TW202223119A - 熱噴塗用釔類顆粒粉末及利用其的熱噴塗皮膜 - Google Patents
熱噴塗用釔類顆粒粉末及利用其的熱噴塗皮膜 Download PDFInfo
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- TW202223119A TW202223119A TW110138741A TW110138741A TW202223119A TW 202223119 A TW202223119 A TW 202223119A TW 110138741 A TW110138741 A TW 110138741A TW 110138741 A TW110138741 A TW 110138741A TW 202223119 A TW202223119 A TW 202223119A
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- yttrium
- powder
- thermal spray
- thermal spraying
- spray coating
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Abstract
本發明涉及熱噴塗用釔類顆粒粉末，更詳細而言，為在Y2O3、YOF、YF3、Y4Al2O9、Y3Al5O12及YAlO3中選擇的某一種以上的釔化合物粉末與二氧化矽（SiO
2）粉末的混合物，包含不足10重量%的Y-Si-O中間相，利用其製備的熱噴塗皮膜形成氣孔率低、非常致密的薄膜，耐電漿體性優秀。
Description
本發明涉及包含二氧化矽成分的熱噴塗用釔類顆粒粉末及利用其的高密度的熱噴塗皮膜。
在半導體製造步驟中，為了矽晶片等基板電路的高積體化所需的微細加工， 電漿體幹式蝕刻步驟的重要性越來越重要。
為了在這種環境下使用，提出了將電漿體抵抗性優秀的材料用作腔室構件或將構件的表面用耐電漿體性優秀的物質形成皮膜而提高構件壽命的方案。
其中，藉由用各種材料被覆基材的表面而賦予新的功能性的技術，以往已在多個領域利用。作為這種表面被覆技術之一，例如已知有熱噴塗法，將由陶瓷等材料構成的熱噴塗顆粒，借助於燃燒或電能，以軟化或熔融狀態噴射於基材表面，從而形成熱噴塗皮膜。
一般而言，熱噴塗塗布是藉由使微細的粉末加熱熔融，使熔融的粉末朝向母材的被塗布面噴射而執行。 該噴射的熔融粉末被急劇冷卻，熔融粉末凝固，主要利用機械性結合力而層疊於該塗布對象面。
在該熱噴塗塗布中，利用高溫的電漿體火焰來熔融該粉末的電漿體熱噴塗塗布，在高熔點的諸如鎢或鉬的金屬及陶瓷的塗布中必須使用。該熱噴塗塗布不僅有利於表現出保持母材的材質特性，生產表現出耐磨損、耐腐蝕、耐熱及熱屏障、超硬、耐氧化、絕緣、摩擦特性、散熱、生物功能耐輻射性特性的高功能性材料，而且與化學氣象沈積或物理氣象沈積等其他塗布方法相比，可以在短時間內塗布寬闊面積的對象物。
而且，在半導體器件等的製造領域，一般借助於使用氟、氯、溴等鹵素類氣體的電漿體的幹式蝕刻，進行在半導體基板表面實施微細加工。另外，在幹式蝕刻後，使用氧氣電漿體對取出半導體基板的腔室（真空容器）內部進行清潔。此時，在腔室內部，暴露於反應性高的氧氣電漿體或鹵素氣體電漿體的構件存在被腐蝕的可能性。而且，如果腐蝕（侵蝕）部分從相應構件呈顆粒狀脫落，則這種顆粒附著於半導體基板，會成為導致電路缺陷的異物（以下將相應異物稱為顆粒）。
因此，自以往起，在半導體器件製造裝置中，出於減小顆粒發生的目的，在暴露於氧氣或鹵素氣體等的電漿體的構件上，設置具備耐電漿體侵蝕性的陶瓷的熱噴塗皮膜。
作為這種顆粒發生因素，除了在真空腔室內附著的反應生成物的剝離之外，還會有使用鹵素氣體電漿體或氧氣電漿體而導致的腔室劣化。另外，根據本發明人的研究獲知，在幹式蝕刻環境下，從熱噴塗皮膜發生的顆粒數或大小起因於構成熱噴塗皮膜的顆粒之間結合力的強弱或未熔融顆粒的存在或高氣孔率。
