TW201708116A - 氧化物半導體膜及其製備方法 - Google Patents

氧化物半導體膜及其製備方法 Download PDF

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TW201708116A
TW201708116A TW104115812A TW104115812A TW201708116A TW 201708116 A TW201708116 A TW 201708116A TW 104115812 A TW104115812 A TW 104115812A TW 104115812 A TW104115812 A TW 104115812A TW 201708116 A TW201708116 A TW 201708116A
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oxide semiconductor
semiconductor film
sputtering
film according
oxide
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TW104115812A
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TWI593630B (zh
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庄大明
趙明
曹明杰
郭力
高澤棟
魏要偉
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鴻海精密工業股份有限公司
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Abstract

本發明涉及一種氧化物半導體膜，含有銦元素(In)、鈰元素(Ce)、鋅元素(Zn)及氧元素(O)，該In:Ce:Zn的摩爾比為2:(0.5~2):1，氧化物半導體膜為n型半導體，載流子濃度為1012 cm-3 ~1020 cm-3 ，載流子遷移率為5.0 cm2 V-1 s-1 ~45.0 cm2 V-1 s-1 。本發明還涉及一種氧化物半導體膜的製備方法。

Description

氧化物半導體膜及其製備方法
本發明涉及一種氧化物半導體膜及其製備方法。
隨著資訊技術的飛速發展，平板顯示技術正向著更高解析度、更快回應速度、更低能耗、全透明器件以及柔性顯示等目標發展，這也對有源驅動顯示（如AMLCD，Active Matrix Liquid Crystal Display）中TFT（thin film transistor）器件的性能提出更高要求。傳統的非晶矽TFT由於其遷移率較低（~ 0.5cm2 V-1 s-1 ）的特性不能滿足高解析度、大尺寸LCD的顯示要求，更限制其在AMOLED（Active Matrix Organic Light Emitting Diode）顯示中的應用。而低溫多晶矽TFT雖然遷移率較高，但是其生產成本過高，大面積均勻性較難保證，不適合應用於大面積、高分辨顯示器。相較於非晶矽TFT和低溫多晶矽TFT，基於非晶氧化物半導體InGaZnO4 的薄膜電晶體（IGZO-TFT）以其透過率高、製備溫度低、工藝相容性好等諸多優點，能夠替代非晶矽TFT，並且有望用於透明顯示以及OLED顯示。
然而，IGZO-TFT器件遷移率在非晶矽TFT和低溫多晶矽TFT之間，若能進一步提高IGZO-TFT的器件遷移率，其優勢將更明顯。研究發現，二元氧化物氧化銦鋅（IZO）的遷移率遠大於三元氧化物IGZO，但由於其載流子濃度過高，且在使用中易受光照及柵壓等影響導致性能參數發生變化，即穩定性差，因此不適合製備TFT器件。
