TW202411441A - 電化電池組件保護層之製作方法 - Google Patents

電化電池組件保護層之製作方法 Download PDF

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Publication number
TW202411441A
TW202411441A TW111148861A TW111148861A TW202411441A TW 202411441 A TW202411441 A TW 202411441A TW 111148861 A TW111148861 A TW 111148861A TW 111148861 A TW111148861 A TW 111148861A TW 202411441 A TW202411441 A TW 202411441A
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Taiwan
Prior art keywords
layer
stainless steel
component
coated
steel component
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TW111148861A
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English (en)
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湯瑪斯 沃勒
史蒂芬 克萊
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英商席瑞絲知識產權有限公司
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Publication of TW202411441A publication Critical patent/TW202411441A/zh

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/10—Fuel cells with solid electrolytes
    • H01M8/12—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte
    • H01M8/1286—Fuel cells applied on a support, e.g. miniature fuel cells deposited on silica supports
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
    • C23C10/02—Pretreatment of the material to be coated
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    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
    • C23C10/28—Solid state diffusion of only metal elements or silicon into metallic material surfaces using solids, e.g. powders, pastes
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    • C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
    • C23C10/28—Solid state diffusion of only metal elements or silicon into metallic material surfaces using solids, e.g. powders, pastes
    • C23C10/34—Embedding in a powder mixture, i.e. pack cementation
