TWI422699B - IZO sputtering target manufacturing method - Google Patents
IZO sputtering target manufacturing method Download PDFInfo
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- TWI422699B TWI422699B TW095123888A TW95123888A TWI422699B TW I422699 B TWI422699 B TW I422699B TW 095123888 A TW095123888 A TW 095123888A TW 95123888 A TW95123888 A TW 95123888A TW I422699 B TWI422699 B TW I422699B
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Description
本發明係關於一種氧化銦以及氧化鋅或這些粉末為主成分之IZO濺鍍靶之製造方法。
近年,顯示裝置顯著的發展,液晶顯示裝置、電激發光顯示裝置、場效發射顯示器等被開發用於個人電腦、文字處理器等的辦公室機器、工廠的控制系統等。於是,這些顯示裝置,任一種皆具有以透明導電膜夾著顯示元件的三明治構造。
作為這些顯示裝置所使用的透明導電膜,以銦錫氧化物(以下簡稱為ITO膜)膜為主流。此係ITO膜除具有優異的透明性、導電性外,可藉由強酸進行蝕刻加工,又與基板的密合性優異。於是,該ITO膜,可藉由一般濺鍍法、離子鍍法、蒸鍍法而製膜。
但是,雖然關於上述的性質ITO具有優異的性能,因其為結晶性金屬氧化物,使用ITO的濺鍍靶藉由濺鍍法等製膜時,進行ITO的結晶化,若其結晶成長,於透明導電膜的表面生成結晶粒,產生所謂膜的表面精度降低的問題。
再者,由該ITO具有結晶性,蝕刻加工時,從透明導電膜的結晶粒的界面部位被蝕刻。如此狀況下,於透明導電膜的蝕刻部位,該結晶粒子取出殘留,成為顯示元件的情況下,變成導通造成不良顯示的原因。
所以,藉由ITO以外的組合,例如提案氧化鋅與氧化錫為主原料者、於氧化錫添加銻者、於氧化鋅添加鋁者、或氧化銦與氧化鋅為主成分之IZO等(例如參照專利文獻1、專利文獻2)。其中,氧化銦與氧化鋅為主成分之IZO,與ITO比較,由於具有蝕刻速度大的特徵,備受矚目。
一般ITO的濺鍍靶,係氧化銦與氧化鋅的粉末經由所謂混合、粉碎、乾燥、煅燒、粉碎、造粒、成型、燒結的許多步驟所製造得到(例如參照專利文獻3)。關於如此多的步驟之濺鍍靶的製造,係導致生產性低、成本增加的重要因素,減少步驟等的改善,並沒有被充分地檢討。即使於IZO濺鍍靶的製造,承襲上述傳統的製造步驟,現狀在減少步驟等的製造面上並沒有改善,所以期望提高生產性以及降低製造成本。
專利文獻1:日本公開專利特開平8-171824號公報專利文獻2:日本公開專利特開2000-256059號公報專利文獻3:國際公開第WO2003/14409號
本發明係於如此的狀況下,係以提供於IZO濺鍍靶的製造時繼續維持IZO濺鍍靶的特性,且藉由減少步驟而可提高生產性以及降低製造成本之製造方法為目的。而且,提供藉由降低燒結溫度而可提高生產性以及降低製造成本之製造方法為目的。
本發明人等為達成上述目的,反覆專心研究的結果,發現使用具有特定性狀之氧化銦粉末以及氧化鋅粉末或這些粉末為主成分之原料粉末,可繼續維持IZO濺鍍靶的特性,且可減少步驟。本發明係基於上述的見解而完成。
亦即,本發明係提供(1)IZO濺鍍靶之製造方法,其特徵為包含將氧化銦粉末以及氧化鋅粉末或這些粉末為主成分之原料粉末進行混合粉碎得到微粉末之混合粉碎步驟;成型該微粉末而得到成型物之成型步驟;以及,將該成形物在氧氣環境中1250~1450℃下或將該成型物在加壓下氧氣環境中1100~1250℃進行燒結而得到燒結體之燒結步驟;其中該氧化銦粉末的比表面積為8~10m2
