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TWI642801B - Sputtering target and manufacturing method thereof - Google Patents

Sputtering target and manufacturing method thereof Download PDF

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Publication number
TWI642801B
TWI642801B TW106139007A TW106139007A TWI642801B TW I642801 B TWI642801 B TW I642801B TW 106139007 A TW106139007 A TW 106139007A TW 106139007 A TW106139007 A TW 106139007A TW I642801 B TWI642801 B TW I642801B
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sputtering target
less
grinding
target
igzo
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TW106139007A
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TW201837213A (zh
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梶山純
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日商Ｊｘ金屬股份有限公司
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Abstract

本發明提供一種抑制電弧之IGZO濺鍍靶。
本發明之IGZO濺鍍靶含有In、Ga、Zn、O，其特徵在於：以原子比計為0.30≦In/(In+Ga+Zn)≦0.36、0.30≦Ga/(In+Ga+Zn)≦0.36、0.30≦Zn/(In+Ga+Zn)≦0.36，相對密度為96%以上，濺鍍靶表面之晶粒之平均粒徑為30.0μm以下，且濺鍍靶表面之粒徑之差異為20%以下(1.0≦Dmax/Dmin≦1.2)。

Description

濺鍍靶及其製造方法
本發明係關於一種濺鍍靶及其製造方法。更具體而言，關於一種IGZO濺鍍靶及其製造方法。
先前，期待IGZO薄膜用作薄膜電晶體，至今特別是顯示器之應用受到關注。該IGZO薄膜主要藉由濺鍍而形成。
於藉由濺鍍法而形成薄膜時，若產生顆粒，則會成為圖案不良等之原因。作為該顆粒之產生原因，最多的是於濺鍍中發生之異常放電(電弧)。特別是，若於靶表面產生電弧，則產生電弧之周邊之靶材以叢集狀(塊狀)自靶釋出。而且，該叢集狀態之靶材附著至基板。
就近年來之顯示器精度之問題而言，較先前更嚴格地要求濺鍍時之顆粒。為了解決此種濺鍍時之問題，嘗試提高靶之密度、或控制晶粒而獲得高強度之靶。
於日本特開2014-125422號公報中，揭示有如下情形：以改善IGZO薄膜之特性不均、以及改善製造靶時與濺鍍時發生的破裂為目的而對X射線繞射時之入射角(2θ)之繞射強度比進行控制。
[先前技術文獻] [專利文獻]
[專利文獻1]日本特開2014-125422號公報
近年來，以提高顯示器之品質要求、或氧化物半導體在新穎之設備的應用為背景而強烈地期望抑制電弧。鑒於此種情況，本發明之目的在於提供一種較先前進一步抑制電弧之產生的IGZO濺鍍靶。
IGZO靶之燒結體(剛燒結後)之組織結構通常於靶之表面部存在變質層。而且，於該變質層存在較多之粒內龜裂。因此，通常藉由充分地研削表面而去除表面之變質層。
