TW201808809A - 氧化鎂濺鍍靶及其製法 - Google Patents
氧化鎂濺鍍靶及其製法 Download PDFInfo
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Abstract
一種用於濺鍍的燒結緻密氧化鎂靶,其具有99.99wt%或更高的純度、3.58g/cm3或更高的密度、以及10%或更高的透明度;一種用於濺鍍的燒結緻密氧化鎂靶,其具有99.99wt%或更高的純度、3.58g/cm3或更高的密度、以及50μm或更大的平均晶體粒度。
Description
本申請案主張於2016年7月13日提申之美國臨時專利申請案序號62/361,562的優先權權益。
本發明係涉及用於形成氧化鎂層的氧化鎂靶,其係用於穿隧磁阻(TMR)元件和其它電子裝置;且係涉及製造此氧化鎂靶的方法。本發明係特別關於一種燒結緻密氧化鎂靶,其用於高純度和高密度之濺鍍、且呈半透明狀;且係關於製造此用於濺鍍之燒結緻密氧化鎂靶的方法。
在藉由熱壓原料粉末來製造氧化鎂燒結緻密濺鍍靶時,存在著這些靶呈白色且含有不均勻密度之問題。通常不會特別注意到這個問題,然而近年來,已變得必須研究並解決這個問題以改善沉積品質。
授予Naguno等人的美國專利案8,454,933揭示了一種可用來作為濺鍍靶的MgO燒結體。靶係產自在單軸壓力下具有1μm或更小的MgO粉末,然而,這些燒結粉末經受了溫度為1273K、在含氧氛圍下的熱處理達1分鐘或更久,且含有較佳為30μm或更小的平均晶體粒度。
授予Misano等人的美國專利公開案2014/0284212 A1揭示了一種用於濺鍍的燒結緻密氧化鎂靶,其具有60%或更低的白度。
授予Okamoto等人的美國專利公開案2014/0318956揭示了一種由氧化鎂燒結體所製成的濺鍍靶,其具有不低於99.99%(質量%)的純度、高於98%的相對密度,以及不大於5-8μm的平均粒度;揭示了一種生產具有不低於99.99%(質量%)的純度、由氧化鎂燒結體所製成的濺鍍靶之方法,其包含在1250至1350℃下進行熱壓燒結以獲得燒結體,且隨後在1250至1400℃下進行退火處理。
授予Takenouchi的日本專利公開案JPH 10158826A揭示了一種具有高純度和密度的MgO濺鍍靶。將以下添加至高純度MgO粉末中並加以混合:10至60wt%的電熔MgO粉末、1至5wt%的MgO細粉(平均粒度100nm)及黏合劑,將此混合物壓實並脫脂,隨後在1250至1350℃下使其經受一次燒結,且接著在1500℃下經受二次燒結;藉由摻合和兩步燒結,可生產高純度和高密度的MgO燒結體;藉由電熔MgO粉末之摻合,可形成結晶度良好的MgO塗層。
近年來,有考慮在穿隧磁阻(TMR)元件和其它電子裝置中使用氧化鎂膜,但需要具有更高純度和更高密度的氧化鎂靶,以均勻地沉積氧化鎂,並使在濺鍍過程中所添加的缺陷最小化。然而,由於對更高度純化和緻密化的期望非常高,故通常難以生產能滿足上述需要的氧化鎂靶。因此,本發明之標的是提供一種能夠實現上述內容的靶,以及一種生產此種靶的方法。
根據本發明的一個態樣,揭示了一種用於濺鍍的燒結緻密氧化鎂靶。燒結緻密氧化鎂靶包含99.99wt%或更高的純度、3.58g/cm3或更高的密度、以及10%或更高的透明度。在一些具體實例中,靶進一步含有純MgO粉末的原料,其中MgO粉末含有小於10-6m的粒徑和小於15 103m2/kg的比表面積;在其它具體實例中,透明性為10%或更高;在其它具體實例中,透明性的變化在1%以內。