特別是陶瓷的熱噴塗皮膜內塗層內部的密度越高，幹式蝕刻步驟中氣孔等缺陷導致的CFx系列步驟序氣體的吸附程度越減小，可以減小電漿體離子碰撞導致的蝕刻。
一般而言，作為用於形成高密度熱噴塗皮膜的塗布方法，有懸浮液電漿體熱噴塗法（Suspension Plasma Spray：SPS）、氣溶膠沈積法（Aerosol Deposition：AD）或物理氣相沉積法（Physical Vapor Deposition：PVD），這三種方法與原有大氣電漿體熱噴塗法（Air Plasma Spray：APS）方式相比，均存在製造方式復雜、製造單價升高的缺點。
就懸浮電漿體熱噴塗法（SPS）技術而言，借助於相對較高熱源進行半導體腔室內塗布時，伴隨高步驟溫度，發生製品變形等問題，隨著顆粒大小的減小，顆粒飛行距離變短，電漿體裝備與要塗布的基板的作業距離變近，作業一部分受限。另外，就SPS技術而言，由於為水及顆粒分散的懸浮液狀態，流入相同體積時，塗層的成膜速度低，發生追加的步驟時間，製造成本高。
另外，作為氣溶膠沈積法（AD）及物理氣相沉積法（PVD），達成數百μm水平的塗布厚度存在技術上的局限，實際塗布時，在復雜形狀的基板上，塗布作業受限。
因此，需要開發一種能夠利用原有的大氣電漿體熱噴塗法（APS）展現高密度熱噴塗皮膜的技術。
通常的APS熱噴塗法使用的熱噴塗材料的粒子，集中數μm水平的一次粉末形成20~40μm的顆粒粉末，因而提出一種方法，將構成這種熱噴塗材料的一次粉末構成得較小，為1μm以下，從而提高熱噴塗皮膜的密度。
但是，就這種方法而言，隨著熱噴塗材料比表面積的增加，熱無法均勻傳遞給處於顆粒粉末內部的一次粉末，在熱噴塗皮膜的表面或內部形成包括非熔融或再熔融狀態的皮膜，在幹式蝕刻 步驟中成為顆粒發生原因。
另外，如果由顆粒粉末形成的二次粒子過小，則借助於顆粒粉末之間的靜電引力，粉末之間結塊，難以事實上在大氣中移送或顆粒粉末移送後因較低的質量而無法移送到中心部框架便散落到其他處的可能性高。
作為以往技術，韓國公佈專利第10-2016-0131918號（2016年11月16日）公佈的熱噴塗用材料記載稱，作為構成元素，包括包含稀土類元素（RE）、氧（O）及鹵素（X）的稀土類元素氧鹵化物（RE-O-X），鹵素相對於稀土類元素的莫耳比（X/RE）為1.1以上，因此，耐電漿體性提高，氣孔率或硬度等特性得到改善。
另外，在韓國公佈專利第10-2005-0013968號（2005年2月5日）中，公佈了氧化釔塗層內含有100至1000 ppm矽元素的耐電漿體構件，但該包含矽元素的氧化釔塗層藉由包含半導體成分而賦予電氣特性，存在電弧危險性，基本顏色為黑色，與半導體步驟的汙染物無法區分，在清潔腔室時，因混同而追加不必要的清潔步驟的隱患較大。
如上所述，以往為了克服氧化釔或氟化釔熱噴塗材料的物性界限，提出了混合、製備氧化釔及氟化釔，從而製備提高了電漿體侵蝕性、氣孔率、硬度等物性的氟氧化釔熱噴塗材料的技術，盡管如此，在產業層面卻持續要求開發用於製備提高耐電漿體性所需的致密熱噴塗皮膜的技術及用於製備其的熱噴塗用顆粒粉末。
現有技術文獻
專利文獻
（專利文獻0001）韓國公佈專利第10-2016-0131918號（2016年11月16日）
（專利文獻0002）韓國公佈專利第10-2005-0013968號（2005年2月5日）
為了解決上述問題，本發明的主要目的是使二氧化矽粉末包含於釔化合物粉末，提供熱噴塗用顆粒粉末，從而釔類化合物的熔點低下，在熱噴塗皮膜製備步驟時，抑製熱噴塗皮膜內氣孔的形成，由於二氧化矽的沸點低於釔類化合物沸點的特性，二氧化矽在熱噴塗皮膜步驟中一部分消失，因而可以製備致密的釔類熱噴塗皮膜。
為了達成如上所述目的，本發明的一個實施例提供一種熱噴塗用釔類顆粒粉末，其特征在於，包含在Y2O3、YOF、YF3、Y4Al2O9、Y3Al5O12及YAlO3中選擇的某一種以上釔化合物粉末及二氧化矽（SiO
2）粉末，包含不足10重量%的Y-Si-O中間相。
在本發明的一個較佳實施例中，該顆粒粉末的大小可以為5至50μm。