    • C23C10/36—Embedding in a powder mixture, i.e. pack cementation only one element being diffused
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    • C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
    • C23C10/28—Solid state diffusion of only metal elements or silicon into metallic material surfaces using solids, e.g. powders, pastes
    • C23C10/34—Embedding in a powder mixture, i.e. pack cementation
    • C23C10/52—Embedding in a powder mixture, i.e. pack cementation more than one element being diffused in one step
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    • C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
    • C23C10/28—Solid state diffusion of only metal elements or silicon into metallic material surfaces using solids, e.g. powders, pastes
    • C23C10/34—Embedding in a powder mixture, i.e. pack cementation
    • C23C10/58—Embedding in a powder mixture, i.e. pack cementation more than one element being diffused in more than one step
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    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
    • C23C14/025—Metallic sublayers
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    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • C—CHEMISTRY; METALLURGY
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    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58—After-treatment
    • C23C14/5806—Thermal treatment
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58—After-treatment
    • C23C14/5846—Reactive treatment
    • C23C14/5853—Oxidation
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/1601—Process or apparatus
    • C23C18/1633—Process of electroless plating
    • C23C18/1689—After-treatment
    • C23C18/1692—Heat-treatment
    • C23C18/1696—Control of atmosphere
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    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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    • C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
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    • C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
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    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
    • C23C8/10—Oxidising
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    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
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Abstract

本發明係關於一種電化電池組件保護層之製作方法及一種電化電池之製造方法。

Description

電化電池組件保護層之製作方法
本發明係關於電化電池領域。更詳言之，本發明係關於固態氧化物電池領域。
固態氧化物電池(SOC)包含三個基本部分，即通常為分設置之燃料電極、固態電解質及空氣或氧化劑電極，其可採管狀或平面配置。將多個平面固態氧化物電池單元彼此疊置可形成「堆」，其中個別電池單元呈電性串聯。SOC之運作溫度通常為600 °C至1000 °C。
SOC可採用固態氧化物燃料電池(SOFC)或固態氧化物電解器電池(SOEC)之方式運行。SOFC係可將電化燃料轉換為電力之能量轉換裝置。詳言之，SOFC藉由電化轉換程序使燃料氧化而產生電力。此程序之進行係使燃料或重組燃料與燃料電極接觸，並使例如空氣或富氧流體等氧化劑與氧化劑電極接觸。而後固態氧化物電解質將負氧離子自氧化劑電極傳導至燃料電極。因此，於SOFC中，燃料電極構成陽極而空氣或氧化劑電極構成陰極。SOEC則是以與SOFC相反模式所運作之SOC，通常用於將水電解而產生氫及氧氣。在SOEC中是以燃料電極構成陰極而空氣或氧化劑電極構成陽極。
燃料電極、固態電解質及空氣或氧化劑電極可為自支撐結構(「電解質支撐型」、「陰極支撐型」或「陽極支撐型」SOC)或分排列在機械性支座上。就現代SOC中之機械性支座及其他電池重複單位構成組件(例如分隔板、互連組件或間隔板或集電片)而言，以不鏽鋼為材質具有多種優於如陶瓷等習用材料之益處。詳言之，不鏽鋼材質之機械性支座更有利於SOC之緊密設計，因而具有提高功率密度之優點。此種SOC通常稱為金屬支撐型SOC (「MS-SOC」)。MS-SOC中之機械性支座可為以粉末金屬前驅物(例如藉由刮刀成形方式產生)所形成之本質多孔金屬基材製成。或更佳者，所述機械性支座上是在金屬支板上設置受非多孔(實心)區域包圍之穿孔或小洞組成之多孔區域。多孔區域貫穿金屬支板，燃料電極塗覆於此區域上，其上在依序塗覆其他體，因而金屬基板可發揮支撐此等堆疊體之效。
然而，在SOC中採用鋼材有其缺點，亦即，以一般鋼材製作之組件在SOC運作條件(例如氧化氣氛及550 - 1000 °C之溫度範圍)下容易發生高溫腐蝕，尤其是氧化，因而對SOC壽命產生不利影響。為避免腐蝕，通常會採用特殊之抗蝕不鏽鋼，例如Hitachi ZMG 232 G10、Sandvik Sanergy HT、Crofer 22 APU、Plansee ITM，但此類特殊鋼材價格較一般等級鋼材昂貴。一種已知替代辦法為採用標準等級不鏽鋼，並於其上設置防蝕。但目前之塗設置方式同樣成本高昂，且製成之塗雖具防護性，亦具絕緣性，不利於燃料電池性能。
本發明係關於一種電化電池組件保護層之製作方法。較佳者，所述電化電池為固態氧化物電池，更佳者為金屬支撐型固態氧化物電池。
