TWI598448B - 積層製造用具生物相容性之鈦基金屬玻璃合金 - Google Patents
積層製造用具生物相容性之鈦基金屬玻璃合金 Download PDFInfo
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Description
本發明提供一種具有生物相容性以及高玻璃形成能力之鈦合金,適合用於製作超細粉體,並且用於積層製造。
鈦或鈦合金具有強度高、耐蝕性佳、耐熱性佳、高生物相容性等特點,已廣泛用於各種產業,特別是醫療器材,例如做為脊椎固定裝置、人工關節、人工髖關節骨幹、脛骨基座、人工牙根等;特別是其具有低彈性係數之特點,若植入材料具有不相應之楊氏係數(Young’s modulus),受到彈性的彎曲變形時,楊氏係數差異過大容易造成骨頭無法均勻將負載分散於植入材料上,引起人體組織受損以及增加康復時間。
積層製造(Additive Manufacturing),又稱3D列印,指稱以三維方式列印物體之方法,已不斷添加材料之過程,在電腦控制下層疊材料。相較於傳統加工方法係利用研磨、鍛造、焊接等方法製造所需之產品,積層製造是利用噴塗、擠壓、堆疊方式製造。
鈦合金金屬玻璃係一種不具有晶粒和晶界之玻璃結構,霧化造粉時內部沒有晶粒大小來影響粉體表面,所以呈現極低表面粗糙度,因此鈦合金
金屬玻璃可提供表面光滑之粉體作為積層製造使用。此外,鈦合金金屬玻璃亦具有低液相溫度、低熔化熱焓、以及低殘留應力等特點。
已發表之先前技術中,US6786984揭示一種用於牙科或骨科器材之鈦合金,包括Sn、Ti或Zr、以及Nb或Ta;其中Nb或Ta於合金之中含量(分子比例)為8-20%,Sn之含量則為2-6%;但其玻璃形成能力(Glass Forming Ability,GFA)不佳,而且熔點較高。此外,EP2530176提供一種醫療用體內植入材料之鈦合金,其構成包括非晶相和準結晶相之TiaZrbNbcMdIe,其中M可為Ni、Co、Fe、或Mn,而I代表不可避免之雜質;但其仍然具有熔點過高的問題。
有鑑於前述先前技術之特性不利於鈦合金用於醫療材料,有必要發展適合用於醫療材料、具有高生物相容性、以及GFA較佳並且適合用於積層製造之鈦合金材料。
本發明之目的係在於提供一種具有生物相容性之鈦合金,係由式TiaZrwTabSixSnyCoz之合金所組成,其中a係40-44;b係1-5;w、x、y、z之總和為51-59;且y及z之其中至少一者不為0。
於本發明一特定實施例,a係4.15-42.5;b係2.5-3.5。
於本發明另一特定實施例,w係22-48;x係1-15;y係1-15;z係1-23。
於本發明特定實施例,該鈦合金係選自Ti42Zr35Ta3Si5Co12.5Sn2.5、Ti42Zr35Ta3Si5Co10Sn5、Ti42Zr35Ta3Si5Co7.5Sn7.5、Ti42Zr35Ta3Si5Co5Sn10、Ti42Zr35Ta3Si5Co2.5Sn12.5、Ti42Zr35Ta3Si6.25Sn2.5CO11.25、Ti42Zr35Ta3Si6.25Sn1.25Co12.5、Ti42Zr35Ta3Si5Sn3.75Co11.25、Ti42Zr35Ta3Si5Sn1.25Co13.75、Ti42Zr35Ta3Si3.75Sn5Co11.25、
Ti42Zr35Ta3Si3.75Sn3.75CO12.5、Ti42Zr35Ta3Si3.75Sn2.5CO13.75、Ti42Zr35Ta3Si2.5Sn6.25CO11.25、Ti42Zr35Ta3Si2.5Sn5CO12.5、Ti42Zr35Ta3Si2.5Sn3.75CO13.75、Ti42Zr35Ta3Si2.5Sn2.5Co15、Ti42Zr35Ta3Si1.25Sn6.25Co12.5、Ti42Zr35Ta3Si1.25Sn5CO13.75、Ti42Zr35Ta3Si1.25Sn3.75CO15、Ti42Zr35Ta3Si0sn3.75Co16.25、Ti42Zr35Ta3Si2.5Sn1.25CO16.25所構成之群組。
於本發明特定實施例,該鈦合金係非晶質合金。
於本發明特定實施例,該鈦合金之熔點小於1000℃並且大於800℃。
於本發明特定實施例,該鈦合金係用於積層製造。
於本發明特定實施例,該鈦合金之玻璃超細粉體係使用氬進行霧化。