在本發明的一個較佳實施例中，相對於該釔的矽元素重量比（Si/Y）可以為0.3至1.00。
在本發明的一個較佳實施例中，該顆粒粉末可以將平均直徑0.1至10μm、90至99.9質量%的釔化合物粉末與平均直徑0.1至10μm、0.1至10質量%的二氧化矽粉末混合而製備。
在本發明的又一較佳實施例中， 提供一種熱噴塗用釔類顆粒粉末的製備方法，其特征在於，包括：（a）將在Y2O3、YOF、YF3、Y4Al2O9、Y3Al5O12及YAlO3中選擇的某一種以上釔化合物粉末與二氧化矽（SiO
2）粉末混合而製備混合物的步驟；（b）將該混合物造粒而製備顆粒粉末的步驟；及（c）以1200至1450℃燒成該顆粒粉末而收得熱噴塗用釔類顆粒粉末的步驟；該熱噴塗用釔類顆粒粉末包含不足10重量%的Y-Si-O中間相。
在本發明的又一較佳實施例中， 提供一種以該熱噴塗用釔類粒子製備方法製備的熱噴塗用釔類粒子。
在本發明的又一較佳實施例中， 提供一種釔類熱噴塗皮膜製備方法，作為製備該釔類熱噴塗皮膜的方法，在熱噴塗皮膜的製備步驟中，該矽元素在熱噴塗皮膜的製備步驟中一部分氣化。
本發明的從包含二氧化矽成分的熱噴塗用釔類顆粒粉末製備的熱噴塗皮膜，由於塗層內部的密度非常高，在幹式蝕刻步驟中，步驟氣體所致蝕刻率減小，用作半導體腔室內構件的塗布材料時，耐久性優秀，抑製蝕刻現象所致塗布物脫離現象，可以有助於提高半導體晶片的收率。
只要未以其他方式定義，本說明書中使用的所有技術性及科學性術語具有與本發明所屬技術領域具有通常知識者通常所理解的內容相同的意義。一般而言，本說明書使用的命名法是本技術領域習知的及通常使用的。
在本申請說明書通篇中，當提到某部分“包括”某構成要素時，只要沒有特別反對的記載，則意指並非排除其他構成要素，而是可以進一步包括其他構成要素。
在半導體的製造步驟中，利用閘極蝕刻裝置、絕緣膜蝕刻裝置、抗蝕膜蝕刻裝置、濺射裝置、CVD裝置等。另一方面，在液晶的製造步驟中，利用用於形成薄膜電晶體的蝕刻裝置等。另外，在這些製造裝置中，以基於微細加工的高積體化等為目的，采用具備電漿體發生機構的構成。
在這些製造步驟中，作為處理氣體，氟類、氯類等鹵素類腐蝕氣體由於他們的高反應性而用於該裝置。作為氟類氣體，可以為SF
6、CF
4、CHF
3、ClF
3、HF、NF
3等，作為氯類氣體，可以例如Cl
2、BCl
3、HCl、CCl
4、SiCl
4等，在導入這些氣體的氣氛下如果接入微波或高頻等，則這些氣體被電漿體化。暴露於這些鹵素類氣體或其電漿體的裝置構件，要求在表面上除材料成份之外的金屬很少，並具有高耐蝕性。因此，本發明的目的在於提供一種熱噴塗用釔類顆粒粉末，該熱噴塗用釔類顆粒粉末用於提供對電漿體蝕刻裝置用構件進行被覆的耐電漿體性優秀的熱噴塗皮膜。
本發明的熱噴塗用釔類顆粒粉末的特征在於，包含在Y2O3、YOF、YF3、Y4Al2O9、Y3Al5O12及YAlO3中選擇的某一種以上釔化合物粉末及二氧化矽（SiO
2）粉末的混合物，包含不足10重量%的Y-Si-O中間相。
作為該熱噴塗用釔化合物粉末的構成成分，包含在Y2O3、YOF、YF3、Y4Al2O9、Y3Al5O12及YAlO3中選擇的某一種或兩種以上，另外，除釔類化合物之外，還包含二氧化矽（SiO
2）成分，從而降低釔類化合物的熔點，在熱噴塗皮膜製備步驟時抑製熱噴塗皮膜內氣孔的形成，有利於製備氣孔率低、致密的釔類熱噴塗皮膜。
此時，該顆粒粉末可以將平均直徑0.1至10μm、90至99.9質量%的釔化合物粉末與平均直徑0.1至10μm、0.1至10質量%的二氧化矽粉末混合而製備。
較佳該熱噴塗用釔類顆粒粉末內釔化合物包含90至99.9質量%，該二氧化矽包含0.1至10質量%，更佳地，釔化合物可以為95至99.5質量%，該二氧化矽可以為0.5至5質量%。
當該二氧化矽的含量不足0.1質量%時，製備熱噴塗皮膜時，降低二氧化矽熔點的效果微弱，另外，如果該二氧化矽的含量超過約10質量%，則應以二氧化矽（SiO
