TWI440722B - Ti-cu-sn titanium alloy composition - Google Patents
Ti-cu-sn titanium alloy composition Download PDFInfo
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本發明係關於一種鈦合金組成物，特別是一種高強度、低彈性模數、耐磨耗及無毒性之Ti-Cu-Sn鈦合金組成物。The present invention relates to a titanium alloy composition, particularly a Ti-Cu-Sn titanium alloy composition having high strength, low modulus of elasticity, wear resistance and non-toxicity.
純鈦或Ti-6Al-4V合金已經廣泛應用於各式需要高強度的材料製程領域，甚至將該些生產成生醫級純鈦或Ti-6Al-4V鈦合金的組成物，應用於生醫材料(如齒用材料、人工骨頭…等)。Pure titanium or Ti-6Al-4V alloy has been widely used in various fields of materials requiring high strength, and even used to produce biomedical grade titanium or Ti-6Al-4V titanium alloy composition for biomedical applications. Materials (such as dental materials, artificial bones, etc.).
習知鈦合金組成物，如中華民國公告第442272號「具有一金屬核心之陶瓷牙科用齒臺」、公告第M348589號「植體癒合帽」及公告第M380793號「齒冠支柱體之結構」等專利案係係揭示用於形成齒用結構(支柱體、癒合帽、植體)之組成成分，該成分係可以為氧化鋯、鈦合金、鋁合金、氮化鈦、純鈦…等合金成分。Conventional titanium alloy compositions, such as the Republic of China Bulletin No. 442272 "Ceramic dental rack with a metal core", Announcement No. M348589 "Plant healing cap" and Announcement No. M380793 "Structure of crown crown" The patent system reveals the components used to form the dental structure (pillar body, healing cap, implant), which may be alloy components such as zirconia, titanium alloy, aluminum alloy, titanium nitride, pure titanium, etc. .
以純鈦或鈦合金產品之製作層面而言，通常必須先對純鈦或鈦合金組成物進行加工處理後方可獲得純鈦或鈦合金之產品。In the production aspect of pure titanium or titanium alloy products, it is usually necessary to process the pure titanium or titanium alloy composition before obtaining a pure titanium or titanium alloy product.
若以純鈦作為加工材質，純鈦的熔點高達1670℃，且其必須於在真空環境下且高於1670℃的高溫情形下，進行真空熔煉及鑄造。由於鈦係為高活性元素，一般在600~900℃情形下進行加工處理，將會容易產生氧化作用，且隨著加工溫度越高，氧化速率越快，所造成之氧化現象越嚴重，將會影響到純鈦產品的性質；再且，純鈦之彈性模數高及韌性較高，以切削工具對其進行切削加工時，容易造成切削工具快速磨損，以及加工精準度不佳之缺點；再且，純鈦之強度、硬度及剛性均明顯不足，造成該材料之應用有所限制。If pure titanium is used as the processing material, the melting point of pure titanium is as high as 1670 ° C, and it must be vacuum smelted and cast under high temperature conditions in a vacuum environment and higher than 1670 ° C. Since titanium is a highly active element, it is generally processed at 600~900 °C, which will easily cause oxidation. As the processing temperature is higher, the oxidation rate will be faster, and the oxidation phenomenon will be more serious. It affects the properties of pure titanium products. Moreover, pure titanium has high elastic modulus and high toughness. When cutting with cutting tools, it is easy to cause rapid wear of cutting tools and the disadvantage of poor processing accuracy. The strength, hardness and rigidity of pure titanium are obviously insufficient, which limits the application of the material.
若以鈦合金作為加工材質，以生醫級Ti-6Al-4V合金為例，雖然其具有優異強度及機械性質，但由於其合金組成物之鋁、釩元素會與人體發生化學反應形成離子，如鋁離子被認為與阿茲海默症的發生有關，且釩離子具有細胞毒性，可能對組織產生不良影響，因此該Ti-6Al-4V鈦合金亦應用於生醫材料領域作為人體植入物之材料使用，以免鋁或釩離子於生物體內溶出而對細胞及組織產生毒性傷害，甚至導致人體各種慢性病的生成。If titanium alloy is used as the processing material, the biomedical grade Ti-6Al-4V alloy is taken as an example. Although it has excellent strength and mechanical properties, the aluminum and vanadium elements of the alloy composition will chemically react with the human body to form ions. For example, aluminum ions are considered to be involved in the occurrence of Alzheimer's disease, and vanadium ions are cytotoxic and may have adverse effects on tissues. Therefore, the Ti-6Al-4V titanium alloy is also used as a human implant in the field of biomedical materials. The material is used to prevent the aluminum or vanadium ions from being dissolved in the living body to cause toxic damage to cells and tissues, and even cause the formation of various chronic diseases in the human body.