在另一例示性具體實例中,揭示了一種用於濺鍍的燒結緻密氧化鎂靶,其包含99.99wt%或更高的純度、3.58g/cm3或更高的密度、以及50μm或更大的平均晶體粒度;在其它此等具體實例中,靶進一步含有純MgO粉末的原料,其中MgO粉末含有小於10-6m的粒徑和小於15 103m2/kg的比表面積;在其它此等具體實例中,透明性為10%或更高;在其它此等具體實例中,透明性的變化在1%以內。
在又一具體實例中,揭示了一種生產用於濺鍍之燒結緻密氧化鎂靶的方法。此方法包含藉由研磨氧化鎂(MgO)來獲得原料,其中原料含有包含氧化鎂(MgO)的粉末,其具有99.99wt%或更高的純度和0.5μm或更小的平均粒度,且在1700℃或更低的溫度、以及至少200kgf/cm2或更高的施加壓力下熱壓經研磨粉末,以獲得燒結緻密氧化鎂靶。
在此等具體實例中,方法進一步包含一種靶,其包含99.99wt%或更高的純度、以及3.58g/cm3或更高的密度;在其它此等具體實例中,方法包含300kgf/cm2或更高的施加壓力。
在本發明的又一具體實例中,揭示了一種生產用於濺鍍之燒結緻密氧化鎂靶的方法。此方法包含藉由研磨氧化鎂(MgO)來獲得原料,
其中原料含有包含氧化鎂(MgO)的粉末,其具有99.99wt%或更高的純度和0.5μm或更小的平均粒度,且在1700℃或更低的溫度、以及至少200kgf/cm2或更高的施加壓力下熱壓經研磨粉末,以獲得燒結緻密氧化鎂靶,其中燒結緻密氧化鎂靶含有99.99wt%或更高的純度、3.58g/cm3或更高的密度、10%或更高的透明度,以及50μm或更大的平均晶體粒度。
本發明提供了一種用於濺鍍之燒結緻密氧化鎂靶,用於濺鍍之燒結緻密氧化鎂靶含有至少99.99wt%或更高的純度;本發明之燒結緻密氧化鎂靶進一步含有3.58g/cm3或更高的密度、以及10%或更高的透明度。
在一些具體實例中,燒結緻密氧化鎂靶含有3.58g/cm3或更高的密度;在其它具體實例中,用於濺鍍之燒結緻密氧化鎂靶含有3.5805g/cm3或更高的密度;在其它具體實例中為至少3.581g/cm3或更高;以及在其它具體實例中為至少3.5815g/cm3或更高。
在一些具體實例中,用於濺鍍之燒結緻密氧化鎂靶含有10%或更高的透明性。亦應將術語「透明性(transparence)」或「透明度(transparency)」理解為意指使光穿透過材料的品質,在一些具體實例中,用於濺鍍之燒結緻密氧化鎂靶含有至少15%或更高的透明性;在一些具體實例中為至少20%或更多的透明性;以及在其它具體實例中為至少30%或更多。
在一些具體實例中,透明性的變化在1%以內;在其它具體
實例中,透明性的變化在.75%以內;以及在其它具體實例中為.50%以內。
在一些具體實例中,用於濺鍍之燒結緻密氧化鎂靶進一步含有純MgO粉末的原料;在一些具體實例中,MgO粉末含有小於10-6m的粒徑和小於15 103m2/kg的比表面積。
在一些具體實例中,本發明展現出具有更高純度和更高密度的氧化鎂靶,與基於原料粉末之選擇和燒結條件之最佳化設定的常見方法相較之下,可用便宜的加工條件來獲得此更高純度和更高密度。
本發明之燒結緻密氧化鎂靶展現出更大的平均晶體粒度。在一些具體實例中,較大的平均晶體粒度導致靶的低顆粒排放,與提供較小平均晶體粒度的那些靶相反,藉由具有更大的平均晶體粒度,則有較少的顆粒固定或暴露於在矽晶圓上。
在一些具體實例中,燒結緻密氧化鎂靶含有50μm或更大的平均晶體粒度;在其它具體實例中,燒結緻密氧化鎂靶含有60μm或更大的平均晶體粒度;在其它具體實例中為70μm或更大的平均晶體粒度;以及在其它些具體實例中為80μm或更大的平均晶體粒度。