2）形態消失的成分變換成Y-Si-O中間相，在熱噴塗皮膜內過量殘留。
該二氧化矽的沸點低於該釔化合物的熔點，在本發明的熱噴塗皮膜製備步驟時，在該熱噴塗用釔類顆粒粉末液化、飛散期間，該二氧化矽的一部分乃至全部氣化，賦予降低該熱噴塗用釔類顆粒粉末的熔點的效果，該熱噴塗皮膜製備步驟的塗布膜中殘存的該二氧化矽，與向該熱噴塗皮膜製備步驟投入前相比，含有量降低。
另外，在Y2O3、YOF、YF3、Y4Al2O9、Y3Al5O12及YAlO3中選擇的釔化合物粉末及二氧化矽粉末的平均直徑較佳為0.1至10μm， 更佳地，可以為0.2至5μm。
在 該釔化合物粉末及二氧化矽粉末的平均直徑不足約0.1μm的情況下，會生成Y-Si-O中間相， 該粉末的控製困難，難以形成球形顆粒粉末，會難以調節物性。另外，作為一次粒子的釔化合物粉末及二氧化矽粉末的平均直徑如果超過約10μm，則該一次粉末結塊形成的顆粒粉末的平均直徑過大，會難以形成均一的熱噴塗皮膜。
另外，該二氧化矽粉末的平均直徑與釔化合物粉末的平均直徑的偏差較佳為30%以下。如果該二氧化矽粉末的平均直徑比釔化合物粉末的平均直徑大30%以上，則在皮膜形成時，會生成過量的Y-Si-O中間相。
另外，本發明的熱噴塗用釔類顆粒粉末的大小可以為5至50μm，較佳地，可以為10 ~ 40μm，更佳地，可以為15 ~ 30μm。
如果該熱噴塗用釔類顆粒粉末的大小不足5μm，則在熱噴塗塗布時，粉末的流動性低，無法展現均一的膜，在粉末傳遞到框架之前被氧化或無法傳遞到框架中心，難以滿足用於形成致密膜所需的液滴飛翔速度及熱量，導致形成氣孔高或硬度低的膜。如果釔類顆粒粉末的平均直徑超過50μm，則顆粒粉末的熔融比表面積減小，無法完全熔融，發生塗布膜質內未熔融部分，難以滿足本發明要求的熱噴塗皮膜的品質。
另外，本發明的熱噴塗用釔類顆粒粉末的縱橫比（aspect ratio）用顆粒粉末的長直徑與短直徑之比表示，從形成致密均一的膜的觀點而言，較佳1.0以上、5.0以下，從這種觀點而言，更佳縱橫比為1.0以上、4.0以下，特佳1.0以上、1.5以下。
熱噴塗用釔類顆粒粉末的流動性作為熱噴塗膜品質的重要要素而發揮作用，因而最佳製作成球形，否則，在製備熱噴塗皮膜時，既定量的粉末無法傳遞到框架，也會無法形成我們要求水平的膜。
作為一個例示，該矽元素可以在熱噴塗皮膜的製備步驟中一部分氣化，熱噴塗用釔類顆粒粉末中相對於該釔的矽元素重量比（Si/Y）可以為0.3至1.00。
作為一個例示，該熱噴塗用釔類粒子可以包含不足10重量%的Y-Si-O中間相。
另外，本發明提供一種熱噴塗用釔類顆粒粉末的製備方法，其特征在於，包括：（a）將在Y2O3、YOF、YF3、Y4Al2O9、Y3Al5O12及YAlO3中選擇的某一種以上釔化合物粉末與二氧化矽（SiO
2）粉末混合而製備混合物的步驟；（b）將該混合物造粒而製備顆粒粉末的步驟；及（c）以1200至1450℃燒成該顆粒粉末而收得熱噴塗用釔類顆粒粉末的步驟；該熱噴塗用釔類顆粒粉末包含不足10重量%的Y-Si-O中間相。
下面對本發明的製備熱噴塗用釔類顆粒粉末的方法進行詳細說明。
作為一次材料的在該Y2O3、YOF、YF3、Y4Al2O9、Y3Al5O12及YAlO3中選擇的某一種以上釔化合物粉末及二氧化矽（SiO
2）粉末材料，由於材料的流動性無法達到熱噴塗所需的水平，因而較佳經過製備成球形形態的混合、造粒及燒成步驟而構成顆粒粉末。
在該（a）步驟的混合步驟中，在該Y2O3、YOF、YF3、Y4Al2O9、Y3Al5O12及YAlO3中選擇的某一種以上釔化合物粉末及二氧化矽（SiO
2）粉末材料中添加燒結助劑及分散介質並混合，收得混合物，根據需要，追加與結合劑混合而製備漿料液滴。
作為追加性的結合劑，較佳有機化合物，可以例如由碳、氫及氧或由碳、氫、氧及氮構成的有機化合物，例如羧甲基纖維素（羧甲基纖維素）、聚乙烯醇（PVA）、聚乙烯吡咯烷酮（PVP）等，但不限於此。
然後，在（b）步驟中，包含該釔化合物粉末及二氧化矽（SiO
