JP6599998B2 - 電解質形成方法 - Google Patents
電解質形成方法 Download PDFInfo
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- JP6599998B2 JP6599998B2 JP2017541329A JP2017541329A JP6599998B2 JP 6599998 B2 JP6599998 B2 JP 6599998B2 JP 2017541329 A JP2017541329 A JP 2017541329A JP 2017541329 A JP2017541329 A JP 2017541329A JP 6599998 B2 JP6599998 B2 JP 6599998B2
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- H01M8/1213—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the electrode/electrolyte combination or the supporting material
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- H01M8/1246—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the process of manufacturing or by the material of the electrolyte the electrolyte consisting of oxides
- H01M8/126—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the process of manufacturing or by the material of the electrolyte the electrolyte consisting of oxides the electrolyte containing cerium oxide
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B18/00—Layered products essentially comprising ceramics, e.g. refractory products
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Description
・移動可能な酸素イオンの形態でカソード(正の空気極)とアノード(負の燃料極)間に電流が流れることを可能にすること。
・セル内での内部短絡を引き起こしうる電子の形態での電極間の電流の通過を妨げること。
・燃料と空気の混合を防止すること、すなわち、電解質は理論密度の少なくとも95%である必要があり、相互接続空隙がなく、そのため電解質層がガス不透過性であり、欠陥が実質的にないこと。
・いくつかのセル(例えば英国特許第2,368,450号に定義されている本出願人のセルなど)は、セルの電気化学の近傍で燃料側反応物と酸化剤側反応物が混合するのを防止するために、電極の1つ(名目上はアノード)の周りの金属基材に接着させることにより気密エッジシールを備えること。
・金属基材の過度の酸化をもたらさない温度(フェライト系ステンレススチール基材を使用するCeres Power設計で典型的には1100℃未満)で電解質層を理論密度の>95%に焼結させること。
・非収縮性金属支持体上に電解質層を焼結させること。これは、焼結収縮が一次元に制約されることを意味し、焼結時の収縮制限が、制約がない等方性焼結に比べて緻密化を阻害することが知られている。
・セラミック層に欠陥を導入することまたは誘発させることを防止する堆積法を開発すること。
a.ドープセリア粉末を必要に応じて焼結助剤及び溶媒と組み合わせてスラリーを形成する工程;
b.前記スラリーをアノード層に適用する工程;
c.乾燥させてグリーン電解質を形成する工程;及び
d.前記グリーン電解質を焼成して焼結電解質を形成する工程;
のうちの1つまたは2つ以上を含み、工程bにおけるスラリーが、二峰性粒度分布、15〜40m2/gの範囲内のBET表面積、球状形態、または、それらの組み合わせから選ばれた物理的特性を有するドープセリア粉末を含む方法が提供される。
a.多くの場合15〜40m2/gの範囲内のBET表面積および/またはほぼ球状の形態を有するドープセリア粉末(典型的にはガドリニウムドープセリア粉末)を、焼成助剤、典型的にはTMO焼結助剤であって、必要に応じて1〜10μmの範囲内の粒度を有する焼結助剤、及び、溶媒と組み合わせて、スラリーを形成する工程;