於本發明特定實施例,該鈦合金之玻璃超細粉體之顆粒大小係至少半數小於53微米。
於本發明特定實施例,該鈦合金之玻璃超細粉體之形狀因數係為0.85-1。
圖1 TiSnCo鈦合金系統製造用於積層製造粉體之顆粒大小分布。
本發明之新穎技術特徵,包含特定特徵,係揭示於申請專利範圍,針對本發明之技術特徵,較佳之理解茲配合說明書、依據本發明原理之實施例、和圖式將本發明詳細說明如下。
本發明說明書及申請專利範圍中所述之所有技術性及科學用語,除非另有所定義,皆為本發明所屬技術領域具有通常知識者可知曉之定義。其中單數用語「一」、「一個」、「該」、或其近似用語,除非另有說明,皆可指涉多於一個對象。本說明書使用之「或」、「以及」、「和」,除非另有說明,皆指涉「或/和」。此外,用語「包含」、「包括」皆非有所限制之開放式連接詞。前述定義僅說明用語定義之指涉而不應解釋為對發明主體之限制。除非另有說明,本發明所用之材料皆市售易於取得。
為測試特定組成之鈦合金所具有之特性,以不同組成之合金TiaZrwTabSixSnyCoz進行測試,其中40≦a≦44,1≦b≦5,w、x、y、z之總和為55且y及z之其中至少一者不為0;較佳地,a係42,b係3;其中,係數a、b、w、x、y、z均為各特定金屬於每單位合金中之原子百分比(at%)。將前述合金於利用氬氣保護之電弧爐反覆熔解成錠狀合金,再將該錠狀合金放入薄帶製造機中,以旋噴熔煉(melt spinning)製作厚度為25-50微米(μm)之長條形金屬玻璃薄帶。
使用X射線和穿透式電子顯微鏡(TEM)確認完成後之該薄帶之顯微結構為非晶質合金,再以掃描式電子顯微鏡(SEM)/能量色散X-射線光譜(EDS)以及電子微探儀(EPMA)分析該合金之設計組成和實際熔煉後之組成差異;確認無差異後,該薄帶分別使用微差掃描熱量法(differential scanning calorimetry,DSC)以及高溫DSC分析其熱性質,包括分析其玻璃轉換溫度(Tg)(以絕對溫度計算)、結
晶化溫度(Tx)、熔化溫度(Tm)、和液相溫度(Tl),接著將相關參數套入玻璃形成能力指標並計算個特定組成之合金之玻璃形成能力,前述指標包括:Trg=Tg/Tl;△Tx=Tx-Tg;γ=Tx/(Tg+Tl);以及γm=(2Tx-Tg)/Tl。
比較實施例
文獻上多孔非晶質合金生醫植入材全都是單一孔洞率,與人體骨頭結構不同,接近仿生植入材應是外層緻度來提供支撐,內層漸近孔洞來提供組織和體液流動,因此上述複雜的幾何結構唯有利用積層製造方能施行,因為本技術著重於可霧化噴粉產生積層製造需要的粉體原料,以及經雷射燒結後,顯微結構為金屬玻璃態。
習知技術者所使用之Ti42ZrTa3Si合金系統,其具有一特定比例之Si,但Si於合金中原子大小最小,較高比例之Si會造成填充密度(packing density)較高;相對地,降低Si之比例可有效地降低合金之液態黏性。
Ti42ZrTa3Si合金系統之特性,揭示於表1。
Ti42ZrTa3Si合金系統,其具有高黏性、玻璃形成能力不佳等缺點。為提供較佳之積層製造之噴粉,較佳應提供高玻璃形成能力以及低黏性之合金,但依據表1所揭示之比較例,Si之含量最低應為12.5%。因此應加入其他元素改良。
實施例1
以TiZrTaSi之合金為基材,分別加入Sn和Co測試其合金特性,本實施例之合金之測試結果,揭示於表2-4。
依據表2所揭示,若以TiZrTaSi之合金為基材,並添加原子百分比2.5-10之Sn,其△Tx約介於30-149,並且其γm約略落於0.5-0.61之間,相較於10%之Sn,若添加5%之Sn,較能降低△Tx。
此外,依據表3所揭示,若以TiZrTaSi之合金為基材,並添加原子百分比7-17.5之Co,其△Tx約介於22-72,並且其γm約略落於0.65-0.76之間。若比較Sn和Co之玻璃形成能力,添加Co後合金可得到更加之玻璃形成能力。因此,
應可以TiZrTaSi之合金為基材,適量添加特定莫耳比之Sn或Co,以得到較佳之玻璃形成能力之合金。
此外,依據表4所揭示,若以TiZrTaSi之合金為基材,並添加特定比例之原子百分比2.5-12.5之Co以及原子百分比2.5-12.5之Sn,則其γm可達到0.76以上,故混和特定比例之Co以及Sn之鈦合金可更有效改善其玻璃形成能力。