因此，確實有必要開發新一代的鈦合金組成物及材料，以取代習用純鈦或鈦合金組成物。Therefore, it is indeed necessary to develop a new generation of titanium alloy compositions and materials to replace the conventional pure titanium or titanium alloy composition.
本發明目的乃改良上述缺點，以提供一種Ti-Cu-Sn鈦合金組成物，透過於該鈦合金中加入錫與銅之成分，形成高性能奈米結構，強化鈦合金之機械性質。SUMMARY OF THE INVENTION The object of the present invention is to improve the above disadvantages by providing a Ti-Cu-Sn titanium alloy composition by incorporating a composition of tin and copper into the titanium alloy to form a high-performance nanostructure and strengthening the mechanical properties of the titanium alloy.
本發明次一目的係提供一低熔點之Ti-Cu-Sn鈦合金組成物，以降低加工過程中的氧化速率。A second object of the present invention is to provide a low melting point Ti-Cu-Sn titanium alloy composition to reduce the rate of oxidation during processing.
本發明再一目的係提供一無毒性之Ti-Cu-Sn鈦合金組成物，且具有良好生物相容性，以供應用於生醫材料領域。Still another object of the present invention is to provide a non-toxic Ti-Cu-Sn titanium alloy composition which has good biocompatibility for supply in the field of biomedical materials.
本發明另一目的係提供一高強度、高硬度之Ti-Cu-Sn鈦合金組成物，以降低加工困難度。Another object of the present invention is to provide a high strength, high hardness Ti-Cu-Sn titanium alloy composition to reduce processing difficulty.
本發明係一種Ti-Cu-Sn鈦合金組成物，係包含以重量百分比計0.1~15%之銅、0.1~20%之錫以及79.9~99.8%之鈦。The present invention is a Ti-Cu-Sn titanium alloy composition comprising 0.1 to 15% by weight of copper, 0.1 to 20% of tin, and 79.9 to 99.8% of titanium.
藉此，本發明之Ti-Cu-Sn鈦合金組成物可形成高性能奈米結構，機械性質優於一般商業純鈦，具有高強度、低彈性模數及耐磨耗等特性，提升鈦合金加工性並減少切削刀具磨耗；再且，本案之Ti-Cu-Sn鈦合金組成物另具有無毒性及生物相容性佳等特性，可應用於生醫材料製作；再且，該銅及錫之添加可降低鈦合金熔點，並降低氧化速率。Thereby, the Ti-Cu-Sn titanium alloy composition of the invention can form a high-performance nanostructure, and the mechanical property is superior to that of the general commercial pure titanium, and has the characteristics of high strength, low elastic modulus and wear resistance, and the titanium alloy is improved. Processability and reduce cutting tool wear; Moreover, the Ti-Cu-Sn titanium alloy composition of the present invention has the characteristics of non-toxicity and good biocompatibility, and can be applied to the production of biomedical materials; further, the copper and tin The addition can lower the melting point of the titanium alloy and reduce the oxidation rate.
為讓本發明之上述及其他目的、特徵及優點能更明顯易懂，下文特舉本發明之較佳實施例作詳細說明如下：本發明之Ti-Cu-Sn鈦合金組成物主要係以於鈦(Ti)金屬中添加銅及錫之成分，以透過該銅(Cu)及錫(Sn)金屬之添加來降低整體鈦金屬之熔點並提高材料硬度及機械性質。The above and other objects, features, and advantages of the present invention will become more apparent from the description of the preferred embodiments of the invention. A component of copper and tin is added to the titanium (Ti) metal to reduce the melting point of the entire titanium metal and improve the hardness and mechanical properties of the material by the addition of the copper (Cu) and tin (Sn) metals.