有鑒於此提供一遷移率較高且穩定性較好的氧化物半導體膜及其製備方法實為必要。
一種氧化物半導體膜，含有銦元素(In)、鈰元素(Ce)、鋅元素(Zn)及氧元素(O)，該In:Ce:Zn的摩爾比為2:(0.5~2):1，氧化物半導體膜為n型半導體，載流子濃度為1012 cm-3 ~1020 cm-3 ，載流子遷移率為5.0 cm2 V-1 s-1 ~45.0 cm2 V-1 s-1 。
相較於先前技術，三元氧化物ICZO中鈰（Ce）元素的加入不僅能降低載流子濃度，同時還能保證高遷移率，從而具有較好的半導體性能，適合用於製備薄膜電晶體，用於平板顯示器或其他電子設備中。另外，由於In、Ce及Zn均可在室溫進行濺射，該濺射形成半導體膜的過程可以在室溫進行，從而簡化了生產工藝。
圖1為本發明實施例薄膜電晶體的結構示意圖。
圖2為本發明實施例2-1氧化物半導體薄膜的XRD圖譜。
圖3為本發明實施例2-1氧化物半導體薄膜的電學性能隨濺射氧氣流量的變化資料圖。
圖4為本發明實施例2-1氧化物半導體薄膜的掃描電鏡照片。
圖5為本發明實施例2-2氧化物半導體薄膜的電學性能隨濺射氧氣流量的變化資料圖。
圖6為本發明實施例2-2氧化物半導體薄膜的掃描電鏡照片。
圖7為本發明實施例2-3氧化物半導體薄膜的電學性能隨濺射氧氣流量的變化資料圖。
圖8為本發明實施例2-3氧化物半導體薄膜的掃描電鏡照片。
下面將結合附圖及具體實施例對本發明提供的氧化物半導體膜及其製備方法作進一步的詳細說明。
本發明實施例提供一種濺射靶，由氧化銦(In2 O3 )、氧化鈰(CeO2 )及氧化鋅(ZnO)混合後燒結形成，該濺射靶中含有化合物In2 Cex ZnO4+2x ，其中x=0.5~2。
優選地，該化合物In2 Cex ZnO4+2x 為晶態。該濺射靶中可以含有非晶態的In、Ce及Zn的氧化物，優選地，晶態In2 Cex ZnO4+2x 在該濺射靶中的含量為80%以上。
在一實施例中，該濺射靶僅含有由In2 O3 、CeO2 及ZnO氧化物混合後燒結形成的物質及微量雜質，該雜質的含量優選為小於10ppm。
在另一實施例中，該濺射靶僅含有晶態In2 Cex ZnO4+2x 及微量雜質，該雜質的含量優選為小於10ppm。
在一實施例中，該濺射靶由In2 O3 、CeO2 及ZnO混合後燒結形成的燒結物經過機械加工成型得到。
該濺射靶的相對密度優選大於或等於90%，該相對密度=濺射靶實際密度:In2 Cex ZnO4+2x 理論密度×100%。
該濺射靶的體電阻優選為10-2 Ωcm ~10Ωcm。
該濺射靶表面的粗糙度優選小於或等於2微米，更優選為小於或等於0.5微米。
該濺射靶的平均抗彎強度優選為大於或等於50MPa，更優選為大於或等於55MPa。
本發明實施例提供一種濺射靶的製備方法，包括：
將In2 O3 粉末、CeO2 粉末及ZnO粉末均勻混合形成一混合體，該混合體中In:Ce:Zn的摩爾比為2:(0.5~2):1；以及
將該混合體在1250°C~1650°C進行燒結。
在該混合體中，該In2 O3 粉末、CeO2 粉末及ZnO粉末的粒徑優選為小於或等於10微米，更優選為0.5微米~2微米。
該In2 O3 粉末、CeO2 粉末及ZnO粉末的純度優選為3N(質量百分比99.9%)~5N(質量百分比99.999%)。
該In2 O3 粉末、CeO2 粉末及ZnO粉末摩爾比例為In2 O3 : CeO2 : ZnO =2: (1 ~4): 2。
該In2 O3 粉末、CeO2 粉末及ZnO粉末可以在空氣或保護氣體（如Ar氣或N2 氣）中進行混合，該混合步驟可進一步包括：
將該In2 O3 粉末、CeO2 粉末及ZnO粉末在液態介質中進行球磨；及
將球磨後的混合物烘乾去除該液態介質。
該液態介質為不與原料In2 O3 粉末、CeO2 粉末及ZnO粉末發生反應，且通過之後的烘乾步驟可以去除，不向混合物中引入其他雜質。該液態介質例如可以是水、乙醇及丙酮中的至少一種。