然而，存在如下情形：即便充分地進行研削而去除變質層，亦仍產生電弧。本發明人進行調查，結果發現以下之情況。於研削靶材後之表面(濺鍍面)中，若晶粒之尺寸產生差異，則判斷產生電弧。進而，對詳細之原因進行研究，結果其原因為於剛燒結後之燒結體發生翹曲。更具體而言，為了將發生翹曲之燒結體加工成平坦之靶材而作為製品，通常進行研削。如圖2所示，為了實施平面研削，通常，視研削面之部分而研削量不同。例如，圖2之中央部與端部以相同之面進行比較時，研削量不同。結果距研削前之燒結體之表面之距離不同的部位露出至靶表面。
因此種距離差異而令熱處理之溫度影響不同之部位、即晶粒的尺寸不同之面露出至同一表面。
本發明人進行努力研究，結果發現如下情形：於燒結成形體時，在達到燒結溫度前保持在特定之溫度，藉此可抑制材料之翹曲量。進而，發現可確保於研削後露出之材料表面之晶粒的均一性。
基於上述見解，如下所述般特定本發明。
(發明1)
一種IGZO濺鍍靶，其含有In、Ga、Zn、O，其特徵在於：以原子比計為0.30≦In/(In+Ga+Zn)≦0.36、0.30≦Ga/(In+Ga+Zn)≦0.36、0.30≦Zn/(In+Ga+Zn)≦0.36，相對密度為96%以上，濺鍍靶表面之晶粒之平均粒徑為30.0μm以下，且濺鍍靶表面之粒徑之差異為20%以下(1.0≦Dmax/Dmin≦1.2)。
(發明2)
如發明1之IGZO濺鍍靶，其中，抗彎強度為40~100MPa，且抗彎強度之差異為20%以下(1.0≦Smax/Smin≦1.2)。
(發明3)
一種IGZO濺鍍靶之製造方法，上述方法包含如下步驟：於1300~1500℃對具有發明1或2之元素之組成的成形體進行5~24小時的燒結；及對燒結體進行研削；上述進行燒結之步驟包含將成形體於800℃~1000℃保持0.5~3小時，上述燒結後之燒結體之翹曲量為2.0mm以下，上述進行研削之步驟包含於消除翹曲後，進而追加研削0.5mm以上。
於一態樣中，本發明之濺鍍靶表面之粒徑的差異為20%以下。藉此，可抑制濺鍍時之電弧等。又，於一態樣中，本發明之濺鍍靶表面之強度的差異為20%以下。藉此，可有效地抑制發生破裂等。
圖1係表示粒徑及強度之取樣方法之圖。
圖2係表示燒結體之翹曲量及研削量之圖。
以下，對用以實施本發明之具體之實施形態進行說明。以下之說明係用以幫助理解本發明。即，並非意欲限定本發明之範圍。
1.靶材之特性
(1)形狀
於本發明之一實施形態中，濺鍍靶之形狀為平板。進而，於一實施形態中，濺鍍靶之形狀為矩形之平板。
(2)成分
於本發明之一實施形態中，濺鍍靶係含有In、Ga、Zn及O之IGZO濺鍍靶。
進而，於一實施形態中，IGZO濺鍍靶可分別按照以下之原子比含有In、Ga、Zn。
0.30≦In/(In+Ga+Zn)≦0.36
0.30≦Ga/(In+Ga+Zn)≦0.36
0.30≦Zn/(In+Ga+Zn)≦0.36
更佳為，可按照以下之原子比含有上述元素。
0.32≦In/(In+Ga+Zn)≦0.34
0.32≦Ga/(In+Ga+Zn)≦0.34
0.32≦Zn/(In+Ga+Zn)≦0.34
又，除上述元素以外，作為剩餘部分，例如亦可含有Sn及/或 Zr。作為含量，例如可分別為1000質量ppm以下、較佳為500質量ppm以下，典型而言，Sn為400質量ppm以下及/或Zr為200質量ppm以下。下限值並無特別限定，例如分別為0質量ppm以上，典型而言，可為Zr為100質量ppm以上及/或Sn為300質量ppm以上。
再者，可藉由螢光X射線分析(XRF)等而特定構成濺鍍靶材之元素之種類及含量。又，亦可藉由發光分光分析(ICP)而特定除In、Ga、Zn以外之元素。
(3)組織