本發明之Ti-Cu-Sn鈦合金組成物係透過下列方式製成的：本發明之Ti-Cu-Sn鈦合金組成物係先於真空環境下，以高溫使鈦、銅及錫金屬熔化後，成均勻鈦銅-錫合金之熔湯，並澆鑄進預定鑄模內，在凝固過程中析出鈦相及介金屬相。更詳言之，該熔融後之鈦-銅-錫合金組成於凝固過程中，經過凝固點時，將會先於凝固成核、成長形成 固溶Sn及Cu之體心結構β-Ti(Sn,Cu)相，稱為β-Ti(Sn,Cu)，以及奈米級Ti3 Sn之介金屬相。The Ti-Cu-Sn titanium alloy composition of the present invention is produced by the following method: the Ti-Cu-Sn titanium alloy composition of the present invention is melted under high temperature to melt titanium, copper and tin metal at a high temperature. A uniform titanium-copper-tin alloy melt is cast into a predetermined mold to precipitate a titanium phase and a metal phase during solidification. More specifically, the molten titanium-copper-tin alloy composition during solidification, passes through the solidification point, and will form a body-center structure β-Ti(Sn, which is solidified and nucleated and grows to form solid solution of Sn and Cu. The Cu) phase, referred to as β-Ti (Sn, Cu), and the mesometallic phase of nanoscale Ti 3 Sn.
接著，隨著溫度下降至轉變溫度835~882℃，該轉變溫度係依組成金屬配比之不同而定〕時，該固溶錫和銅之β-Ti(Sn,Cu)將會轉變為固溶錫之六方緊密堆積結構之α-Ti(Sn)並析出成(Ti,Sn)2 Cu之介金屬相。其中，錫固溶於六方緊密堆積結構之α-Ti(Sn)相，能有效地造成晶格扭曲效果，而增加差排密度，成為固溶強化作用。其二，奈米級Ti3 Sn介金屬相能成為析出(Ti,Sn)2 Cu介金屬相之成核點，進而促進析出近似奈米級(Ti,Sn)2 Cu介金屬相。如添加5wt%錫之Ti-7Cu-5Sn的微組織結構，其能使Ti2 Cu達到奈米級，如圖2b所表示。如此，前述所產生之Ti3 Sn介金屬相於此階段將能夠促使Ti2 Cu介金屬相成長為奈米級的晶相，係能提升該Ti2 Cu晶相之緻密度，使得本案之Ti-Cu-Sn鈦合金組成物於凝固後係為具有奈米級組織結構、高機械性質型態高強度、的鈦-銅-錫三元鈦合金合金。因此本案可增加鈦-銅-錫合金之固溶強化相作用及提高奈米級之介金屬的析出量及，進而提升本案Ti-Cu-Sn鈦合金組成物的整體強度。Then, as the temperature drops to a transition temperature of 835 to 882 ° C, which is determined by the composition of the metal, the solid solution of tin and copper β-Ti (Sn, Cu) will be converted into solid solution. The hexagonal hexagonal structure closely accumulates α-Ti(Sn) and precipitates into a mesometallic phase of (Ti,Sn) 2 Cu. Among them, the tin solid is dissolved in the α-Ti(Sn) phase of the hexagonal close-packed structure, which can effectively cause the lattice distortion effect, and increase the difference density, and become a solid solution strengthening effect. Second, the nano-Ti 3 Sn intermetallic phase can precipitate the nucleation point of the (Ti,Sn) 2 Cu mesophase, and promote the precipitation of a similar nano-scale (Ti,Sn) 2 Cu intermetallic phase. For example, a micro-structure of Ti-7Cu-5Sn of 5 wt% tin is added, which enables Ti 2 Cu to reach the nanometer level, as shown in Fig. 2b. Thus, Ti 3 Sn intermetallic phase arising from the preceding stage will be able to cause this Ti 2 Cu intermetallic phase growth of nanoscale crystal phase, can improve the system Ti 2 Cu density of the crystal phase, so that the case of Ti The -Cu-Sn titanium alloy composition is a titanium-copper-tin ternary titanium alloy alloy having a nano-structure structure and a high mechanical strength and high strength after solidification. Therefore, the present invention can increase the solid solution strengthening phase effect of the titanium-copper-tin alloy and increase the precipitation amount of the nano-scale intermetallics, thereby improving the overall strength of the Ti-Cu-Sn titanium alloy composition.