該球磨是在球磨機中進行，該液態介質與該原料In2 O3 粉末、CeO2 粉末及ZnO粉末置入該球磨機中。該球磨機的轉速優選為100 rpm~600rpm。在球磨的過程中，一方面可以將該In2 O3 粉末、CeO2 粉末及ZnO粉末充分混合均勻，另一方面可以將粉末的粒徑細化，得到所需粒徑的原料粉末。該球磨時間以混合均勻並且原料粒度達到要求為準。
該烘乾的溫度優選為30°C~60°C，該烘乾步驟可以在空氣或保護氣體（如Ar氣或N2 氣）中進行，優選為在高純(3N~5N)保護氣體中進行烘乾。
該燒結的步驟可以是將該混合體進行熱壓燒結（非等靜壓）、常壓燒結或熱等靜壓燒結。該熱壓燒結的壓力可以為30MPa~100MPa，燒結時間可以為1小時~24小時。該熱等靜壓燒結的壓力可以為100MPa~300MPa，燒結時間可以為1小時~40小時。該常壓燒結的燒結時間可以為1小時~40小時。
該燒結過程在保護氣體中進行，該保護氣體可以為Ar氣或N2 氣，優選為純度為3N~5N的Ar氣或N2 氣。
當燒結過程中同時施加壓力時，該混合體可以在燒結過程中成型，以形成預定形狀的濺射靶，適於後續濺射使用。具體可以是將該燒結體放入具有預定形狀的模具中進行熱壓燒結或等靜壓燒結。
當該燒結為常壓燒結時，該混合體可以在燒結前先進行成型，以形成預定形狀的濺射靶，適於後續濺射使用。具體可以是將該燒結體放入具有預定形狀的模具中進行壓制。該壓制所用的壓力可以為30MPa~300MPa。
另外，當採用任何燒結方式進行燒結前，均可對混合體進行預成型步驟，例如可以採用模具、澆鑄或注射等方式使混合體預成型，在預成型過程中可以在混合體中加入粘結劑和/或溶劑。該粘結劑和/或溶劑在後續的燒結步驟中可以被完全去除。
在燒結後得到具有預定形狀的燒結體後可以直接作為該濺射靶使用，也可以進一步進行加工成型、打磨等步驟。
在燒結過程中，原料In2 O3 粉末、CeO2 粉末及ZnO粉末反應生成晶態In2 Cex ZnO4+2x 。
本發明實施例進一步提供一種氧化物半導體膜，包括體銦元素(In)、鈰元素(Ce)、鋅元素(Zn)及氧元素(O)，該In:Ce:Zn的摩爾比為2:(0.5~2):1，氧化物半導體膜為n型半導體，載流子濃度為1012 cm-3 ~1020 cm-3 ，載流子遷移率為5.0 cm2 V-1 s-1 ~45.0 cm2 V-1 s-1 。
該氧化物半導體膜優選為非晶質氧化物。在另一實施例中，該氧化物半導體膜中也可含有晶態In2 Cex ZnO4+2x 。
在一實施例中，該氧化物半導體膜除該In、Ce、Zn及O元素外，僅含有微量雜質，該雜質的含量優選為小於10ppm。
該氧化物半導體膜的禁帶寬度優選為3.0 eV ~3.5 eV。
該氧化物半導體膜的可見光透過率優選為60%~90%。
該氧化物半導體膜的厚度優選為50nm~1000nm。
該氧化物半導體膜的載流子濃度優選為1013 cm-3 ~1015 cm-3 。
該氧化物半導體膜的載流子遷移率優選為12.3 cm2 V-1 s-1 ~45.0 cm2 V-1 s-1 。
該氧化物半導體膜可以通過使用上述濺射靶，通過濺射法獲得。
本發明實施例進一步提供一種氧化物半導體膜的製備方法，包括使用上述濺射靶，通過濺射法在基底上濺射形成氧化物膜。
該濺射法可以為磁控濺射法，例如直流濺射法或交流濺射法（如中頻磁控濺射法或射頻磁控濺射法），優選為中頻磁控濺射法或射頻磁控濺射法。該濺射的電流優選為0.1A~2.0A。該濺射的時間優選為1分鐘~120分鐘。
該濺射的溫度可以為常溫或高溫，優選小於或等於400°C。當採用高溫時，該製備方法可進一步包括在濺射前將該基底在真空中預熱的步驟，該預熱溫度例如可以為50°C~400°C。