所述組件是以鉻(Cr)含量為10%wt以上之不鏽鋼製成。所述不鏽鋼製組件可為機械性支座、SOC等金屬支撐型電化電池之透氣支撐或電化電池之互連組件。所述不鏽鋼製組件可為電化電池中之任何板狀或片狀不鏽鋼組件(例如分隔板或集電片)。所述不鏽鋼製組件可為由粉末金屬前驅物所形成之本質多孔金屬基材，或可由金屬支撐板製成，所述金屬支撐板包含設有通孔或小孔之多孔區域及圍繞多孔區域之非多孔(實心)區域。
所述方法包含步驟(i)、步驟(ii)及對至少一不鏽鋼製之組件進行處理之隨選步驟(iii)。
於步驟(i)中，對至少一以不鏽鋼製成之組件塗覆一塗層。對該至少一以不鏽鋼製組件塗覆之範圍可涵蓋其整個外表面。或者，可僅於其外表面之一部分進行塗覆，例如在其整個外表面之一(或多)面。較佳者，塗覆範圍至少為其表面之完整一面。
所述塗層可為單層，包含鈮(Nb)、鈦(Ti)、鋯(Zr)及/或鎢(W)。或者，所述塗層可為多層塗層，其中至少一包含鈮(Nb)、鈦(Ti)、鋯(Zr)及/或鎢(W)(亦即金屬間相形成層)。
在步驟(ii)中對該至少一經塗覆之不鏽鋼製組件進行熱處理。所述熱處理係在至少為1000 °C且至多為1200 °C之溫度中進行。較佳者，所述熱處理係在至少為1050 °C且至多為1100 °C之溫度中進行。所述熱處理之持續時間至少為30分鐘且至多為5小時，尤以2小時以內為佳。在熱處理步驟中，該至少一經塗覆之不鏽鋼製組件係保持在低於50 mbar之低壓氣氛或真空中。為此，步驟(ii)之熱處理可在一圍合空間中執行，例如在一真空烘箱中執行。
於隨選步驟(iii)中，可在至少為800 °C且至多為1000 °C之溫度中對該至少一經塗覆之不鏽鋼製組件進行熱處理而使之氧化。較佳者，在步驟(iii)中，所述熱處理是在一含氧氣氛中持續至少 30分鐘且至多5小時。步驟(iii)之熱處理可在周遭空氣中執行，較佳者是在大氣壓力中執行。
利用本發明方法可在不鏽鋼製組件上形成具有高度抗蝕性之保護層，延長電池運作壽命，且製造成本低廉。所述保護層可採用相對廉價之標準等級鋼材(例如1.4016,1.4509)製作，因此可大幅降低成本。其侵蝕防護原理係在不鏽鋼製組件之表面區域形成至少一金屬間相(intermetallic phase)(亦稱為金屬互化物)。在步驟(ii)之熱處理過程中，鈮(Nb)、鈦(Ti)、鋯(Zr)及/或鎢(W)等元素擴散進入不鏽鋼組件表面。因此可在不鏽鋼組件之近表面區域中形成富鐵金屬間相。此等金屬間相兼具高度抗蝕能力與良好導電性。
所述塗層可施作為多層。如此可進一步提升防蝕性能。例如，藉由調整個別子層之順序及材料組成，可控制擴散程序及因此形成保護塗層之相及/或微結構。此外，多層塗層對不鏽鋼製組件之附著力更強。
於所述程序之一種範例中，步驟(i)製作之塗層為多層，並於步驟(ii)中接受熱處理。所述多層除至少一由鈮(Nb)、鈦(Ti)、鋯(Zr)及/或鎢(W)所構成構成之(金屬間相形成)層外，並可包含至少一含有鉿(Hf)或如鈰(Ce)、鑭(La)或釔(Y)等稀土元素之層。稀土元素有助於提升抗蝕性且能夠有助於加強步驟(iii)中或SOFC運作條件下所形成氧化物之附著。除此之外或以為替代，所述多層除上述至少一由鈮(Nb)、鈦(Ti)、鋯(Zr)及/或鎢(W) 所構成構成之層外，並可包含至少一由鉻(Cr)、鉬(Mo)、釩(V)、錳(Mn)、鈷(Co)、矽(Si)或鋁(Al)中之一或多種所構成之層。此等元素可促進至少一金屬間相之形成。詳言之，至少一金屬間相可包含鉻(Cr)、鉬(Mo)、釩(V)、錳(Mn)、鈷(Co)、矽(Si)或鋁(Al)等元素，以進一步提升抗蝕性。此外，於執行步驟(iii)後，矽(Si)及鋁(Al)可額外形成防護性氧化物(例如氧化矽(SiO 2)、氧化鋁(Al 2O 3))。
於所述程序之一種範例中，可在步驟(ii)後施作至少一附加層。例如，在步驟(i)中將塗層施作成多層，並於執行步驟(ii)後將至少一附加層施作於此多層上。或者，可在步驟(i)中將塗層施作為單層，並於執行步驟(ii)後將至少一附加層施作於此單層上。步驟(ii)後所施作之至少一附加層可為一由鉻(Cr)、鉬(Mo)、釩(V)、錳(Mn)、鈷(Co)、矽(Si)、鈦(Ti)、銅(Cu)或鋁(Al)中之一或多種所構成之層。較佳者，所述附加層係由鋁(Al)或矽(Si)所構成。較佳者，至少一附加層可在執行步驟(iii)前施作。