因此，本發明之Ti-Cu-Sn鈦合金組成物係包含有以重量百分比計0.1~15%之銅、0.1~20%之錫以及作為平衡相79.9~99.8%之鈦。其中，該銅及錫之添加係用以於鈦合金凝固過程中共同析出固溶強化之錫元素於α-Ti(Sn)純鈦相及奈米級介金屬相；再且，該錫之添加如前述可增加鈦之固溶強化並促使Ti2 Cu介金屬相析出成為奈米級的晶相，因此可增加鈦合金之整體強度；再且，該銅及錫之添加亦可用以降低純鈦的高熔點及高彈性模數，有利於後續加工製程之進行。而本案之Ti-Cu-Sn鈦合金組成物由於並未含有如鋁或釩等可能對細胞產生毒性之物質，具有極佳的生物相容性，因此可進一步應用於人體植入物等生醫材料之製備，而不會有對生物體產生不良影響之疑慮。Therefore, the Ti-Cu-Sn titanium alloy composition of the present invention contains 0.1 to 15% by weight of copper, 0.1 to 20% of tin, and 79.9 to 99.8% of titanium as an equilibrium phase. Wherein, the addition of copper and tin is used for co-precipitating solid solution strengthening tin element in α-Ti(Sn) pure titanium phase and nano-scale intermetallic phase during solidification of titanium alloy; and further, adding tin As described above, the solid solution strengthening of titanium can be increased and the Ti 2 Cu intermetallic phase precipitates to become a nano phase crystal phase, thereby increasing the overall strength of the titanium alloy; further, the addition of copper and tin can also be used to reduce pure titanium. The high melting point and high modulus of elasticity are beneficial to the subsequent processing. The Ti-Cu-Sn titanium alloy composition of the present invention can be further applied to human implants and the like because it does not contain substances such as aluminum or vanadium which may be toxic to cells and has excellent biocompatibility. Preparation of materials without doubts about adverse effects on the organism.
其中，本發明之Ti-Cu-Sn鈦合金組成物中，該銅金屬之含量若高於15wt%，則可能會形成過多Ti2 Cu介金屬相成為脆化而難於加工成形；若低於0.1wt%，則該奈米級Ti2 Cu之介金屬相的比例不高，對提升鈦合金整體強度及硬度的效果相對較為有限。Wherein, in the Ti-Cu-Sn titanium alloy composition of the present invention, if the content of the copper metal is more than 15% by weight, excessive Ti 2 Cu intermetallic phase may be formed to become embrittled and difficult to be formed; if less than 0.1 When wt%, the ratio of the mesophase phase of the nano-Ti 2 Cu is not high, and the effect of improving the overall strength and hardness of the titanium alloy is relatively limited.
而該錫金屬之含量若高於20wt%，則可能會形成過多Ti-Sn介金屬相成為脆化而難於加工成形；若低於0.1wt%，則固溶錫之α-Ti(Sn)相之含量較低，可能無法有效促使Ti2 Cu介金屬相成長為奈米級的晶相，因此對提升鈦合金整體強度及硬度的效果亦不佳。If the content of the tin metal is more than 20% by weight, excessive Ti-Sn intermetallic phase may be formed to become embrittled and difficult to be formed; if less than 0.1 wt%, the α-Ti(Sn) phase of solid solution tin may be formed. The lower content may not effectively promote the growth of the Ti 2 Cu mesophase to the nanocrystalline phase, and thus the effect on improving the overall strength and hardness of the titanium alloy is also poor.