該濺射法中使用的載氣可以為稀有氣體、稀有氣體與氧氣的混合氣或稀有氣體與氫氣的混合氣，該稀有氣體優選為Ar氣。該載氣優選為Ar氣與氧氣的混合氣。該氧氣的流量優選小於3sccm。載氣中各氣體的純度優選為3N~5N。
該濺射時濺射室內的壓力優選為0.1Pa~2.0Pa。
該基板的材料為絕緣材料且能夠耐受該氧化物半導體膜製備過程中的加熱溫度。當該氧化物半導體膜製備過程所用溫度較低，如採用常溫濺射，該基板的材料選擇範圍較寬。該基板的材料可以列舉為玻璃、矽或聚合物（如PI、PE、PET等）。
在進行濺射前，該製備方法可進一步包括對基底進行清潔的步驟，以去除基底表面的雜質。
在進行濺射前，該基底材料可以安裝在夾具上進行固定，該基底與該濺射靶可以相互平行，也可以呈一夾角，該夾角可以為20º~85º之間。該基底與該濺射靶之間的距離優選小於或等於8cm。
在進行濺射在該基底上形成氧化物膜後，該氧化物膜可直接作為氧化物半導體膜。在另一實施例中，該製備方法還可進一步包括將該氧化物膜退火的步驟。具體地，是在真空、氮氣或保護氣體（如Ar氣）中進行退火。該退火過程的本底真空優選為10-3 Pa~10Pa。該退火溫度優選為100°C~400°C，升溫速率優選為1°C/min~20°C/min，退火時間優選為1小時~10小時。該退火過程可在一定程度上提高該氧化物膜的結晶度，從而對氧化物半導體膜產品的性能進行調整。
本發明實施例提供的氧化物半導體膜及其製備方法中，採用原位摻雜Ce的氧化銦鋅得到In2 Cex ZnO4+2x 濺射靶，其中x=0.5~2。利用該濺射靶濺射得到n型氧化物半導體膜，In:Ce:Zn的摩爾比例為2:(0.5~2):1。該n型氧化物半導體膜的載流子霍爾遷移率在5.0 cm2 V-1 s-1 ~45.0 cm2 V-1 s-1 ，載流子濃度在1012 cm-3 ~1020 cm-3 ，可以用於製備n型薄膜電晶體，用於平板顯示器或其他電子設備中。該Ce元素在該氧化物半導體膜中的含量不能太小或太大，當x<0.5，半導體氧化物膜的性質偏向IZO，容易導致膜的穩定性降低，應用到半導體元件在使用中易受光照及柵壓等影響使該半導體氧化物膜的參數發生變化；當x>2時，該半導體氧化物膜的遷移率下降，影響半導體元件性能。
本發明實施例還提供一種半導體元件，該半導體元件包括所述氧化物半導體膜。
請參閱圖1，本發明實施例還提供一種薄膜電晶體10，該薄膜電晶體包括絕緣基底110、半導體層140、源極151、漏極152、柵極120及絕緣層130。該源極151與漏極152間隔設置，該半導體層140與該源極151和漏極152電連接，該柵極120通過該絕緣層130與該半導體層140、源極151及漏極152絕緣設置。該半導體層140為所述氧化物半導體膜。該薄膜電晶體10中除該氧化物半導體膜外的其他元件可根據先前技術設置及製備。圖1中的薄膜電晶體10為一頂柵結構，可以理解，該薄膜電晶體10也可以為底柵結構或其他薄膜電晶體結構。
實施例1：濺射靶及其製備方法
實施例1-1
稱量純度為4N的209g In2 O3 粉末、260g CeO2 粉末和61g ZnO粉末（三種氧化物摩爾比例為In2 O3 : CeO2 : ZnO =1:2:1），將三種粉末放入球磨罐中混合。球磨介質選為無水乙醇，球磨轉速200 rpm，球磨時間10 h。球磨結束後在壓力為1 atm、純度為5N的Ar氣保護下烘乾1 h。烘乾後將粉末放入熱壓燒結爐中，在高純Ar氣氛圍中進行熱壓燒結，燒結壓力為50 MPa，燒結溫度為1350℃，升溫速率為15 ºC /min，燒結時間為5 h。燒結結束後隨爐冷卻至室溫取樣。靶材相對密度>87%，體電阻0.75Ωcm。將靶材用於中頻交流磁控濺射，起弧容易，濺射穩定。
實施例1-2