2）粉末的混合物經過造粒過程。作為造粒裝置，例如可以利用噴霧幹燥（spray drying）裝置。在噴霧幹燥裝置中，包含經粉碎的多個粒子的漿料液滴，在熱風中滴下，液滴因此而固化，造粒成包括多個粒子的中間粒子。
最後，在（c）步驟中，該顆粒粉末經過燒成步驟，較佳燒成溫度為1200至1450 ℃。在該溫度範圍下燒成，從而顆粒粉末內釔化合物粉末與二氧化矽（SiO
2）粉末以物理方式結合。
按照燒成溫度為該範圍的條件，該燒成時間較佳為2小時以上、8小時以下。
燒成氣氛可以使用大氣氣氛等含氧氣氛，但較佳氬氣等惰性氣體氣氛或真空氣氛。
另外，本發明提供一種以該熱噴塗用釔類粒子的製備方法製備的熱噴塗用釔類粒子。
另外，本發明可以熱噴塗該熱噴塗用釔類顆粒粉末而製備在基材上形成的釔類熱噴塗皮膜。
該熱噴塗可以為火焰熱噴塗、電弧（wire arc）熱噴塗、電漿體熱噴塗、真空電漿體熱噴塗、高速火焰熱噴塗（HVOF）、低溫熱噴塗及爆炸熱噴塗中某一種。
該電漿體熱噴塗法包括向該電漿體射流投入熱噴塗用材料，經加熱、加速而堆積於基材，從而獲得熱噴塗皮膜的普通塗布方法。另外，電漿體熱噴塗法可以是在大氣中進行的大氣電漿體熱噴塗（Air Plasma Spray：APS）、在低於大氣壓的氣壓下進行熱噴塗的減壓電漿體熱噴塗（low pressure plasma spraying：LPS）、在高於大氣壓的加壓容器內進行電漿體熱噴塗的加壓電漿體熱噴塗（high pressure plasma spraying）等形態。
借助於這種電漿體熱噴塗，例如作為一個例示，借助於10000 K至15000 K左右的電漿體射流使熱噴塗材料熔融及加速，從而可以使熱噴塗用顆粒粉末以300 m/s至1000 m/s左右速度碰撞基材並堆積。
此時，借助於噴霧裝置而移送的送料器的移送速度較佳為10至30 g/分鐘，該送料器的移送速度超過30 g/分鐘，單位時間期間移送的送料粉末的供應量過多時，難以製備均一的熱噴塗塗布皮膜，送料粉末的一部分無法完全熔融，出現熱噴塗皮膜氣孔率增加的現象。另外，如果送料器的移送速度不足10 g/分鐘，則送料器的移送量不足，由於熱噴塗皮膜的脈動現象，發生熱噴塗皮膜的均一度低下、生產收率低下的問題。
在本發明中，被覆熱噴塗皮膜的基材不特別限定。例如，如果是提供用於這種熱噴塗用材料的熱噴塗並包括可具備所需耐性的材料的基材，則其材質或形狀等不特別限製。作為構成這種熱噴塗的基材的材料，例如較佳在構成半導體製造裝置用構件等的鋁、鎳、鉻、鋅及他們的合金、氧化鋁、氮化鋁、氮化矽、碳化矽及石英玻璃中的至少一種以上的組合中選擇。
這種基材例如為構成半導體器件製造裝置的構件，也可以為暴露於反應性高的氧氣電漿體或鹵素氣體電漿體的構件。
較佳該基材表面在電漿體熱噴塗之前，根據JIS H 9302規定的陶瓷熱噴塗作業標準進行處理。例如，去除該基材表面的銹或油脂等後，噴射Al
2O
3、SiC等磨削粒子而進行表面粗糙化，預處理成熱噴塗顆粒粉末容易附著的狀態。
另外，該熱噴塗皮膜的製備方法除了電漿體熱噴塗之外，也可以藉由將在此公開的熱噴塗材料提供給基於習知熱噴塗方法的熱噴塗裝置而形成。適宜地熱噴塗這種熱噴塗用材料的熱噴塗方法，例如采用高速框架熱噴塗法、框架熱噴塗法、爆炸熱噴塗法等熱噴塗方法。
熱噴塗皮膜的特性會有在某種程度上依賴於熱噴塗方法及其熱噴塗條件的情形。但是，無論采用哪種熱噴塗方法及熱噴塗條件，藉由使用在此公開的熱噴塗用材料，與使用其他熱噴塗材料時相比，可以形成氣孔率低、致密的熱噴塗皮膜。
以往的釔類熱噴塗膜較高地形成塗層內氣孔率，相反，在本發明中添加二氧化矽成分作為一次粉末，降低釔類化合物的熔點，在熱噴塗皮膜製備步驟時，抑製熱噴塗皮膜內氣孔的形成，二氧化矽成分在高溫的皮膜製備步驟中自動消失，因而製備氣孔率低、致密的釔類熱噴塗皮膜。
作為一個例示，以釔類熱噴塗皮膜的製備方法形成的釔類熱噴塗皮膜，氣孔率可以不足2%，較佳地，可以不足1.5%，更佳地，可以不足1%。
因此，本發明的釔類熱噴塗皮膜相比原有熱噴塗皮膜，氣孔率水平優秀，應用於原有蝕刻步驟使用的半導體腔室，表現出優秀的耐久性，抑製蝕刻氣體所致的塗布物脫離現象。