此外，本發明之Ti-Cu-Sn鈦合金組成物中亦可依需求選擇性的添加1～3%之鈀(Pd)、1～3%之鉬(Mo)、1～3%之鉑(Pt)、1~3%之鋯(Zr)或1～3%之鉭(Ta)等成分，以透過鈀、鉑及鉭提升合金的耐候性及機械性質，透過無毒性之鉬及鋯提升合金β相的穩定性，並增加延性及機械性質。In addition, in the Ti-Cu-Sn titanium alloy composition of the present invention, 1 to 3% of palladium (Pd), 1 to 3% of molybdenum (Mo), and 1 to 3% of platinum may be selectively added as needed ( Pt), 1 to 3% zirconium (Zr) or 1 to 3% of tantalum (Ta), etc., to enhance the weatherability and mechanical properties of the alloy through palladium, platinum and rhodium, through non-toxic molybdenum and zirconium lifting alloys The stability of the beta phase increases ductility and mechanical properties.
為證實本案之Ti-Cu-Sn鈦合金組成物具有前述優異奈米級結構組織機械性質優異等特點，另將本案不同配比之Ti-Cu-Sn鈦合金組成物之性質詳列於下，並配合第1a、1b及2a、2b圖所示。其中，第1a及1b圖皆係為Ti-7Cu鈦合金微組織結構圖，且第1a圖係為光學顯微圖(OM)；第1b圖則為掃描式電子顯微圖(SEM)。第2a及2b圖係為Ti-7Cu-5Sn鈦合金微組織結構圖，且第2a圖係為光學顯微圖(OM)；第2b圖則為掃描式電子顯微圖(SEM)。In order to confirm that the Ti-Cu-Sn titanium alloy composition of the present invention has the characteristics of excellent mechanical properties of the above-mentioned excellent nano-structure, and the properties of the Ti-Cu-Sn titanium alloy composition of different ratios in this case are listed below. It is shown in Figures 1a, 1b and 2a and 2b. Among them, Figures 1a and 1b are all microstructure diagrams of Ti-7Cu titanium alloy, and Figure 1a is an optical micrograph (OM); Figure 1b is a scanning electron micrograph (SEM). 2a and 2b are micro-structure diagrams of Ti-7Cu-5Sn titanium alloy, and Fig. 2a is an optical micrograph (OM); and Fig. 2b is a scanning electron micrograph (SEM).
由第1a、1b及2a、2b圖所示，第1a及1b圖皆係為Ti-7Cu鈦合金微組織結構圖，其第1b圖中之灰色為α-Ti基底，白色為Ti2 Cu介金屬相；第2a及2b圖則皆為再添加5wt%錫之Ti-7Cu-5Sn鈦合金SEM為組織結構圖，其第2b圖中之白色為Ti2 Cu介金屬相，其係因錫元素添加於鈦合金而細化成奈米級Ti2 Cu。As shown in Figures 1a, 1b, 2a, and 2b, the first and first graphs are the microstructure of the Ti-7Cu titanium alloy. The gray in the first graph is the α-Ti substrate and the white is the Ti 2 Cu. The metal phase; the 2a and 2b plans are the SEM of the Ti-7Cu-5Sn titanium alloy with 5wt% tin added, and the white in the 2b figure is the Ti 2 Cu mesophase, which is the tin element. It is added to a titanium alloy to be refined into nano-sized Ti 2 Cu.
再者，表一所述之Ti-7Cu-1Sn係指鈦合金中含有7wt%之銅、1wt%之錫以及達平衡之鈦金屬，其餘標示依此類推，且下述各實施例之Ti-Cu-Sn鈦合金組成物皆是以前述方式所製成。Further, the Ti-7Cu-1Sn described in Table 1 means that the titanium alloy contains 7 wt% of copper, 1 wt% of tin, and the balance of titanium metal, and the rest is labeled, and the following examples are Ti- The Cu-Sn titanium alloy compositions were all produced in the manner described above.
由表一可得知，本案之Ti-Cu-Sn鈦合金組成物由於如前述具有較為緻密之晶相，因此相較於習用純鈦確實具有較高的硬度及機械性質，相較於純鈦具有較低之降低彈性係數，有利於後續加工製程之進行。其中，另加入鉑、鈀及鉭係能於Ti-Cu-Sn鈦合金組成物表面形成一層氧化物保護膜，進而增加Ti-Cu-Sn鈦合金組成物的耐蝕性，並會提高Ti-Cu-Sn鈦合金組成物之硬度及機械性質。It can be seen from Table 1 that the Ti-Cu-Sn titanium alloy composition of the present invention has a relatively dense crystal phase as described above, and therefore has higher hardness and mechanical properties than conventional pure titanium, compared with pure titanium. It has a lower coefficient of elasticity, which is beneficial to the subsequent processing. Among them, the addition of platinum, palladium and lanthanum can form an oxide protective film on the surface of the Ti-Cu-Sn titanium alloy composition, thereby increasing the corrosion resistance of the Ti-Cu-Sn titanium alloy composition and increasing Ti-Cu. -Sn titanium alloy composition hardness and mechanical properties.