於本發明之一實施形態中，IGZO濺鍍靶具有同型晶體結構(homologous crystal structure)。此處，所謂同型結構係指於含有In、Ga及Zn之氧化物之情形時，以InGaO3(ZnO)m(m為1~20之自然數)的組成式表示之六方晶單元之層狀結構。進而，於本發明之一實施形態中，IGZO濺鍍靶主要具有以InGaZnO4(InGaO3(ZnO)m，m=1)表示之同型結構。例如，IGZO濺鍍靶以80%以上、更佳為85%以上之比率具有同型晶體結構。
再者，可藉由利用XRD檢測峰值而辨別有無同型晶體結構。於本發明之一實施形態中，若藉由XRD進行分析，則IGZO濺鍍靶具有相當於InGaZnO4之峰值(應變等峰值位移可為±1°)。又，於本發明之一實施形態中，若藉由XRD進行分析，則IGZO濺鍍靶不與InGaZnO4一致之(即便考慮應變等峰值位移亦不一致)相的峰值強度、與InGaZnO4之峰值強度之比為20%以下(較佳為15%以下)。
例如，上述XRD之測定條件如下。
．X射線繞射裝置：RIGAKU股份有限公司製造之全自動水平型多用途X射線繞射裝置SmartLab(X射線源：Cu射線)；．測角器：Ultima IV．管電壓：40kV、 ．管電流：30mA、．掃描速度：5°/min、．步進：0.02°
背景去除：峰值強度係自藉由X射線繞射獲得之資料去除背景而算出各峰值強度。背景去除方法可使用Sonneveld-Visser法。
原料以上述In、Ga、Zn之原子比構成，且以下文敍述之溫度進行燒結，藉此可製造具有同型晶體結構之IGZO濺鍍靶。
(4)粒徑
於本發明之一實施形態中，IGZO濺鍍靶之結晶粒徑為30.0μm以下、更佳為25.0μm以下。若為該等範圍，則可適當地抑制顆粒或龜裂等。下限值並無特別限定，典型而言，可為5.0μm以上或7.0μm以上。
再者，如下所述般定義本說明書中所提及之結晶粒徑。如圖1所示，將靶材分割成9個區間(縱3等分×橫3等分)。自該9個區間之中央切割樣品。對於各樣品，分別對樣品之表面(製品面側)與背面(與背襯板之接著面側)進行鏡面研磨、蝕刻(2min)，藉由FE-EPMA實施組織觀察。於觀察、保存之組織照片中，在照片上描繪直線直至成為粒子數量N=200，使用存在於直線上之粒子數量(N200)與直線之總長度(L)，以L/N算出該觀察部位、即各區間之表面、背面的各粒徑。於各區間(18個區間)進行表面、背面之粒徑算出，將表面之9個區間之粒徑設為D1~D9，將背面之9個區間之粒徑定義為D10~D18。根據該18個部位之粒徑測定值而算出靶材之粒徑的最大及最小差異。又，靶之平均粒徑係根據各樣品之N、L之合計Nsum、Lsum而以Lsum/Nsum算出平均粒徑。
於本發明之一實施形態中，IGZO濺鍍靶之結晶粒徑之差異為20%以下。較佳為15%以下。再者，本說明書中敍述之結晶粒徑之差異能夠以上 述結晶粒徑D1~D18中的最大值Dmax與最小值Dmin之比(Dmax/Dmin)表示。下限值並無特別規定，典型而言，可為0%以上、1%以上或3%以上。
(5)相對密度
於本發明之一實施形態中，IGZO濺鍍靶之相對密度為96%以上，較佳為96.3%以上。若為96%以上，則進一步抑制電弧之產生。上限值並無特別是規定，典型而言，可為100%以下、99%以下、98%以下或97%以下。
再者，本說明書中所提及之相對密度係藉由(實測密度/真密度)×100(%)而算出。此處，「實測密度」之測定係使用阿基米德法。「真密度」係根據靶之各元素之分析值(重量%比)而換算成各氧化物即In2O3、Ga2O3、ZnO進行計算。各氧化物之密度使用In2O3：7.18g/cm3、Ga2O3：6.44g/cm3、ZnO：5.61g/cm3。
(6)抗彎強度
於本發明之一實施形態中，IGZO濺鍍靶之抗彎強度為40~100MPa，更佳為70~100MPa。抗彎強度係與上述結晶粒徑相同地將材料分割成9個部分而進行測定。更具體而言，以成為下文敍述之試樣尺寸之方式切出9個區間(縱3等分×橫3等分)之中心部分。而且，將分別自9個區間切割之試樣所測得之抗彎強度之值分別定義為S1~S9。而且，將S1~S9之平均值設為IGZO濺鍍靶之抗彎強度。