作為一個例示，在該釔類熱噴塗皮膜的製備方法中，矽元素可以在熱噴塗皮膜的製備步驟中一部分氣化，因此，相對於該釔的矽元素重量比（Si/Y）具有0.3至1.00範圍。
另外，就本發明的釔類熱噴塗皮膜而言，在該釔化合物為氧化釔（Y2O3）的情況下，作為該氧化釔的結晶結構，可以包含70至90%單斜晶（monoclinic）形態。此時，解釋為氧化釔（Y2O3）的單斜晶結晶結構賦予提高氧化釔粉末之間接合強度的效果，可以有助於較小地形成熱噴塗皮膜內氣孔的大小。
另外，較佳本發明的釔類熱噴塗皮膜不包含Y-Si-O中間相，可以至少包含不足10重量%的Y-Si-O中間相。
如果該Y-Si-O中間相生成10重量%以上，則發生矽元素（Si）與鹵素類蝕刻氣體反應而氣化的情形，因而生成空隙的可能性升高，腐蝕氣體等步驟氣體會沿著所生成的空隙侵入而發生顆粒。
另外，在該Y-Si-O中間相生成的同時，無法形成顆粒粉末內均質膜，會發生各部位的功能差異，因此，在賦予特性方面發生困難。
下面藉由實施例，更詳細地說明本發明。但是，下述實施例只是對本發明的例示，並非本發明由該實施例所限定。
製備例1~2
在氧化釔粉末及二氧化矽粉末中混合粘合劑後，借助於噴霧幹燥機獲得造粒粉末，然後，對該造粒粉末脫脂後進行燒結，獲得了燒結粉末。各製備例使用的氧化釔粉末及二氧化矽粉末的大小及混合比率等實驗條件顯示於下表1，製備的熱噴塗用顆粒粉末的電子掃描顯微鏡（SEM）照片圖示於第1圖。
[表1]
| 成分 | 顆粒粉末的大小 （μm） | 一次粉末的混合比率 （wt%） | 顆粒粉末內混合比率 （wt%） | |
| 製備例1 | Y 2O 3 | 8.2 | 99.0 | Y：65.93 Si1.45 O：32.62 |
| SiO 2 | 0.8 | 1.0 | ||
| 製備例2 | Y 2O 3 | 0.7 | 99.0 | Y：68.20 Si1.21 O：30.58 |
| SiO 2 | 0.8 | 1.0 | ||
| 製備例3 | Y 2O 3 | 0.7 | 95.0 | Y：70.02 Si5.35 O：24.63 |
| SiO 2 | 0.8 | 5.0 | ||
| 製備例 4 | Y 2O 3 | 0.7 | 90.0 | Y：73.07 Si2.94 O：23.99 |
| SiO 2 | 0.8 | 10.0 | ||
| 製備例 5 | Y 2O 3 | 0.7 | 65.0 | Y：55.54 Si12.41 O：32.06 |
| SiO 2 | 0.8 | 35.0 | ||
| 製備例 6 | Y 2O 3 | 0.7 | 50.0 | Y：41.00 Si19.70 O：39.29 |
| SiO 2 | 0.8 | 50.0 |
實施例1~8
利用該製備例1及4準備的熱噴塗材料及電漿體槍，作為熱源氣體流入氬氣及氫氣，在移動熱噴塗槍的同時，在40~50 kW功率下生成電漿體，利用所生成的電漿體使原料粉末熔融，在母材上形成塗布膜。塗布膜的厚度形成得具有150~200μm，實驗條件顯示於下下表2。另外，製備的熱噴塗皮膜側面的電子掃描顯微鏡（SEM）照片顯示於第2圖。
[表2]
| 類別 | 材料 | 電漿體條件 | 送料器條件 | 隔開距離 （mm） | |
| Ar （NLPM） | 電流 （a） | 送料器 移送速率 （g/分鐘） | |||
| 實施例1 | 製備例1 | 48 | 600 | 20 | 200 |
| 實施例2 | 製備例1 | 48 | 600 | 20 | 150 |
| 實施例3 | 製備例2 | 48 | 600 | 20 | 200 |
| 實施例4 | 製備例2 | 48 | 600 | 20 | 150 |
| 實施例5 | 製備例3 | 48 | 600 | 20 | 200 |
| 實施例6 | 製備例3 | 48 | 600 | 20 | 150 |