本發明進一步提供了一種生產用於濺鍍之燒結緻密氧化鎂靶的方法,方法包含藉由研磨氧化鎂(MgO)來獲得原料,以及熱壓經研磨粉末以獲得燒結緻密氧化鎂靶。
在一些具體實例中,研磨來獲得原料之步驟含有包含以下之氧化鎂:99.99wt%或更高的純度,以及0.5μm或更小的平均粒度。
在一些具體實例中,熱壓經研磨粉末之步驟發生在1700℃或更低的溫度下;在一些具體實例中,熱壓經研磨粉末之步驟發生在
1400-1700℃的溫度之間;在其它具體實例中為1500-1700℃的溫度之間;以及在其它具體實例中為1600-1700℃的溫度之間。
在一些具體實例中,熱壓經研磨粉末之步驟發生在至少200kgf/cm2或更高的施加壓力下;在其它具體實例中,熱壓經研磨粉末之步驟發生在至少300kgf/cm2或更高的施加壓力下。
關於彩色深淺(color shading)的出現,在一些具體實例中,本發明之方法生產了用於濺鍍之燒結緻密氧化鎂靶,其含有均勻地半透明(translucent)氧化物靶。在一些具體實例中,本發明之半透明氧化物靶無彩色深淺,或基本上無彩色深淺;在其它具體實例中,本發明之半透明氧化物靶包含中等的氧缺陷。
在一些具體實例中,本文中所揭示的用於濺鍍之燒結緻密氧化鎂靶和方法並不要求添加添加劑。舉例而言,此等添加劑含有MgCO3或Mg(OH)2;在一些具體實例中,本文中所揭示的用於濺鍍之燒結緻密氧化鎂靶和方法並不要求任何電熔粉末。
在一些具體實例中,本文中所揭示的用於濺鍍之燒結緻密氧化鎂靶和方法並不在熱壓之後要求任何額外燒結步驟。本發明提供良好的顆粒性能,而無額外燒結步驟,從消除額外燒結步驟可理解到的好處為,本發明使得生產成本降低。
在特定具體實例中,提供了一種生產用於濺鍍之燒結緻密氧化鎂靶的方法。此方法包含藉由研磨氧化鎂(MgO)來獲得原料,其中原料含有包含氧化鎂(MgO)的粉末,其具有99.99wt%或更高的純度和0.5μm或更小的平均粒度,且在1700℃或更低的溫度、以及至少200kgf/cm2或更
高的施加壓力下熱壓經研磨粉末,以獲得燒結緻密氧化鎂靶;在此等具體實例中,燒結緻密氧化鎂靶含有99.99wt%或更高的純度、3.58g/cm3或更高的密度、10%或更高的透明度,以及50μm或更大的平均晶體粒度。
以下實施例係經囊括以作為本發明之說明,且不應被解釋為限定本發明之範疇。
在300kgf/cm2的施加壓力、1500℃的溫度熱壓氧化鎂粉末(比表面積8 103m2/kg、平均粒徑0.5 10-6m及純度99.99%),因而將本發明所生產的氧化鎂濺鍍靶燒結為3.581g/cm3的密度、16%的透明度及70μm的粒度;為了進行比較,生產以下氧化鎂濺鍍靶:99.99%的純度、3.576g/cm3的密度、0.8%的中心透明度及15μm的粒度。本發明之燒結體和比較性燒結體皆在相同條件下進行濺鍍,兩者的表現顯示於表1中,我們看到了例示性氧化鎂靶的顆粒表現遠優於比較性靶,希望能在矽晶圓上具有較少顆粒以提高產量。
雖然已利用特定實施例來描述本發明,但所屬技術領域中熟諳此技藝者而言,本發明的許多其它形式和修飾明顯地為顯而易見的,應
將隨附申請專利範圍和本發明解釋為涵蓋所有此等顯而易見之形式和修飾。
Claims (12)
- 一種用於濺鍍之燒結緻密氧化鎂靶,其包含:99.99wt%或更高的純度、3.58g/cm3或更高的密度、以及10%或更高的透明度。