另,依據表5所揭示,若以TiZrTaSi之合金為基材,並添加特定比例之Sn或Co,其中進一步測試Sn於莫耳比例小於6.25時對於改善玻璃形成能力之影響;則γm至少為0.78,另於較佳之實施方式,可達成0.8-0.82之γm。
適當之用於積層製造之具有生物相容性之鈦合金,其具有之特性應以低黏性、低熔點、高玻璃形成能力(GFA)為佳,並且低熔點之合金通常具有較佳之玻璃形成能力,並且低熔點之合金僅需使用低功率之雷射即可作用。於本發明實施方式中,加入Sn有效降低黏性、增加玻璃形成能力,但對於熔點無影響,並且造成△Tx增加;相對地,加入Co有效降低黏性、熔點、和△Tx,並可增加玻璃形成能力。。
實施例2
由於鈦合金金屬玻璃黏度高、不易形成噴粉,本發明另提供一種製造實施例1所揭示之鈦合金之噴粉製造方法,可製作適合用於積層製造之粉體,具有低表面粗糙度、真圓率高等特性。
配合本說明書實施例1之合金,以Ti42Zr40Ta3Si7.5Sn7.5製造噴粉。噴粉製造方法包括:將錠狀合金置於坩堝中,並用高週波加熱至錠狀合金成為液相;再將該液相合金倒入保溫坩堝之中,並於該保溫坩堝中加壓使該保溫坩
堝中之該液相合金流入該保溫坩堝之霧化噴嘴區;自該霧化噴嘴區中流出之該液相合金經由氬(Ar)進行霧化,得到合金之粉體。
前述合金粉體之顆粒細小,並且其表面粗糙度低,可提供良好之鋪粉流動性以及粉床密度,適合用於積層製造。依據前述方法所製造之合金粉體,其顆粒大小之分布揭示於圖1;若為TiSnCo合金系統,粉體顆粒直徑小於37μm之比例為26%,粉體顆粒直徑介於37-53μm之比例為25.7%,顆粒直徑小於53μm之粉體佔顆粒小於105μm之粉體之比例為51.7%。
Claims (10)
- 一種具有生物相容性之鈦合金,係由式TiaZrwTabSixSnyCoz之合金所組成,其中a係40-44;b係1-5;w、x、y、z之總和為51-59;且y及z之其中至少一者不為0。
- 如申請專利範圍第1項所述之鈦合金,其中a係41.5-42.5;b係2.5-3.5。
- 如申請專利範圍第2項所述之鈦合金,其中w係22-48;x係1-15;y係1-15;z係1-23。
- 如申請專利範圍第1項所述之鈦合金,其中該鈦合金係選自Ti42Zr35Ta3Si5CO12.5Sn2.5、Ti42Zr35Ta3Si5Co10Sn5、Ti42Zr35Ta3Si5CO7.5Sn7.5、Ti42Zr35Ta3Si5CO5Sn10、Ti42Zr35Ta3Si5Co2.5Sn12.5、Ti42Zr35Ta3Si6.25Sn2.5CO11.25、Ti42Zr35Ta3Si6.25Sn1.25CO12.5、Ti42Zr35Ta3Si5Sn3.75CO11.25、Ti42Zr35Ta3Si5Sn1.25CO13.75、Ti42Zr35Ta3Si3.75Sn5Co11.25、Ti42Zr35Ta3Si3.75Sn3.75Co12.5、Ti42Zr35Ta3Si3.75Sn2.5CO13.75、Ti42Zr35Ta3Si2.5Sn6.25CO11.25、Ti42Zr35Ta3Si2.5Sn5CO12.5、Ti42Zr35Ta3Si2.5Sn3.75CO13.75、Ti42Zr35Ta3Si2.5Sn2.5CO15、Ti42Zr35Ta3Si1.25Sn6.25CO12.5、Ti42Zr35Ta3Si1.25Sn5CO13.75、Ti42Zr35Ta3Si1.25Sn3.75Co15、Ti42Zr35Ta3Si0sn3.75Co16.25、Ti42Zr35Ta3Si2.5Sn1.25CO16.25所構成之群組。
- 如申請專利範圍第1項所述之鈦合金,其中該鈦合金係非晶質合金。
- 如申請專利範圍第1項所述之鈦合金,其中該鈦合金之熔點小於1000℃。
- 如申請專利範圍第1項所述之鈦合金,其中該鈦合金係用於積層製造。
- 如申請專利範圍第7項所述之鈦合金,其中該鈦合金為使用氬進行霧化所形成之玻璃超細粉體。
- 如申請專利範圍第8項所述之鈦合金,其中該玻璃超細粉體之顆粒大小係至少半數小於53微米。
- 如申請專利範圍第8項所述之鈦合金,其中該玻璃超細粉體之形狀因數係為0.85-1。
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