120295100A1 (en) | 2012-11-22 |
TW201314774A (zh) | 2013-04-01 |
CN102787356A (zh) | 2012-11-21 |
EP2525393B1 (en) | 2020-10-21 |
EP2525393A3 (en) | 2014-07-09 |
KR101926194B1 (ko) | 2018-12-06 |
US8951603B2 (en) | 2015-02-10 |
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