| 實施例7 | 製備例4 | 48 | 600 | 20 | 200 |
| 實施例8 | 製備例4 | 48 | 600 | 20 | 150 |
比較例1~6
下述比較例1及比較例2中使用的釔氧化物顆粒粉末內一次粉末的大小為5μm，釔氧化物顆粒粉末的大小為35μm，釔氧化物顆粒粉末內釔元素與氧元素的混合比率為78/22。
利用該釔氧化物顆粒粉末及該製備例5及6中準備的熱噴塗材料，以與該實施例相同方法形成了塗布膜，實驗條件顯示於下表3。
[表3]
| 類別 | 材料 | 電漿體條件 | 送料器條件 | 隔開距離 （mm） | |
| Ar （NLPM） | 電流 （a） | 送料器 移送速率 （g/分鐘） | |||
| 比較例1 | Y 2O 3 | 48 | 600 | 20 | 200 |
| 比較例2 | Y 2O 3 | 48 | 600 | 20 | 150 |
| 比較例3 | 製備例5 | 48 | 600 | 20 | 200 |
| 比較例4 | 製備例5 | 48 | 600 | 20 | 150 |
| 比較例5 | 製備例6 | 48 | 600 | 20 | 200 |
| 比較例6 | 製備例6 | 48 | 600 | 20 | 150 |
實驗例1：熱噴塗皮膜的觀察
第2圖是本發明的實施例1至實施例4的熱噴塗皮膜側面的電子掃描顯微鏡（SEM）照片，藉由第2圖的熱噴塗皮膜側面的電子掃描顯微鏡（SEM）照片，確認形成了熱噴塗皮膜內氣孔率低、致密的薄膜。
另外，氣孔率的測量如下進行。即，將熱噴塗皮膜截斷成與基材表面直交的面，對獲得的剖面進行樹脂包埋研磨後，使用電子顯微鏡（JEOL、JS-6010）拍攝該剖面圖像（第2圖）。使用圖像解析軟件（MEDIA CYBERNETICS，Image Pro）解析該圖像，從而對剖面圖像中的氣孔部分的面積進行特定，算出這種氣孔部分的面積在全體剖面中所占比率，從而求出氣孔率，將藉由在熱噴塗皮膜剖面出現的氣孔面積獲得的氣孔率（porosity）顯示於表4。
比較例1及比較例2製備的熱噴塗皮膜的氣孔率（prosity）表現出2%以上的值，相反，實施例1至4的氣孔率顯示出不足1.5%的值，表明本發明的釔類熱噴塗皮膜的致密度比以往所利用的組成的熱噴塗皮膜增加。
另外，如第3圖所示，實施例1至實施例4的熱噴塗皮膜利用電子掃描顯微鏡（SEM）進行x射線衍射分析法（XRD）分析結果，確認了單斜晶（monoclinic）結晶結構以高於立方晶（cubic）結構的比率存在。有報告稱，氧化釔隨著單斜晶（monoclinic）結晶結構的存在，具有提高一次粉末之間接合強度的效果，根據這種氧化釔的結晶結構預測氣孔率將減小。
[表4]
| 類別 | 熱噴塗皮膜的成分比率 | 測量數據 | |||||
| Y | Si | O | 氣孔率（%） | 硬度（Hv） | 粗糙度（Ra、μm s） | 沈積率 （μm /pass） | |
| 實施例1 | 78.35 | 0.55 | 21.10 | ＜1.5 | 400~450 | 4.6~5.3 | ＞10 |
| 實施例2 | 78.51 | 0.62 | 20.87 | ＜1.0 | 400~450 | 3.2~3.9 | ＞9 |
| 實施例3 | 77.37 | 0.53 | 22.09 | ＜1.0 | 400~450 | 4,7~5.5 | ＞10 |
| 實施例4 | 77.91 | 0.55 | 21.51 | ＜1.0 | 450~500 | 3.1~3.7 | ＞10 |
| 實施例5 | 76.35 | 1.22 | 22.43 | ＜1.0 | 400~450 | 3.8~4.1 | 8.9 |
| 實施例6 | 75.42 | 1.32 | 23.26 | ＜1.0 | 400~450 | 3.3~3.7 | 6.6 |
| 實施例7 | 72.41 | 2.97 | 24.62 | ＜1.5 | 400~450 | 3.6~4.0 | 9.2 |