於所述程序之另一範例中，可將第一層直接塗覆於不鏽鋼製組件上，再將第二層塗覆於第一層上。較佳者，所述第一層係由鈮(Nb)、鈦(Ti)、鋯(Zr)及/或鎢(W)所構成，而所述第二層係由鉻(Cr)、鉬(Mo)、釩(V)、錳(Mn)、鈷(Co)、矽(Si)、鈦(Ti)、銅(Cu)或鋁(Al)中之一或多種所構成。可在熱處理步驟(ii)中對由鈮(Nb)、鈦(Ti)、鋯(Zr)及/或鎢(W)所構成之第一層進行熱處理之前或之後施作第二層。可於步驟(iii)對所述第二層進行氧化後進一步將不鏽鋼製組件加工形成具保護功效之氧化物(例如氧化鋁(Al 2O 3)、氧化矽SiO 2))。
於所述程序之另一範例中，於步驟(i)中，第一層可直接塗覆於不鏽鋼製組件上，且第二層可塗覆於第一層上。第一層可為由鉿(Hf)或鈰(Ce)、鑭(La)或釔(Y)等稀土元素所構成，第二層可為由鈮(Nb)、鈦(Ti)、鋯(Zr)及/或鎢(W)所構成。此種多層結構有助於提升保護層對不鏽鋼製組件之附著力。若可於第二層上再覆蓋一第三層則更為有益，其中，該第三層係由鉻(Cr)、鉬(Mo)、釩(V)、錳(Mn)、鈷(Co)、矽(Si)、鈦(Ti)、銅(Cu)或鋁(Al)所構成。較佳者，所述第三層係由鋁(Al)或矽(Si)所構成。所述第三層可在步驟(ii)中對第一層及第二層進行熱處理之前或之後塗覆上。具體是，所述第三層是在步驟(iii)執行前施作。較佳者，於步驟(iii)中先將所述第三層氧化，而後再進行不鏽鋼製組件之加工以形成保護性氧化物(例如氧化鋁(Al 2O 3)、氧化矽SiO 2))。
為避免不鏽鋼製組件在步驟(ii)之熱處理過程中發生氧化，可在惰性氣體氣氛中進行熱處理。較佳者，所述熱處理係在一氣氛中執行，所述氣氛具體是包含氬(Ar)、氦(He)或氮(N 2)中之一或多種。
或者，步驟(ii)之熱處理可在一還原氣氛中執行，具體是含有氫(H 2)之氣氛。或者，步驟(ii)之熱處理亦可在含有氬(Ar)、氦(He)、氮(N 2)及氫(H 2)中二或多種之混合物之氣氛中執行。
在某些實施例中，一或多個所述塗覆塗層可藉由物理氣相沉積法製作，具體是利用磁控濺鍍技術。與此相輔或以為替代，一或多個所述塗覆塗層可利用電漿輔助熱蒸鍍或電子束蒸鍍法製作。與此相輔或以為替代，一或多個所述塗覆塗層可利用化學沉積法或電化沉積法製作。
在某些實施例中，所述塗層可具有至少為10 nm、具體是至少為25 nm、具體是至少為50 nm之塗層厚度及/或小於2000 nm、具體是小於1000 nm、具體是小於500 nm之塗層厚度。
本發明亦關於一種製造一電化電池之方法。所述電化電池包含至少一燃料電極、一電解質、一空氣或氧化劑電極及至少一以不鏽鋼製成之組件，其所用不鏽鋼之鉻(Cr)含量超過10%wt。例如，燃料電極可包含氧化鎳或鎳-釔安定氧化鋯(Ni-YSZ)。固態電解質層可包含釔安定氧化鋯(YSZ)、氧化釓摻雜鈰或鈰釓氧化物(CGO)。空氣或氧化劑電極可包含鑭鍶氧化錳((La,Sr)MnO3)、鑭鍶氧化鈷((La, Sr)CoO3)、氧化鑭鎳(LaNiO3)或氧化鑭鐵(LaFeO3)。
所述電化電池製造方法包含步提供至少一以不鏽鋼製成之組件以及藉由上述方法在所述至少一以不鏽鋼製成之組件上塗覆一塗層。上述關於保護層製作方法所說明之特性及優點亦適用於此電化電池製造方法。在不鏽鋼組件上塗覆保護層後，亦即至少執行上述步驟(i)、步驟(ii)及隨選之步驟(iii)後，可進行電化電池之組裝步驟。較佳者，電化電池之組裝步驟包含施作一燃料電極、一電解質及一空氣或氧化劑電極。
所述電化電池可為固態氧化物電池。所述電化電池可為固態氧化物燃料電池(SOFC)。此時，燃料電極構成電池陽極而空氣或氧化劑電極構成電池陰極。或者，所述電化電池可為固態氧化物電解器電池(SOEC)。此時，燃料電極構成電池陰極而空氣或氧化劑電極構成電池陽極。
所述電化電池可為金屬支撐型電化電池，例如金屬支撐型固態氧化物電池。在某些實施例中，所述至少一以不鏽鋼製成之組件可為一電化電池中之機械性支座、透氣載體或互連組件(例如電池重複單位)，且具體是固態氧化物電池中之機械性支座，更佳者為固態氧化物電池中之透氣載體。此時，電化電池之組裝步驟可包含在機械性支座上施作一燃料電極、一電解質及一空氣或氧化劑電極(取決於電池種類，電極層順序可能相反)。
藉由以下說明及圖示可推知更多實施方式。