此處，抗彎強度可依據JIS R 1601而測定。於上述JIS標準中，試樣之厚度被規定為3mm。以加工成該厚度為目的而自表面及背面僅研削相同之量。而且，於分割成9個區間後，以成為4×40mm之矩形尺寸之方式自各區間之中央部分切出試樣。具體如下。
(抗彎強度之測定條件)
試驗方法：3點彎曲試驗
支點間距離：30mm
試樣尺寸：3×4×40mm
測頭速度：0.5mm/min
於本發明之一實施形態中，IGZO濺鍍靶之抗彎強度之差異亦可為20%以下。更佳亦可為16%以下。靶材係即便整體之抗彎強度較大，若局部地存在抗彎強度較小之部分，則亦存在由此發生破裂之可能性。然而，本發明之IGZO濺鍍靶其抗彎強度之差異為20%以下，藉此可更有效地抑制發生破裂。再者，本說明書中敍述之抗彎強度之差異能夠以上述抗彎強度S1~S9中的最大值Smax與最小值Smin之比(Smax/Smin)表示。下限值並無特別規定，典型而言，可為0%以上、1%以上或3%以上。
4.靶材之製造方法
(1)粉末
可使用分別含有In、Ga、Zn之粉末。更具體而言，可使用In化合物之粉末、Ga化合物之粉末、Zn化合物之粉末。或者，亦可使用含有該等元素之組合之粉末。作為In化合物之粉末之例，可列舉氧化銦、氫氧化銦等。作為Ga化合物之粉末之例，可列舉氧化鎵、硝酸鎵等。作為Zn化合物之粉末之例，可列舉氧化鋅、氫氧化鋅等。摻合量只要為可實現上述In、Ga、Zn之原子比之量即可。
(2)混合及粉碎
其次，粉碎該等原料粉末並進行混合。原料粉末之粉碎混合處理可使用乾式法或濕式法。於乾式法中，可列舉使用氧化鋯、氧化鋁、尼龍樹脂等之球或珠粒之乾式法。另一方面，於濕式法中，可列舉使用上述球或珠粒之介質攪拌研磨機。進而，於濕式法中，可列舉無介質之容器旋轉式、機械攪拌式、氣流式濕式法。此處，濕式法通常粉碎及混合能力優於乾式法。因此，較佳為使用濕式法進行混合。
粉碎後之粒子之尺寸並無特別限定，越小則越可提高相對密度，因此較理想。又，若粉碎不充分，則於所製造之靶中各成分偏析而存在高電阻率區域與低電阻率區域。藉此，於濺鍍成膜時成為異常放電之原因，該異常放電係因高電阻率區域帶電等引起之電弧等。因此，需要充分地混合及粉碎。
(3)成形
其次，將混合粉末填充至模具，以面壓400~1000kgf/cm2、保持1~3分鐘之條件進行單軸壓製而獲得成形體。若面壓未達400kgf/cm2，則無法獲得足夠密度之成形體。又，於生產上並不特別需要超過1000kgf/cm2之面壓。即，即便施加過大之面壓，成形體之密度亦變得難以提高至某個固定值以上。又，若實施超過1000kgf/cm2之面壓，則單軸壓製於原理上易於在成形體內產生密度分佈而成為燒結時之變形或破裂之原因。
其次，利用塑膠對該成形體進行雙層真空包裝，以壓力1500~4000kgf/cm2、保持1~3分鐘之條件實施CIP(冷均壓加壓法)。若壓力未達1500kgf/cm2，則無法獲得充分之CIP之效果。另一方面，即便施加超過4000kgf/cm2之壓力，成形體之密度亦變得難以提高至某個固定值以上。因此，於生產上並不特別需要超過4000kgf/cm2之面壓。成形體之尺寸並無特別規定，但若厚度過大，則變得難以獲得相對密度較高之燒結體。因此，較佳為以燒結體之厚度成為15mm以下之方式調節成形體之厚度。
(4)燒結
上述成形體能夠以適當之燒結溫度進行燒結而獲得燒結體。較佳為於升溫至燒結溫度前，暫時先保持於特定條件之範圍內。IGZO之燒結體之各種相係取決於溫度而增加及減少。例如，I2O3及ZnGa2O4等之相呈如下傾向：若升溫至800℃以上，則減少。另一方面，InGaZnO4之相呈如下傾向：若升溫超過1000℃，則急遽地開始成長。因此，藉由不瞬間升溫而保持於800℃~1000℃之溫度範圍 內，可抑制成為翹曲之原因的現象(即，燒結體內部之IGZO相之成長程度產生差異之現象)。而且，能夠以IGZO相之成長程度之差異得到抑制之狀態進行燒結。根據此種原因，較佳為設為800℃以上且1000℃以下(較佳為850℃~1000℃、進而較佳為880℃~920℃)。處理時間較佳為0.5小時以上、進而較佳為1小時以上。上限時間較佳為3小時以下。其原因在於：若變得長於3小時，則導致IGZO相之成長發展至燒結體整體，變得難以去除燒結體中之孔而導致相對密度下降或靶之抗彎強度下降等。