稱量純度為4N的249g In2 O3 粉末、231g CeO2 粉末和73g ZnO粉末（三種氧化物摩爾比例為In2 O3 : CeO2 : ZnO =2:3:2），將三種粉末放入球磨罐中混合。球磨介質選為無水乙醇，球磨轉速為400 rpm，球磨時間為20 h。球磨結束後在壓力為1 atm、純度為5N的Ar氣保護下烘乾1 h。採用常壓燒結製備靶材，將粉末放入普通壓機中，壓力為75MPa，保壓時間為60 min。脫模後放入燒結爐，在高純N2 氣氛圍中進行燒結，燒結溫度為1450℃，升溫速率為10 ºC /min，燒結時間為8h。燒結結束後隨爐冷卻至室溫取樣。靶材相對密度>85%，體電阻0.12Ωcm。將靶材用於中頻交流磁控濺射，起弧容易，濺射穩定。
實施例1-3
稱量純度為4N的209g In2 O3 粉末、260g CeO2 粉末和61g ZnO粉末（三種氧化物摩爾比例為In2 O3 : CeO2 : ZnO =1:2:1），放入球磨罐中混合。球磨介質選為無水乙醇，球磨轉速500 rpm，球磨時間為10 h。球磨結束後在壓力為1 atm、純度為5N的N2 氣保護下烘乾1 h。將粉末進行包裹後，放入等靜壓機中，在高純Ar氣氛圍中進行燒結。燒結壓力為100 MPa，燒結溫度為1450℃，升溫速率為10 ºC /min，燒結時間為20 h。燒結結束後隨爐冷卻至室溫取樣。靶材相對密度>86%，體電阻0.62Ωcm。將靶材用於中頻交流磁控濺射，起弧容易，濺射穩定。
實施例2：氧化物半導體膜
實施例2-1
選用市售普通鈉鈣玻璃作為基底，將基底洗淨並用N2 吹幹後置入磁控濺射儀中。基底與靶材表面平行，距離8 cm。靶材為實施例1-1摻鈰氧化銦鋅靶材In2 Cex ZnO4+2x ，三種氧化物摩爾比例為In2 O3 : CeO2 : ZnO =1:2:1。採用40 sccm的Ar和0 ~ 2sccm的O2 作為工作氣體，工作電流為1.0 A，工作氣壓為0.7 Pa，在室溫進行磁控濺射，濺射時間為28 min，制得250 nm厚的ICZO薄膜，經過Hall測試測得該ICZO薄膜霍爾遷移率達14 cm2 V-1 s-1 ~25.6 cm2 V-1 s-1 ，載流子濃度在1013 cm-3 ~1020 cm-3 。請參閱圖2，從XRD譜圖可以看到該ICZO薄膜為無定形結構。請參閱圖3，ICZO薄膜載流子濃度及霍爾遷移率隨濺射使用的O2 流量的變化資料如圖3所示。請參閱圖4，ICZO薄膜掃描電鏡表面形貌如圖4所示。
實施例2-2
選用市售普通鈉鈣玻璃作為襯底，將基片洗淨並用N2 吹幹後置入磁控濺射儀中。基底與靶材表面平行，距離8 cm。靶材為實施例1-2摻鈰氧化銦鋅靶材In2 Cex ZnO4+2x ，製備該靶材所用的三種氧化物摩爾比例為In2 O3 : CeO2 : ZnO =2:3:2，用40 sccm的Ar和0 ~ 3sccm的O2 作為工作氣體，基底預熱溫度為250℃，工作電流為1.0 A，工作氣壓為0.7 Pa，濺射時間為28 min，制得250 nm厚的ICZO薄膜。經過Hall測試測得該ICZO薄膜霍爾遷移率達17.8 cm2 V-1 s-1 ~ 45.0 cm2 V-1 s-1 ，載流子濃度在1015 cm-3 ~1020 cm-3 。請參閱圖5，ICZO薄膜載流子濃度及霍爾遷移率隨濺射使用的O2 流量的變化資料如圖5所示。請參閱圖6，ICZO薄膜掃描電鏡表面形貌如圖6所示。
實施例2-3
選用市售普通鈉鈣玻璃作為基底，將基片洗淨並用N2 吹幹後置入磁控濺射儀中。基底與靶材表面平行，距離8 cm。靶材為實施例1-3摻鈰氧化銦鋅靶材In2 Cex ZnO4+2x ，製備該靶材所用的三種氧化物摩爾比例為In2 O3 : CeO2 : ZnO =1:2:1。採用40 sccm的純Ar作為工作氣體，工作電流為1.0 A，工作氣壓為0.7 Pa，在室溫進行磁控濺射，濺射時間為28 min，制得250 nm厚的ICZO薄膜，經過Hall測試測得該ICZO薄膜霍爾遷移率達15.6 cm2 V-1 s-1 ，載流子濃度為1020 cm-3 。將濺射態薄膜放入石英管式爐內退火，在1 Pa真空下退火1 h，退火溫度為150ºC到350 ºC，可得載流子濃度在1014 cm-3 ~1020 cm-3 ，霍爾遷移率在17.1 cm2 V-1 s-1 ~20.6 cm2 V-1 s-1 之間的ICZO薄膜，適合製備TFT器件。請參閱圖7，ICZO薄膜載流子濃度及霍爾遷移率隨退火溫度的變化資料如圖7所示。請參閱圖8，ICZO薄膜掃描電鏡表面形貌如圖8所示。
