JP2019002700A - ガスセンサ素子に備わる電極の検査方法 - Google Patents
ガスセンサ素子に備わる電極の検査方法 Download PDFInfo
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Abstract
Description
図1は、本実施の形態に係る検査方法における検査対象の一例としてのガスセンサ100Aの構成を概略的に示す断面模式図である。図1(a)は、ガスセンサ100Aの主たる構成要素であるセンサ素子101Aの長手方向に沿った垂直断面図である。また、図1(b)は、図1(a)のA−A’位置におけるセンサ素子101Aの長手方向に垂直な断面を含む図である。本実施の形態に係る検査方法とは、概略、ガスセンサ100Aの製造プロセスにおいて、センサ素子101Aの表面に設けた検知電極10を対象に行う検査に関するものである。
図1に例示するような層構造を有するセンサ素子101Aは、例えば、特許文献1および特許文献2に開示されているような製造プロセスによる製造可能である。
次に、上述した製造プロセスを経て製造されたガスセンサ100Aを対象に、上述した種々の検査工程の1つとして行う、センサ素子101Aの表面に設けた検知電極10におけるAu濃化度の検査について説明する。
本態様では、Au存在比あるいはAu表面濃度と相関のある、検知電極10と基準電極20との間の反応抵抗(電極反応抵抗)を、センサ素子101Aの製造プロセス(量産プロセス)において代替濃化度指標として用いる。以下、センサ素子101Aにおける検知電極10と基準電極20との間の反応抵抗を単に、センサ素子101Aの反応抵抗とも称する。
750℃:y=250.69x+1803、R2=0.9684;
850℃:y=77.271x+218.5、R2=0.9522。
上述した第1の態様による検査は、反応抵抗を求めるために周波数を違えたインピーダンス測定を行う必要があることから、検査に時間を要する。本態様では、検知電極10におけるAu濃化度の検査を、第1の態様よりも簡易にかつ短時間で行うべく、検知電極10と基準電極20との間の直流抵抗を、Au濃化度を評価する際の代替濃化度指標として用いる。
上述の実施の形態でセンサ駆動温度として採用している640℃および850℃という温度を上下限値とする、640℃〜850℃という温度範囲は、上述したような混成電位型のガスセンサのセンサ素子のみならず、電気化学的ポンプセルを使用するような限界電流型のガスセンサに備わるセンサ素子など、他の種類のガスセンサにおいて用いられる、固体電解質体を用いた種々のセンサ素子についてのセンサ駆動温度をも含んでいる。例えば、電界電流型のNOxセンサのセンサ駆動温度は、800℃〜850℃程度に設定される。それゆえ、上述の実施の形態に係る検査方法は、混成電位型のガスセンサに備わるセンサ素子のみならず、固体電解質体を主構成材料とするセンサ素子であって、貴金属粒子の表面においてAuを濃化させたPt−Au合金を用いて形成された電極を備えるものについての、当該電極におけるAuの濃化度合いの評価に、適用が可能である。
10 検知電極
20 基準電極
30 基準ガス導入層
40 基準ガス導入空間
50 表面保護層
60 電位差計
70 ヒータ部
71 ヒータ電極
72 ヒータ
73 スルーホール
74 ヒータ絶縁層
75 圧力放散孔
100A ガスセンサ
101A センサ素子
E1 (センサ素子の)先端部
E2 (センサ素子の)基端部
Sa (センサ素子の)表面
Sb (センサ素子の)裏面
Claims (8)
- 酸素イオン伝導性の固体電解質からなるガスセンサ素子に備わる検査対象電極の貴金属粒子表面におけるAu濃化度を検査する方法であって、
前記検査対象電極は、貴金属成分としてPtおよびAuを含むものであり、
前記ガスセンサ素子は、内部にヒータを備えており、
前記Au濃化度は、前記検査対象電極を対象とするXPS分析あるいはAES分析の結果から算出される、前記貴金属粒子表面におけるAuが露出している部分の面積の比率に基づいて定義される値であり、
前記Au濃化度と、前記Au濃化度と相関を有しかつ前記ヒータにて所定の温度に加熱した前記ガスセンサ素子から非破壊で取得される所定の代替濃化度指標との関係を示す検量線を、あらかじめ作成しておく準備工程と、
検査対象である前記ガスセンサ素子を前記所定の温度に加熱した状態で当該ガスセンサ素子の前記検査対象電極についての前記代替濃化度指標の値を検査値として取得する検査値取得工程と、
前記準備工程で作成した前記検量線と前記検査値取得工程において取得された前記検査値とに基づいて前記検査対象電極におけるAu濃化度が所定の規格を満たしている否かを判定する判定工程と、
を備えることを特徴とする、ガスセンサ素子に備わる電極の検査方法。 - 請求項1に記載の検査方法であって、
インピーダンス測定によって求まる前記検査対象電極と前記ガスセンサ素子に備わる所定の基準電極との間の反応抵抗を前記代替濃化度指標とする、
ことを特徴とする、ガスセンサ素子に備わる電極の検査方法。 - 請求項1に記載の検査方法であって、
前記検査対象電極と前記ガスセンサ素子に備わる所定の基準電極との間に所定の直流電圧を印加したときの前記検査対象電極と前記基準電極との間の直流抵抗値を前記代替濃化度指標とする、
ことを特徴とする、ガスセンサ素子に備わる電極の検査方法。 - 請求項1に記載の検査方法であって、
前記検査対象電極と前記ガスセンサ素子に備わる所定の基準電極との間に所定の直流電圧を印加したときに前記検査対象電極と前記基準電極との間に流れる直流電流値を前記代替濃化度指標とする、
ことを特徴とする、ガスセンサ素子に備わる電極の検査方法。 - 請求項1ないし請求項4のいずれかに記載の検査方法であって、
前記Au濃化度が、前記貴金属粒子表面の全体の面積に対する前記Auが露出している部分の面積の比率であるAu表面濃度によって規定される、
ことを特徴とする、ガスセンサ素子に備わる電極の検査方法。 - 請求項1ないし請求項4のいずれかに記載の検査方法であって、
前記Au濃化度が、前記貴金属粒子表面におけるPtが露出している部分の面積に対する前記Auが露出している部分の面積の比率であるAu存在比によって規定される、
ことを特徴とする、ガスセンサ素子に備わる電極の検査方法。 - 請求項1ないし請求項6のいずれかに記載の検査方法であって、
前記所定の温度が640℃〜850℃である、
ことを特徴とする、ガスセンサ素子に備わる電極の検査方法。 - 請求項1ないし請求項7のいずれかに記載の検査方法であって、
前記ガスセンサ素子が、混成電位型のガスセンサ素子であり、
前記検査対象電極が、PtおよびAuとジルコニアとのサーメットからなり、被測定ガス中の測定対象ガス成分を検知する検知電極であり、
前記基準電極が、Ptとジルコニアとのサーメットからなる電極である、
ことを特徴とする、ガスセンサ素子に備わる電極の検査方法。
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