/g,該氧化鋅粉末的比表面積為10m2
/g以上;(2)IZO濺鍍靶之製造方法,其特徵為包含,將氧化銦粉末以及氧化鋅粉末或這些粉末為主成分之原料粉末進行混合粉碎得到微粉末之混合粉碎步驟;成型該微粉末而得到成型物之成型步驟;以及,將該成型物在氧氣環境中1250~1450℃下或將該成型物在加壓下氧氣環境中1100~1250℃進行燒結而得到燒結體之燒結步驟;其中該氧化銦粉末的粒度分佈的直徑中位數為1~2μm,該氧化鋅粉末的粒度分佈的直徑中位數為65nm~0.2μm,該混合粉碎步驟後的直徑平均中位數為0.5~1μm;(3)如上述(1)或(2)記載之IZO濺鍍靶之製造方法,其中該成型步驟前,不進行煅燒;(4)如上述(1)~(3)中任一項記載之IZO濺鍍靶之製造方法,其中該燒結體的密度為6.5g/cm3
以上。
根據本發明,可提供於IZO濺鍍靶的製造時繼續維持IZO濺鍍靶的特性,且藉由減少步驟而可提高生產性以及降低製造成本之製造方法。而且,可提供藉由降低燒結溫度而可提高生產性以及降低製造成本之製造方法。
本發明係使用具有特定性狀之氧化銦粉末以及氧化鋅粉末或這些粉末為主成分之原料粉末而可減少製造步驟者。
本發明使用作為原料之氧化銦粉末以及氧化鋅粉末的比表面積,為減少所謂濺鍍靶表面的白點(白色斑點不均)之缺陷的發生,必須分別為8~10m2
/g以及10m2
/g以上。
而且,本發明使用作為原料之氧化銦粉末以及氧化鋅粉末的粒度分佈的直徑中位數,為減少白點的發生,必須分別為1~2μm以及65nm~0.2μm。混合粉碎步驟後的微粉末的直徑平均中位數,雖然越細越好,粉碎為0.5~1μm。只要於該範圍內,可得高密度的IZO濺鍍靶,可減少粉碎時從粉碎機等的不純物的混入量。而且,成為上述原料的粉末,滿足上述比表面積以及直徑中位數兩者較理想。
上述氧化銦粉未以及氧化鋅粉末的使用量,以重量比75:25~95:5較理想,80:20~94:6更理想。
關於本發明的製造之IZO濺鍍靶的原料,只限於氧化銦粉末以及氧化鋅粉末為主成分,以提高該濺鍍靶的特性的目的,也可添加其他成分。例如為降低IZO濺鍍靶的體電阻值,可添加100~2000ppm程度的錫、鋯、鈦、鉿、鍺、鈰等的正4價的元素。
IZO濺鍍靶可由如下述的方式製造。將氧化銦粉末以及氧化鋅粉末或這些粉末為主成分之混合物進行濕式粉碎之微粉末,使用噴霧乾燥機等,將乾燥的粒子進行擠壓成型、燒結後,其成型物的燒結體進行切削加工而可製得。
所謂混合粉碎步驟,係將氧化銦粉末以及氧化鋅粉末或這些粉末為主成分之原料粉末,使用例如濕式球磨機、珠磨機、超音波等之濕式混合粉碎機,均勻混合.粉碎,得到微粉末的步驟。粉碎的微粉末的粒徑,根據如上述IZO濺鍍靶的密度以及減少粉碎時的從粉碎機等的不純物的混入量的觀點而調整。
然後,將所得的微粉末乾燥。於微粉末的乾燥,可使用噴霧乾燥機、一般粉末用乾燥機等。
乾燥的微粉末,經過填充於鑄模,使用一般的冷壓機等,擠壓成型為所期望的形狀之成型步驟。擠壓成型可使用一軸擠壓、常溫靜水壓(CIP)等。
擠壓成型所得的成型物,經過燒結步驟,成為IZO濺鍍靶用燒結體。燒結係於氧氣環境下進行。所謂氧氣環境,係指氧氣濃度21%~未達50%,較理想為21%~未達40%。只要於該範圍內,可有效率地進行燒結,不燒毀燒成爐。而且,也可於空氣環境下進行燒結。而且,燒結也可在大氣壓下進行,在提高燒結密度、不提高含有燒結爐之燒結裝置的價格的目的下,可在加壓、超過大氣壓~0.5MPa下進行。
在大氣壓下進行燒結的情況,燒結溫度為1250~1400℃,較理想為1300~1400℃,只要於該範圍內,燒結密度變高,可降低製造成本。為提高燒結密度、降低製造成本,燒結時間為2~48小時,較理想為4~36小時,燒結時較理想的升溫速度為2~24℃/分。
而且,在加壓下進行燒結的情況,燒結溫度為1100~1250℃,較理想為1150~1250℃,可以在比大氣壓下進行燒結的情況下低的溫度進行燒結,只要於該範圍內,燒結密度變高,可降低製造成本。為提高燒結密度、降低製造成本,燒結時間為2~48小時,較理想為10~36小時,燒結時較理想的升溫速度為2~24℃/分。