綜上所述，本發明確已符合發明專利之要件，遂依法提出專利申請。惟，以上所述者僅為本發明之較佳實施例，自不能以此限制本案之申請專利範圍。舉凡習知本案技藝之人士援依本發明之精神所作之等效修飾或變化，皆應涵蓋於以下申請專利範圍內。
10‧‧‧薄膜電晶體
110‧‧‧絕緣基底
120‧‧‧柵極
130‧‧‧絕緣層
140‧‧‧半導體層
151‧‧‧源極
152‧‧‧漏極
無

Claims (17)

  1. 一種氧化物半導體膜，其改進在於，含有銦元素(In)、鈰元素(Ce)、鋅元素(Zn)及氧元素(O)，該In:Ce:Zn的摩爾比為2:(0.5~2):1，氧化物半導體膜為n型半導體，載流子濃度為1012 cm-3 ~1020 cm-3 ，載流子遷移率為5.0 cm2 V-1 s-1 ~45.0 cm2 V-1 s-1 。
  2. 如請求項1所述的氧化物半導體膜，其中，該氧化物半導體膜的材料為非晶態氧化物。
  3. 如請求項1所述的氧化物半導體膜，其中，該氧化物半導體膜的禁帶寬度為3.0 eV ~3.5 eV。
  4. 如請求項1所述的氧化物半導體膜，其中，該氧化物半導體膜的載流子濃度為1013 cm-3 ~1015 cm-3 。
  5. 如請求項1所述的氧化物半導體膜，其中，該氧化物半導體膜的透過率為60%~90%。
  6. 如請求項1所述的氧化物半導體膜，其中，該氧化物半導體膜的厚度50 nm為1000 nm。
  7. 一種氧化物半導體膜的製備方法，包括使用一濺射靶，通過濺射法在基底上濺射形成氧化物膜的步驟，該濺射靶含有化合物In2 Cex ZnO4+2x ，其中x=0.5~2。
  8. 如請求項7所述的氧化物半導體膜的製備方法，其中，該濺射靶由氧化銦(In2 O3 )、氧化鈰(CeO2 )及氧化鋅(ZnO)混合後燒結形成。
  9. 如請求項7所述的氧化物半導體膜的製備方法，其中，該濺射法為直流濺射法或交流濺射法，該交流濺射法為中頻磁控濺射法或射頻磁控濺射法。
  10. 如請求項7所述的氧化物半導體膜的製備方法，其中，該濺射的溫度為常溫濺射。
  11. 如請求項7所述的氧化物半導體膜的製備方法，其中，進一步包括在濺射前將該基底在真空中預熱的步驟，該預熱溫度為50°C~400°C。
  12. 如請求項7所述的氧化物半導體膜的製備方法，其中，該濺射法中使用的載氣為稀有氣體、稀有氣體與氧氣的混合氣或稀有氣體與氫氣的混合氣。
  13. 如請求項7所述的氧化物半導體膜的製備方法，其中，該濺射時濺射室內的壓力為0.1Pa~2.0Pa。
  14. 如請求項7所述的氧化物半導體膜的製備方法，其中，該基板的材料為玻璃、矽或聚合物。
  15. 如請求項7所述的氧化物半導體膜的製備方法，其中，在進行濺射前，進一步包括對基底進行清潔的步驟，以去除基底表面的雜質。
  16. 如請求項7所述的氧化物半導體膜的製備方法，其中，該基底與該濺射靶相互平行或呈一夾角，該夾角為20º~85º之間，該基底與該濺射靶之間的距離小於或等於8cm。
  17. 如請求項7所述的氧化物半導體膜的製備方法，其中，進一步包括將該氧化物膜在真空、氮氣或Ar氣中退火的步驟，該退火溫度為100°C~400°C，升溫速率為1°C/min~20°C/min，退火時間為1小時~10小時。
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