綜上所述，本發明之Ti-Cu-Sn鈦合金組成物透過前述製程，可藉由銅及錫共同添加所形成的二次變相，使鈦合金具有固溶強化、析出強化等強化機構，可促使由添加銅金屬所析出之Ti2 Cu介金屬成長為近似奈米級的晶相，因此可進一步強化鈦合金之整體硬度及強度，有利於後續之切削加工，提升該組成物的加工性，進而減緩切削刀具之磨損。As described above, the Ti-Cu-Sn titanium alloy composition of the present invention can pass through the above-mentioned process, and the secondary alloy formed by the addition of copper and tin can be used to strengthen the titanium alloy by solid solution strengthening and precipitation strengthening. The Ti 2 Cu intermetallic precipitated by the addition of copper metal can be promoted to a crystal phase of approximately nanometer order, thereby further strengthening the overall hardness and strength of the titanium alloy, facilitating subsequent cutting processing and improving the processability of the composition. , thereby slowing the wear of the cutting tool.
本案之Ti-Cu-Sn鈦合金組成物透過添加該銅與錫之成分可於凝固過程中與鈦形成穩定介金屬相，同時可降低整體鈦合金之熔點，因此可減緩氧化速率。The Ti-Cu-Sn titanium alloy composition of the present invention can form a stable intermetallic phase with titanium during solidification by adding the copper and tin components, and at the same time reduce the melting point of the whole titanium alloy, thereby slowing down the oxidation rate.
本案之Ti-Cu-Sn鈦合金組成物具有良好生物相容性且無細胞毒性，因此可應用於生醫材料。例如本案實施例係以該鈦、銅及錫的組成成份製作支台齒，使得該支台齒具有較佳的生物相容性且不會釋出對人體有害的毒性，藉以達到耐磨損及耐酸蝕等的功效。The Ti-Cu-Sn titanium alloy composition of the present invention has good biocompatibility and is non-cytotoxic, and thus can be applied to biomedical materials. For example, in the embodiment of the present invention, the abutment teeth are made of the titanium, copper and tin components, so that the abutment teeth have better biocompatibility and do not release harmful toxicity to the human body, thereby achieving wear resistance and Resistance to acid corrosion, etc.
雖然本發明已利用上述較佳實施例揭示，然其並非用以限定本發明，任何熟習此技藝者在不脫離本發明之精神和範圍之內，相對上述實施例進行各種更動與修改仍屬本發明所保護之技術範疇，因此本發明之保護範圍當視後附之申請專利範圍所界定者為準。While the invention has been described in connection with the preferred embodiments described above, it is not intended to limit the scope of the invention. The technical scope of the invention is protected, and therefore the scope of the invention is defined by the scope of the appended claims.
第1a圖：本發明Ti-Cu-Sn鈦合金組成物之微組織結構之光學顯微圖。Fig. 1a is an optical micrograph of the microstructure of the Ti-Cu-Sn titanium alloy composition of the present invention.
第1b圖：本發明Ti-Cu-Sn鈦合金組成物之微組織結構之掃描式電子顯微圖。Fig. 1b is a scanning electron micrograph of the microstructure of the Ti-Cu-Sn titanium alloy composition of the present invention.
第2a圖：本發明Ti-Cu-Sn鈦合金組成物之微組織結構之光學顯微圖又一。Fig. 2a is a view showing an optical micrograph of the microstructure of the Ti-Cu-Sn titanium alloy composition of the present invention.
第2b圖：本發明Ti-Cu-Sn鈦合金組成物之微組織結構之掃描式電子顯微圖又一。Figure 2b: Scanning electron micrograph of the microstructure of the Ti-Cu-Sn titanium alloy composition of the present invention.
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