圖1至圖4依據多種範例概要繪示於其外表面頂面14設有保護層12之不鏽鋼製組件10。如將於下文詳述者，所述保護層12可為單層(見圖1)或為多層(見圖2至圖4)。所述不鏽鋼製組件10可為電化電池中之機械性支座、互連裝置或透氣支撐件(例如電池重複單位)，較佳者為固態氧化物燃料電池或固態氧化物電解器電池(圖未示)中之組件。所述電化電池可於保護層12施作在不鏽鋼製組件10上之後組裝。
依據圖1所示之第一實施例，在步驟(i)中於不鏽鋼製組件10上塗覆由鈮(Nb)、鈦(Ti)、鋯(Zr)及/或鎢(W)由所構成之單層16。隨後，在步驟(ii)中對經塗覆之不鏽鋼製組件10進行熱處理，其中，該熱處理係在至少為1000 °C且至多為1200 °C之溫度中執行，具體是至少為1050 °C且至多為1100 °C之溫度。所述熱處理係執行達至少為30分鐘且至多為5小時之持續時間，具體是至多為2小時之持續時間。在熱處理過程中，係將經塗覆之不鏽鋼製組件10保持在小於50 mbar之低壓氣氛中或維持在真空中。在熱處理期間，(Nb)、鈦(Ti)、鋯(Zr)或鎢(W)自單層16擴散進入組件10之表面，因此使得富鐵金屬間相形成於不鏽鋼製組件10進表面區域。
依據圖2所示之第二實施例，繼步驟(ii)後，在由鈮(Nb)、鈦(Ti)、鋯(Zr)或鎢(W)所構成之第一層16上施作一由鋁或矽所構成之附加層18。待附加層18施作完成，於步驟(iii)中藉由一附加熱處理使經塗覆之不鏽鋼製組件10氧化，形成防護氧化物，亦即氧化鋁(Al 2O 3)或氧化矽(SiO 2)。步驟(iii)中之附加熱處理是在含氧氣氛中於至少為800 °C且至多為1000 °C之溫度下達至少為30分鐘且至多為5小時之持續時間，其中所述含氧氣氛，具體是周遭空氣，具體是大氣壓力。
依據圖3所示之第三實施例，在步驟(ia)中，於不鏽鋼製組件10上塗覆第一層20，其中，該第一層20係由鉿(Hf)或一稀土元素所構成，所述稀土元素具體是鈰(Ce)、鑭(La)或釔(Y)。隨後，於步驟(ib)中，在第一層20上塗覆第二層22，其中，該第二層22係由鈮(Nb)、鈦(Ti)、鋯(Zr)或鎢(W)所構成。隨後，在步驟(ii)中，對已塗覆有第一層20及第二層22之不鏽鋼製組件10進行熱處理以形成上述之金屬間相。例如，步驟(ii)中，熱處理是在至少為1000 °C且至多為1200 °C之溫度中執行，具體是至少為1050 °C且至多為1100 °C之溫度。所述熱處理可達例如至少為30分鐘且至多為5小時之持續時間，具體是至多為2小時之持續時間。於熱處理期間，經塗覆之不鏽鋼製組件10係保持在低於50 mbar之低壓氣氛或真空中。
依據圖4所示之第四實施，在由鈮(Nb)、鈦(Ti)、鋯(Zr)或鎢(W)所構成之第二層22上再施作一由鋁或矽所構成之附加層24。施作附加層24後，於步驟(iii)中藉由附加熱處理使經塗覆之不鏽鋼製組件10氧化，形成防護氧化物，亦即氧化鋁(Al 2O 3)或氧化矽(SiO 2)。步驟(iii)中之附加熱處理例如是在含氧氣氛中於至少為800 °C且至多為1000 °C之溫度下達至少為30分鐘且至多為5小時之持續時間，其中，所述含氧氣氛，具體是周遭空氣，具體是大氣壓力。
在不鏽鋼製組件10上施作保護層12後，即可進行電化電池之組裝。例如，所述不鏽鋼製組件10可為固態氧化物燃料電池或固態氧化物電解器電池中之機械性支座。此時，組裝SOFC或SOEC之步驟可包括在已設有保護層12之不鏽鋼製組件10上塗覆一燃料電極、一固態電解質及一空氣或氧化劑電極(取決於電池種類，個別電極順序可能相反)。
10:組件 12:保護層 14:頂面 16:單層/第一層 18:附加層 20:第一層 22:第二層 24:附加層
[圖1]為依據第一實施例所繪製經塗覆之不鏽鋼製組件示意圖。 [圖2]為依據第二實施例所繪製經塗覆之不鏽鋼製組件示意圖。 [圖3]為依據第三實施例所繪製經塗覆之不鏽鋼製組件示意圖。 [圖4]為依據第四實施例所繪製經塗覆之不鏽鋼製組件示意圖。
10:組件
12:保護層
14:頂面
16:單層/第一層

Claims (17)