- 根據申請專利範圍第1項的用於濺鍍之燒結緻密氧化鎂靶,其中該用於濺鍍之燒結緻密氧化鎂靶進一步含有純MgO粉末的原料,其中該MgO粉末含有小於10-6m的粒徑和小於15 103m2/kg的比表面積。
- 根據申請專利範圍第1項的用於濺鍍之燒結緻密氧化鎂靶,其中該透明性為10%或更高。
- 根據申請專利範圍第1項的用於濺鍍之燒結緻密氧化鎂靶,其中該透明性的變化在1%以內。
- 一種用於濺鍍之燒結緻密氧化鎂靶,其包含:99.99wt%或更高的純度、3.58g/cm3或更高的密度、以及50μm或更大的平均晶體粒度。
- 根據申請專利範圍第5項的用於濺鍍之燒結緻密氧化鎂靶,其中該燒結緻密氧化鎂靶進一步含有純MgO粉末的原料,其中該MgO粉末含有小於10-6m的粒徑和小於15 103m2/kg的比表面積。
- 根據申請專利範圍第5項或第6項的用於濺鍍之燒結緻密氧化鎂靶,其中該透明性為10%或更高。
- 根據申請專利範圍第5項至第7項中任一項的用於濺鍍之燒結緻密氧 化鎂靶,其中該透明性的變化在1%以內。
- 一種生產用於濺鍍之燒結緻密氧化鎂靶的方法,該方法包含:藉由研磨氧化鎂(MgO)來獲得原料,其中該原料含有包含氧化鎂(MgO)的粉末,其具有99.99wt%或更高的純度和0.5μm或更小的平均粒度;且在1700℃或更低的溫度、以及至少200kgf/cm2或更高的施加壓力下熱壓該經研磨粉末,以獲得燒結緻密氧化鎂靶。
- 根據申請專利範圍第9項的生產燒結緻密氧化鎂靶的方法,其中該燒結緻密氧化鎂靶包含99.99wt%或更高的純度,以及3.58g/cm3或更高的密度。
- 根據申請專利範圍第9項的生產燒結緻密氧化鎂靶的方法,其中該施加壓力為300kgf/cm2或更高。
- 一種生產用於濺鍍之燒結緻密氧化鎂靶的方法,該方法包含:藉由研磨氧化鎂(MgO)來獲得原料,其中該原料含有包含氧化鎂(MgO)的粉末,其具有99.99wt%或更高的純度和0.5μm或更小的平均粒度;且在1700℃或更低的溫度、以及至少200kgf/cm2或更高的施加壓力下熱壓該經研磨粉末,以獲得燒結緻密氧化鎂靶,其中該燒結緻密氧化鎂靶含有:99.99wt%或更高的純度、3.58g/cm3或更高的密度、10%或更高的透明度、以及 50μm或更大的平均晶體粒度。
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CN111465712A (zh) * | 2018-09-13 | 2020-07-28 | 捷客斯金属株式会社 | MgO烧结体溅射靶 |
TWI807114B (zh) * | 2018-10-10 | 2023-07-01 | 日商Jx金屬股份有限公司 | 氧化鎂濺鍍靶 |
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JP4955916B2 (ja) * | 2004-06-17 | 2012-06-20 | タテホ化学工業株式会社 | 単結晶酸化マグネシウム焼結体及びその製造方法並びにプラズマディスプレイパネル用保護膜 |
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JP2008189493A (ja) * | 2007-02-02 | 2008-08-21 | Sumitomo Electric Ind Ltd | 多結晶MgO焼結体 |
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