b.必要に応じて、スラリーをミリングして二峰性粒度分布のドープセリア粉末を生成させる工程;
c.必要に応じて、分散剤、バインダーおよび界面活性剤のうちの1種または2種以上を必要に応じてスラリーに添加することによって、インク、典型的にはスクリーン印刷可能なインクを形成する工程;
d.必要に応じて、金属基材にアノード層を適用する工程、前記金属基材は、必要に応じて非穿孔領域により囲まれた穿孔領域を含み、独立に必要に応じてスチール基材である;
e.必要に応じて、アノード層を焼成する工程;
f.スラリーを、必要に応じて複数層で、アノード層に適用する工程;
g.乾燥させてグリーン電解質を形成する工程;
h.必要に応じて、グリーン電解質からいかなる溶媒及び有機物も除去する工程であって、必要に応じて100〜250℃の範囲内の温度で必要に応じて溶媒の蒸発によって、必要に応じて250〜500℃の範囲内の温度に必要に応じて5〜20分間の範囲内の時間加熱することより必要に応じて有機物の分解によって、グリーン電解質から溶媒及び有機物を除去する工程;
i.必要に応じて、グリーン電解質をプレスしてグリーン電解質の密度を増加させる工程であって、必要に応じて50〜500MPaの範囲内の圧力を印加することによりグリーン電解質をプレスしてグリーン電解質の密度を増加させ、圧力が必要に応じて冷間等方圧プレス、一軸ブラダープレスまたはこれらの組み合わせを使用して印加される工程;
j.必要に応じて、アノードも電極材料も適用されていない金属支持体の部分の少なくとも一部に素材を適用して電解質の焼結中に金属支持体の少なくともその部分を平坦に保つ工程;および
k.グリーン電解質を焼成して焼結電解質を形成する工程であって、必要に応じて800〜1000℃の温度範囲内の間に5〜20℃/分の範囲内の昇温速度で、必要に応じて20〜120分間の範囲内の全加熱時間で、グリーン電解質を焼成して焼結電解質を形成する工程。
本発明に関連する発明の実施態様の一部を以下に示す。
[態様1]
金属支持型固体酸化物燃料電池用の電解質を形成する方法であって、
a.ドープセリア粉末を焼結助剤及び溶媒と組み合わせてスラリーを形成する工程;
b.前記スラリーをアノード層に適用する工程;
c.乾燥させてグリーン電解質を形成する工程;及び
d.前記グリーン電解質を焼成して焼結電解質を形成する工程;
を含み、工程bにおけるスラリーが、二峰性粒度分布、15〜40m 2 /gの範囲内のBET表面積、球状形態、または、それらの組み合わせから選ばれた物理的特性を有するドープセリア粉末を含む、方法。
[態様2]
アノード層の適用前に前記スラリーをアトリッションミリングするさらなる工程を含む、上記態様1に記載の方法。
[態様3]
前記二峰性粒度分布が、0.1〜0.4μmの範囲内のピークと0.5〜1.5μmの範囲内のピークを成す粒子から構成される、上記態様1又は2に記載の方法。
[態様4]
前記焼結助剤が全カチオンの0.5〜5%の範囲内で存在する、上記態様1〜3のいずれか一つに記載の方法。
[態様5]
スクリーン印刷可能なインクから前記グリーン電解質を形成するさらなる工程を含む、上記態様1〜4のいずれか一つに記載の方法。
[態様6]
前記グリーン電解質が、前記アノード層上に複数層に前記スラリーを適用し、各層の適用の間に乾燥させることにより形成された複数の電解質層を含む、上記態様1〜5のいずれか一つに記載の方法。
[態様7]
前記アノード層が焼結アノード層である、上記態様1〜6のいずれか一つに記載の方法。
[態様8]
前記アノード層がグリーンアノード層であり、前記グリーンアノード層及びグリーン電解質が単一焼成工程で焼結される、上記態様1〜6のいずれか一つに記載の方法。
[態様9]
前記電解質が前記アノード層及び金属支持体を覆う、上記態様1〜8のいずれか一つに記載の方法。
[態様10]
工程dの焼結温度が1100℃未満である、上記態様1〜9のいずれか一つに記載の方法。
[態様11]
工程dの焼結プロセスが空気中で実施される、上記態様1〜10のいずれか一つに記載の方法。
[態様12]
前記アノード層に前記スラリーを適用した後であるがグリーン電解質の焼成前に、プレス工程をさらに含む、上記態様1〜11のいずれか一つに記載の方法。
[態様13]
上記態様1〜12のいずれか一つに記載の方法を使用して金属支持型アノード層上に電解質を形成すること、及び、前記電解質にカソード材料を適用することを含む、燃料電池を形成する方法。
[態様14]
上記態様1〜13のいずれか一つに記載の方法により得られる電解質。
[態様15]
上記態様14に記載の電解質を含む燃料電池。
[態様16]
上記態様15に記載の燃料電池を少なくとも2つ含む燃料電池スタック。
[態様17]
電気エネルギーの生成における上記態様14又は15に記載の燃料電池又は燃料電池スタックの使用。
[態様18]