例如，可於上述時間之期間，以固定之溫度進行處理。或者，亦可於上述時間之期間，減小升溫速度(例如，0.1~0.3℃/min)而達到上述燒結溫度前花費固定時間。進行上述保持直至達到燒結溫度為止，藉此可抑制燒結體之翹曲。此種處理步驟於抑制具有於「1.靶材之特性」、「(2)成分」之段落敍述之組成及/或於「(3)組織」的段落敍述之組織結構之燒結體之翹曲的情形時特別有效。
其次，可於大氣環境或氧氣環境下，以溫度1300~1500℃(較佳為1350~1450℃)對成形體進行5~24小時(較佳為10小時~22小時、進而較佳為15~21小時)之燒結而獲得燒結體。若燒結溫度低於1300℃，則無法獲得足夠密度之燒結體。又，無法充分地獲得結晶相InGaZnO4。若燒結溫度超過1500℃，則有燒結體中晶粒之尺寸變得過大而使燒結體的機械強度下降之虞。又，若時間未達5小時，則無法獲得足夠密度之燒結體，若時間長於24小時，則於生產成本之觀點而言欠佳。
又，於成形、燒結步驟中，除上述方法以外，亦可使用HP(熱壓)或HIP(熱均壓加壓法)。如上所述般獲得之燒結體係藉由研削、研磨等機械加工而製成靶形狀，藉此可製作濺鍍靶。
燒結體之翹曲量為2.0mm以下，更佳為1.5mm以下。若為2.0mm 以下，則可將研削後之靶材表面之結晶粒徑之差異抑制在固定值以下。而且，可抑制電弧之產生。下限值並無特別規定，可為0mm以上、0.5mm以上或0.8mm以上。
再者，本說明書中敍述之翹曲量係使用簡易翹曲測定機(測定部：基恩士製造之LK-085)，將燒結後(機械加工前)之燒結體中之高度(Z座標)最高之部位、與最低之部位的高度差異設為「翹曲量」。
(5)研削
於獲得燒結體後，以加工成平坦之形狀為目的、且以去除變質層為目的而進行研削。研削係自兩個面進行，可獲得平板之靶材。因此，需至少研削至獲得平坦之形狀為止。例如，若翹曲量為2.0mm以上，則需研削至少2.0mm以上。更佳為，可於研削至翹曲消除為止後，進一步追加研削+0.5mm以上(即，將自平面之研削量設為0.5mm以上、更佳為0.8mm以上)。藉此，可縮小研削後之靶材表面之結晶粒徑之差異。又，藉此於研削至翹曲消除為止時，可去除殘留於表面之一部分之變質層。再者，「翹曲消除」之狀態不僅係指翹曲量為0mm之情形，而且還指翹曲量為0.1mm以下之狀態。關於研削量之上限值，就良率下降之原因而言，較佳為最大表面研削量為3.0mm以下，該最大表面研削量係將上述「翹曲消除為止」之研削量與「追加研削」量相加所得者。關於研削量之下限值，就典型之翹曲量為0.5mm以上、及較佳之追加研削量為0.5mm以上的原因而言，較佳為最大表面研削量為1.0mm以上，該最大表面研削量係將上述「翹曲消除為止」之研削量與「追加研削」量相加所得者。
經由以上之步驟可獲得作為本發明之目標之IGZO濺鍍靶。
5.靶材之有用性
於本發明之一實施形態中，可使用IGZO濺鍍靶並藉由通常進行之濺鍍法(例如，DC濺鍍法等)進行成膜。於本發明之一實施形態中，IGZO濺鍍靶之翹曲較 少，故而加工成平坦之狀態為止之研削量少於先前。因此，可減輕材料損耗。又，由於翹曲較少，故而可確保濺鍍面之均勻性。因此，可抑制電弧。又，材料整體之強度為固定以上，且強度之差異亦較少，故而難以發生破裂或龜裂。
[實施例]
(1)各種試驗條件
按照以下之條件實施試驗。
(1-1)靶材之分析
進行藉由螢光X射線分析(XRF)之In、Ga、Zn之元素分析。
(1-2)粒徑評估方法
藉由上述「1.靶材之特性」之「(4)粒徑」之項中所說明之方法進行評估。
(1-3)強度測定方法
藉由上述「1.靶材之特性」之「(6)抗彎強度」之項中所說明之方法進行評估。
(1-4)翹曲量之測定