  1. 一種在一電化電池之一組件上製作一保護層之方法， 其中，該組件係以不鏽鋼製成，所述不鏽鋼之鉻(Cr)含量超過10%wt， 所述方法包含； 步驟(i)：在該不鏽鋼製組件上塗覆一塗層， 其中，該塗層為一由鈮(Nb)、鈦(Ti)、鋯(Zr)及/或鎢(W)所構成之單層結構，或為一多層結構，所述多層結構中包含至少一由鈮(Nb)、鈦(Ti)、鋯(Zr)及/或鎢(W)所構成之層體； 步驟(ii)：對經該塗覆之不鏽鋼製組件進行熱處理，其中，該熱處理係在一至少為1000 °C且至多為1200 °C之溫度中執行，且該熱處理係執行達至少為30分鐘且至多為5小時之持續時間，其中，該塗覆之不鏽鋼製組件在所述熱處理過程中係保持於一低於50 mbar之低壓氣氛中或保持於真空中。
  2. 如請求項1所述之方法，其中，在步驟(ii)中，所述熱處理係在一至少為1050 °C且至多為1100 °C之溫度中進行。
  3. 如請求項1或2所述之方法，其中，在步驟(ii)中，所述熱處理係執行達一至多為2小時之持續時間。
  4. 如以上任一請求項所述之方法，進一步包含一步驟(iii)：在一含氧氣氛中於一至少為800 °C且至多為1000 °C之溫度下對該經塗覆之不鏽鋼製組件進行熱處理達一至少為30分鐘且至多5小時之持續時間，使該經塗覆之不鏽鋼製組件氧化。
  5. 如以上任一請求項所述之方法，其中，於步驟(i)中該塗層係施作成一多層結構，該多層結構包含至少一由鉿(Hf)或一稀土元素所構成之層體(20)及/或至少一由鉻(Cr)、鉬(Mo)、釩(V)、錳(Mn)、鈷(Co)、矽(Si)或鋁(Al)所構成之層體，其中，該稀土元素較佳者為鈰(Ce)、鑭(La)或釔(Y)。
  6. 如以上任一請求項所述之方法，其中，於步驟(ii)後施作至少一附加層，其中，該附加層係由鉻(Cr)、鉬(Mo)、釩(V)、錳(Mn)、鈷(Co)、矽(Si)、鈦(Ti)、銅(Cu)或鋁(Al)所構成。
  7. 如以上任一請求項所述之方法，其中係在該不鏽鋼製組件上直接塗覆一第一層，並在該第一層上塗覆一第二層，其中，該第一層係由鈮(Nb)、鈦(Ti)、鋯(Zr)或鎢(W)所構成，且該第二層係由鋁(Al)、鈦(Ti)、鉻(Cr)、銅(Cu)、鈷(Co)、錳(Mn)或矽(Si)所構成。
  8. 如請求項7所述之方法，其中，該第二層係在一步驟(iii)中氧化。
  9. 如請求項1至6中任一項所述之方法，其中，該不鏽鋼製組件上直接塗覆有一第一層，且該第一層上塗覆有一第二層，其中，該第一層係由鉿(Hf)或一稀土元素所構成，所述稀土元素較佳者為鈰(Ce)、鑭(La)或釔(Y)，且該第二層係由鈮(Nb)、鈦(Ti)、鋯(Zr)及/或鎢(W)所構成。
  10. 如請求項9所述之方法，其中，該第二層上塗覆有一第三層，該第三層係由鉻(Cr)、鉬(Mo)、釩(V)、錳(Mn)、鈷(Co)、矽(Si)、鈦(Ti)、銅(Cu)或鋁(Al)所構成。
  11. 如請求項10所述之方法，其中，該第三層係於一步驟(iii)中氧化。
  12. 如以上任一請求項所述之方法，其中，在步驟(ii)中，該熱處理係在一含有氮(N 2)、氬(Ar)、氦(He)及氫(H 2)中一或多種之氣氛中執行。
  13. 如以上任一請求項所述之方法，其中，該保護層之施作係利用一物理氣相沉積法、利用一熱蒸鍍法或電子束蒸鍍法及/或利用一化學或一電化沉積方法。
  14. 如以上任一請求項所述之方法，其中，該保護層具有一至少為10 nm、具體是至少25 nm、具體是至少50 nm之塗層厚度，及/或一小於2000 nm、具體是小於1000 nm、具體是小於500 nm之塗層厚度。
  15. 如以上任一請求項所述之方法，其中，所述不鏽鋼製組件係一電化電池中之一機械性支座、一透氣載體或一互連組件，所述電化電池隨選為一固態氧化物燃料電池或一固態氧化物電解器電池。
  16. 一種製造一電化電池之方法，其中，該電化電池包含至少一燃料電極、一電解質、一空氣或氧化劑電極及至少一以不鏽鋼製成之組件，其中該不鏽鋼之鉻(Cr)含量高於10%wt，所述方法包含： a. 提供該至少一不鏽鋼製組件； b. 藉由如以上任一請求項所述之方法對所述至少一不鏽鋼製組件塗覆一保護層； c. 組裝該電化電池。
  17. 如請求項16所述之方法，其中，該至少一以不鏽鋼製成之組件係該電化電池中一機械性支座，且其中組裝該電化電池之步驟包含對其上設有該保護層之該機械性支座塗覆一燃料電極、一電解質及一空氣或氧化劑電極。
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