從所得的成型物的燒結體製作濺鍍靶時,切削加工該燒結體成為適合設置於濺鍍裝置的形狀,可將其製成裝設用治具的配件。此時,為提高該濺鍍靶的平均表面粗糙度,可進行鏡面加工。於該鏡面加工,可使用化學研磨、機械研磨、化學機械研磨等一般的研磨方法。
如此藉由使用具有特定性狀之氧化銦粉末以及氧化鋅粉末或這些粉末為主成分之原料粉未,不進行一般擠壓成型之成型步驟前之煅燒步驟,於大氣壓下可得具有6.9g/cm3
以上的高密度之IZO濺鍍靶用燒結體。而且,於加壓下可得具有6.5g/cm3
以上的高密度之IZO濺鍍靶用燒結體。將所得的燒結體切削加工而製造的IZO濺鍍靶,具有高密度且於該濺鍍靶表面不存在所謂白點(白色斑點不均)缺陷之優異的特性。本發明的製造方法,可繼續維持IZO濺鍍靶的特性,且藉由減少步驟而可提高生產性以及降低製造成本。
由本發明的製造方法所得的IZO濺鍍靶,因具有上述特性,以濺鍍法製膜時可抑制濺鍍靶表面產生所謂小塊(nodule)之黑色析出物(突起物)。所以,因為不導致製膜速度降低、不引起異常放電時飛散的小塊之朝透明導電膜的異物混入,可安定地進行濺鍍,而且可得膜的特性優異之透明導電膜。
以下藉由實施例以及比較例,更詳細說明本發明,但本發明不限於這些實施例。
實施例1將比表面積9m2
/g的氧化銦粉末90重量份以及比表面積12m2
/g的氧化鋅粉末10重量份,使用濕式珠磨機,混合粉碎24小時。使用1mm Φ的氧化鋯珠作為媒體。混合粉碎後,以噴霧乾燥機乾燥所得的微粉未,填入鑄模,使用冷壓以及常溫等向壓擠壓,以1t/cm2
進行擠壓成型。所得的成型物,裝入燒成爐,在氧氣濃度25%的氧氣環境中1350℃下燒結4小時。雖然無煅燒步驟,所得的IZO濺鍍靶用燒結體為6.92g/cm3
高密度的燒結體。
實施例2直徑中位數1.5μm的氧化銦粉末90重量份以及直徑中位數0.1μm的氧化鋅粉末10重量份,使用濕式珠磨機,混合粉碎24小時,粉碎後的直徑中位數為0.8μm。使用1mm Φ的氧化鋯珠作為媒體。混合粉碎後,以噴霧乾燥機乾燥所得的微粉末,填入鑄模,使用冷壓以及常溫等向壓擠壓,以1t/cm2
進行擠壓成型。所得的成型物,裝入燒成爐,在氧氣濃度30%的氧氣環境中1280℃下燒結4小時。雖然無煅燒步驟,所得的IZO濺鍍靶用燒結體為6.91g/cm3
高密度的燒結體。
實施例3將比表面積9m2
/g的氧化銦粉末90重量份以及比表面積12m2
/g的氧化鋅粉末10重量份,使用濕式珠磨機,混合粉碎24小時。使用1mm Φ的氧化鋯珠作為媒體。混合粉碎後,以噴霧乾燥機乾燥所得的微粉末,填入鑄模,使用冷壓以及常溫等向壓擠壓,以1t/cm2
進行擠壓成型。所得的成型物,裝入燒成爐,於0.15MPa加壓下,氧氣濃度25%的氧氣環境中1230℃下燒結24小時。雖然無煅燒步驟,所得的IZO濺鍍靶用燒結體為6.72g/cm3
高密度的燒結體。
實施例4直徑中位數1.5μm的氧化銦粉末90重量份以及直徑中位數0.1μm的氧化鋅粉末10重量份,使用濕式珠磨機,混合粉碎24小時,粉碎後的直徑中位數為0.8μm。使用1mm Φ的氧化鋯珠作為媒體。混合粉碎後,以噴霧乾燥機乾燥所得的微粉末,填入鑄模,使用冷壓以及常溫等向壓擠壓,以1t/cm2
進行擠壓成型。所得的成型物,裝入燒成爐,於0.12MPa加壓下,氧氣濃度30%的氧氣環境中1180℃下燒結24小時。雖然無煅燒步驟,所得的IZO濺鍍靶用燒結體為6.65g/cm3
高密度的燒結體。
比較例1將比表面積9m2
/g的氧化銦粉末90重量份以及比表面積3m2
/g的氧化鋅粉末10重量份,使用濕式珠磨機,混合粉碎24小時。使用1mm Φ的氧化鋯珠作為媒體。混合粉碎後,以噴霧乾燥機乾燥所得的微粉末,填入鑄模,使用冷壓以及常溫等向壓擠壓,以1t/cm2
進行擠壓成型。所得的成型物,裝入燒成爐,在氧氣濃度25%的氧氣環境中1400℃下燒結4小時。所得的IZO濺鍍靶用燒結體的密度為低如6.10g/cm3
者。