使用簡易翹曲測定機(測定部：基恩士製造之LK-085)，將燒結後(機械加工前)之燒結體中之高度(Z座標)最高之部位與最低之部位的高度差異設為「翹曲量」。
(1-5)相對密度
藉由上述「1.靶材之特性」之「(5)相對密度」之項中所說明之方法進行評估。
(1-6)濺鍍條件
使用所獲得之燒結體並按照以下之條件進行DC濺鍍。
濺鍍氣體：Ar：100%
濺鍍氣壓：0.5Pa
輸入電力：500W
輸入電力量：20kWh
基板溫度：室溫
(2)實施例及比較例
以各金屬元素之比率、即In：Ga：Zn大致成為1：1：1之方式(具體而言，以成為表1中所記載之原子比之方式)藉由濕式方式對含有In2O3粉、Ga2O3粉、ZnO粉之基本材料(母材)進行混合、微粉碎，之後藉由噴霧乾燥器進行乾燥、造粒而獲得原料粉。將該原料粉投入模具，花費1分鐘運用800kgf/cm2之壓力來獲得成形體。於電爐內，按照表1之條件對該成形體進行加熱(於300~900℃之間以5℃/min之速度升溫、900℃以後係以0.5℃/min之速度升溫)而獲得燒結體(除比較例5以外，厚度為10mm)。此後，按照表1之條件並利用使用#80~#400之磨石的平面研削機進行研削來製作濺鍍靶(靶表面精加工為#400)。
此後，以上述條件評估相對密度、強度、粒徑。又，於上述條件下進行濺鍍，調查有無電弧。將結果示於表2。
保持在900℃之實施例1~3之靶其翹曲量較少，粒徑及強度之差異變小。又，亦可確保固定以上之相對密度。又，亦可將電弧之產生抑制至固定程度以下。另一方面，未進行保持於900℃下之比較例1其翹曲量變大，結果粒徑之差異亦變大。而且，電弧之產生變多。
實施例4與比較例2係提高燒結溫度而增大結晶粒徑之例。此處，與實施例1~3及比較例1相比，發現相同之傾向。
比較例3~4係與實施例1相同地進行保持於900℃下，但研削量不足，故而於表面殘留變質層，或粒徑之差異變大。
比較例5係以如下方式製作之例：為了達成與實施例1相同之粒徑之差異，將燒結體之厚度設為20mm，按照該程度增加研削量。粒徑差異本身可抑制在與實施例1~3相同之程度，但相對密度變低。結果電弧之產生仍較多。
於本說明書中，「或」及「或者」之記載包含僅滿足選項中之任一項之情形、或滿足所有選項之情形。例如，於記載為「A或B」、「A或者B」之情形時，意味著包含滿足A且不滿足B之情形、滿足B且不滿足A之情形、及滿足A且滿足B之情形中之任一者。
以上，對本發明之具體實施形態進行了說明。上述實施形態僅為 本發明之具體例，本發明並不限定於上述實施形態。例如，上述實施形態中之一實施形態所揭示之技術特徵可應用於其他實施形態。又，特定之方法中，可將一部分之步驟與其他步驟之順序調換，亦可於特定之2個步驟之間進而追加步驟。本發明之範圍係由發明專利申請範圍界定。

Claims (3)

  1. 一種IGZO濺鍍靶，其含有In、Ga、Zn、O，其特徵在於：以原子比計為0.30≦In/(In+Ga+Zn)≦0.36、0.30≦Ga/(In+Ga+Zn)≦0.36、0.30≦Zn/(In+Ga+Zn)≦0.36，相對密度為96%以上，濺鍍靶表面之晶粒之平均粒徑為30.0μm以下，且濺鍍靶表面之粒徑之差異為20%以下(1.0≦Dmax/Dmin≦1.2)。
  2. 如申請專利範圍第1項之IGZO濺鍍靶，其中，抗彎強度為40~100MPa，且抗彎強度之差異為20%以下(1.0≦Smax/Smin≦1.2)。
  3. 一種IGZO濺鍍靶之製造方法，上述方法包含如下步驟：於1300~1500℃對具有申請專利範圍第1或2項之元素之組成的成形體進行5~24小時的燒結；及對燒結體進行研削；上述進行燒結之步驟包含：將成形體於800℃~1000℃保持0.5~3小時；上述燒結後之燒結體之翹曲量為2.0mm以下，上述進行研削之步驟包含：於翹曲消除後，進而追加研削0.5mm以上。
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