| 實施例8 | 73.44 | 3.12 | 23.44 | ＜1.5 | 400~450 | 3.2~4.0 | 6.7 |
| 比較例3 | 54.72 | 13.32 | 31.96 | ＜2.5 | 350~400 | 3.7~4.3 | 8.9 |
| 比較例4 | 53.61 | 12.80 | 33.59 | ＜2.5 | 350~400 | 4.7~4.9 | 6.3 |
| 比較例5 | 39.86 | 20.08 | 40.06 | ＜3.5 | 300~350 | 4.8~5.5 | 10.6 |
| 比較例6 | 39.63 | 19.47 | 40.90 | ＜3.5 | 300~350 | 4.6~5.3 | 8.3 |
| 比較例1 | 3.5~5.0 | 400~450 | 3.5~5.5 | 2.5~3.5 | |||
| 比較例2 | 2.0~2.5 | 500~550 | 5~7 | 5~6 |
實驗例2：硬度測量
上表4中的 “硬度” 欄代表各熱噴塗皮膜的維氏硬度的測量結果。維氏硬度的測量使用微小硬度測量儀（公司名，型號名），測量了借助於對面角136°的金剛石壓頭而施加294.2 mN實驗力時求出的維氏硬度（Hv0.2）。
如上表2所示，確認了實施例1至4的熱噴塗皮膜表現出與比較例1及2的熱噴塗皮膜的硬度類似的範圍。
實驗例3：粗糙度測量
利用粗糙度測量儀（SJ-201），測量了本發明實施例及比較例製備的塗布膜的表面粗糙度（roughness、μm），其結果記載於上表4。
實驗例4：沈積率測量
利用掃描電子顯微鏡圖像觀察了本發明實施例及比較例製備的塗布膜厚度，將除以進行相應塗布的次數所得的值記載於上表4。
以上詳細記述了本發明內容的特定部分，所屬技術領域的具有通常知識者不言而喻，這種具體記述只是較佳的實施形態，本發明的範圍並非由此限定。因此，本發明的實質性範圍由附帶的發明申請專利範圍及其等價物所定義。
無。
第1圖是本發明的（a）製備例1及（b）製備例2的熱噴塗用氧化釔顆粒粉末的電子掃描顯微鏡（SEM）照片。
第2圖是本發明的（a）實施例1、（b）實施例2、（c）實施例3、（d）實施例4的熱噴塗皮膜側面的電子掃描顯微鏡（SEM）照片。
第3圖是本發明的（a）實施例1、（b）實施例2、（c）實施例3、（d）實施例4的熱噴塗皮膜的X射線衍射分析（XRD）的結果。
Claims (7)
- 一種熱噴塗用釔類顆粒粉末，作為熱噴塗用釔類顆粒粉末，其中， 包含在Y2O3、YOF、YF3、Y4Al2O9、Y3Al5O12及YAlO3中選擇的某一種以上釔化合物粉末及二氧化矽（SiO 2）粉末， 該顆粒粉末的平均直徑為5至50μm，包含超過0重量%、不足10重量%的Y-Si-O中間相。
- 刪除
- 如請求項1所述的熱噴塗用釔類顆粒粉末，其中， 相對於該釔的矽元素重量比（Si/Y）為0.3至1.00。
- 如請求項1所述的熱噴塗用釔類顆粒粉末，其中， 該顆粒粉末是 將平均直徑0.1至10μm、90至99.9質量%的釔化合物粉末與平均直徑0.1至10μm、0.1至10質量%的二氧化矽粉末混合而製備。
- 一種熱噴塗用釔類顆粒粉末的製備方法，其中，包括： （a）將在Y2O3、YOF、YF3、Y4Al2O9、Y3Al5O12及YAlO3中選擇的某一種以上釔化合物粉末與二氧化矽（SiO 2）粉末混合而製備混合物的步驟； （b）將該混合物造粒而製備顆粒粉末的步驟；及 （c）以1200至1450℃燒成該顆粒粉末而收得熱噴塗用釔類顆粒粉末的步驟； 該熱噴塗用釔類顆粒粉末包含超過0重量%、不足10重量%的Y-Si-O中間相，平均直徑5至50μm。
- 一種熱噴塗用釔類粒子，係以請求項5所述的製備方法製備。
- 一種釔類熱噴塗皮膜的製備方法，作為製備如請求項6記載的釔類熱噴塗皮膜的方法，其中， 在熱噴塗皮膜的製備步驟中，該矽元素在熱噴塗皮膜的製備步驟一部分氣化。
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