比較例2直徑中位數1.5μm的氧化銦粉末90重量份以及直徑中位數1.0μm的氧化鋅粉末10重量份,使用濕式珠磨機,混合粉碎24小時,粉碎後的直徑中位數為1.2μm。使用1mm Φ的氧化鋯珠作為媒體。混合粉碎後,以噴霧乾燥機乾燥所得的微粉末,填入鑄模,使用冷壓以及常溫等向壓擠壓,以1t/cm2
進行擠壓成型。所得的成型物,裝入燒成爐,在氧氣濃度25%的氧氣環境中1400℃下燒結10小時。所得的IZO濺鍍靶用燒結體的密度為低如6.00g/cm3
者。
比較例3於比較例1以及比較例2,混合粉碎後且擠壓成型前,於空氣環境中於1200℃進行2小時的煅燒,所得的煅燒粉末使用濕式珠磨機粉碎以外,與比較例1以及比較例2同樣地得到IZO濺鍍靶用燒結體。所得的燒結體的密度,與比較例1以及比較例2比較,分別變高成為6.73 g/cm3
、6.73 g/cm3
。上述密度的上升雖藉由進行煅燒,除不及實施例1以及實施例2的密度外,因其增加煅燒步驟以及粉碎步驟,生產性降低。
比較例4將比表面積9m2
/g的氧化銦粉末90重量份以及比表面積3m2
/g的氧化鋅粉末10重量份,使用濕式珠磨機,混合粉碎24小時。使用1mm Φ的氧化鋯珠作為媒體。混合粉碎後,以噴霧乾燥機乾燥所得的微粉末,填入鑄模,使用冷壓以及常溫等向壓擠壓,以1t/cm2
進行擠壓成型。所得的成型物,裝入燒成爐,在空氣環境中1400℃、大氣壓下燒結24小時。所得的IZO濺鍍靶用燒結體的密度為低如6.10g/cm3
者。
比較例5直徑中位數1.5μm的氧化銦粉末90重量份以及直徑中位數1.0μm的氧化鋅粉末10重量份,使用濕式珠磨機,混合粉碎24小時,粉碎後的直徑中位數為1.2μm。使用1mm Φ的氧化鋯珠作為媒體。混合粉碎後,以噴霧乾燥機乾燥所得的微粉末,填入鑄模,使用冷壓以及常溫等向壓擠壓,以1t/cm2
進行擠壓成型。所得的成型物,裝入燒成爐,在空氣環境中1200℃、大氣壓下燒結24小時。所得的IZO濺鍍靶用燒結體的密度為低如6.00g/cm3
者。
比較例6於比較例4以及比較例5,混合粉碎後且擠壓成型前,於空氣環境中於1200℃進行2小時的煅燒,所得的煅燒粉末使用濕式珠磨機粉碎以外,與比較例1以及比較例2同樣地得到IZO濺鍍靶用燒結體。所得的燒結體的密度,與比較例4以及比較例5比較,分別變高成為6.73 g/cm3
、6.73 g/cm3
。上述密度的上升雖藉由進行煅燒,可得比實施例3以及實施例4的高密度燒結體,但增加煅燒步驟以及粉碎步驟,使生產性降低。
本發明的IZO濺鍍靶的製造,可繼續維持IZO濺鍍靶的特性,且藉由減少步驟而可提高生產性以及降低製造成本。而且,可藉由降低燒結溫度而提高生產性以及降低製造成本。
Claims (4)
- 一種IZO濺鍍靶之製造方法,其特徵為:包含混合粉碎步驟,將氧化銦粉末以及氧化鋅粉末或這些粉末為主成分之原料粉末進行混合粉碎得到微粉末;成型步驟,成型該微粉末而得到成型物;以及,燒結步驟,將該成型物在氧氣環境中1250~1450℃下或將該成型物在加壓下氧氣環境中1100~1250℃進行燒結而得到燒結體;其中該氧化銦粉末的比表面積為8~10m2 /g,該氧化鋅粉末的比表面積為10m2 /g以上。
- 一種IZO濺鍍靶之製造方法,其特徵為:包含混合粉碎步驟,將氧化銦粉末以及氧化鋅粉末或這些粉末為主成分之原料粉末進行混合粉碎得到微粉末;成型步驟,成型該微粉末而得到成型物;以及,燒結步驟,將該成型物在氧氣環境中1250~1450℃下或將該成型物在加壓下氧氣環境中1100~1250℃進行燒結而得到燒結體;其中該氧化銦粉末的粒度分佈的直徑中位數為1~2μm,該氧化鋅粉末的粒度分佈的直徑中位數為65nm~0.2μm,該混合粉碎步驟後的直徑平均中位數為0.5~1μm。
- 如申請專利範圍第1項或第2項之IZO濺鍍靶之製造方法,其中該成型步驟前,不進行煅燒。
- 如申請專利範圍第3項之IZO濺鍍靶之製造方法,其中該燒結體的密度為6.5g/cm3 以上。
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