図面を参照して本明細書に実質的に記載したとおりの、方法、電解質、燃料電池、燃料電池スタック及び使用。
Claims (14)
- 金属支持型固体酸化物燃料電池用の電解質を形成する方法であって、
a.ドープセリア粉末を焼結助剤及び溶媒と組み合わせて電解質スラリーを形成する工程;
b.前記電解質スラリーを、金属基材上に支持されたアノード層に適用する工程;
c.前記電解質スラリーを乾燥させてグリーン電解質を形成する工程;及び
d.前記グリーン電解質を1100℃未満の焼結温度で焼成して焼結電解質を形成する工程;
を含み、工程bにおける電解質スラリーが、二峰性粒度分布、15〜40m2/gの範囲内のBET表面積及び球状形態を有するドープセリア粉末を含む、方法。 - 前記電解質スラリーを前記アノード層に適用する前に前記電解質スラリーをアトリッションミリングするさらなる工程を含む、請求項1に記載の方法。
- 前記二峰性粒度分布が、0.1〜0.4μmの範囲内のピークと0.5〜1.5μmの範囲内のピークを成す粒子から構成される、請求項1又は2に記載の方法。
- 前記焼結助剤が全カチオンの0.5〜5%の範囲内で存在する、請求項1〜3のいずれか一項に記載の方法。
- 前記電解質スラリーがスクリーン印刷可能なインクを構成する、請求項1〜4のいずれか一項に記載の方法。
- 前記グリーン電解質が、工程aと工程dとの間に工程bと工程cとが繰り返されるように、前記電解質スラリーを前記アノード層上に複数層に適用し、各層の適用の間に乾燥を行うことにより形成された複数の電解質層を含む、請求項1〜5のいずれか一項に記載の方法。
- 前記アノード層が焼結アノード層である、請求項1〜6のいずれか一項に記載の方法。
- 前記アノード層がグリーンアノード層であり、前記グリーンアノード層及びグリーン電解質が単一焼成工程で焼結される、請求項1〜6のいずれか一項に記載の方法。
- 前記電解質が前記アノード層及び前記金属基材を覆う、請求項1〜8のいずれか一項に記載の方法。
- 前記金属基材がフェライト系ステンレススチール箔を含む、請求項1〜9のいずれか一項に記載の方法。
- 工程dの焼結プロセスが空気中で実施される、請求項1〜10のいずれか一項に記載の方法。
- 前記アノード層に前記電解質スラリーを適用した後であるがグリーン電解質の焼成前に、プレス工程をさらに含む、請求項1〜11のいずれか一項に記載の方法。
- 請求項1〜12のいずれか一項に記載の方法を使用して金属支持型アノード層上に電解質を形成すること、及び、前記電解質にカソード材料を適用することを含む、燃料電池を形成する方法。
- 工程bにおける前記電解質スラリーが、20〜40m 2 /gの範囲内のBET表面積を有するドープセリア粉末を含む、請求項1〜13のいずれか一項に記載の方法。
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ES2829048T3 (es) | 2021-05-28 |
RU2017127684A3 (ja) | 2019-06-03 |
DK3254326T3 (da) | 2020-11-09 |
WO2016124929A1 (en) | 2016-08-11 |
KR20170116064A (ko) | 2017-10-18 |
SG11201706319TA (en) | 2017-09-28 |
RU2017127684A (ru) | 2019-03-06 |
US10897056B2 (en) | 2021-01-19 |
TWI700857B (zh) | 2020-08-01 |
HK1215758A1 (zh) | 2016-09-09 |
CN113394439A (zh) | 2021-09-14 |
CA2974773C (en) | 2020-06-30 |
MX2017009781A (es) | 2017-12-04 |
GB2524638A (en) | 2015-09-30 |
EP3254326A1 (en) | 2017-12-13 |
HUE051968T2 (hu) | 2021-04-28 |
RU2696618C2 (ru) | 2019-08-05 |
GB201502032D0 (en) | 2015-03-25 |
KR102066121B1 (ko) | 2020-01-14 |
CN107223289A (zh) | 2017-09-29 |
CA2974773A1 (en) | 2016-08-11 |
JP2018508953A (ja) | 2018-03-29 |
GB2524638B (en) | 2016-04-06 |
CN107223289B (zh) | 2021-07-02 |
US20160233535A1 (en) | 2016-08-11 |
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