生物相容性鈦基金屬玻璃合金粉末用於積層製造之研製

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研究生：	李宗雄 Tsung-Hsiung Li
論文名稱：	生物相容性鈦基金屬玻璃合金粉末用於積層製造之研製 Development and fabrication of the bio-compatible Ti-based metallic glass powders for additive manufacturing
指導教授：	鄭憲清 Shian-Ching Jang
口試委員:
學位類別：	博士 Doctor
系所名稱：	工學院 - 材料科學與工程研究所 Graduate Institute of Materials Science & Engineering
論文出版年：	2019
畢業學年度：	107
語文別：	英文
論文頁數：	90
中文關鍵詞：	金屬玻璃、生物相容性、積層製造、鈦合金
外文關鍵詞：	metallic glass, bio-compatible, additive manufacturing, Ti alloy
相關次數：	點閱：17 下載：0
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為了達到利用氣體霧化方式來製作出具高真圓度的球形粉體，降低具生物相容性Ti42Zr40Ta3Si15的液相溫度是必須的，所以鈦合金低液相溫度的設計理念是傾向該合金成份是接近於共晶點。一系列的Ti-Zr-Ta-Si-Sn-Co合金系統，將利用熔體紡絲技術來製作出薄帶，並以差示掃描量熱來探究熱性質和X光繞射儀來鑑定非晶質狀態，而由差示掃描量熱的結果顯示，將以適當的Co和Sn元素含量來取代該合金組成中的Zr和Si，可大幅降低從1728 K的Ti42Zr40Ta3Si15液相溫度轉變成1200 K，同時該合金成份的玻璃形成能力也向上提升。依據四種不同液相溫度的合金成份，利用氣體霧化技術來製作出具金屬玻璃結構的粉體，其結果顯示，較低液相溫度的合金成份，容易經氣體霧化技術後，得到球形的金屬玻璃粉體。同樣的在雷射再燒熔測試，在適當燒熔參數下，使用部分結晶的Ti42Zr35Ta3Si5Sn2.5Co12.5進行SLM，可得到連續全非晶的平面顯微結構，這表示該合金成份與雷射參數可進一步進行得到層與層堆疊的非晶構造。因此Ti42Zr35Ta3Si5Sn2.5Co12.5相信這有潛力的合金系統，可以製作出具高真圓度的粉體來運用於SLM

In order to reduce the liquidus temperature of the bio-compatible Ti42Zr40Ta3Si15 alloy for fabrication the spherical powder by gas-atomization process, the concept of lower liquidus temperature tendency near eutectic alloy composition was applied to design the Ti-based alloy with lower liquidus temperature. A series of Ti-Zr-Ta-Si-Sn-Co alloy ribbons were prepared by melt-spinning for evaluating their thermal properties and amorphous state by using differential scanning calorimeter (DSC) and X-ray diffraction analysis (XRD), respectively. The DSC results show that the liquidus temperature of Ti42Zr40Ta3Si15 alloy can be dramatically decreased by adding suitable amount of Co and Sn to substitute Zr and Si contents, liquidus temperature decreases from 1728 K to 1200 K. Meanwhile, the glass forming ability is also significantly improved. Accordingly, three alloy compositions with different liquidus temperatures were selected for fabricating the metallic glass powders by gas- atomization. The results reveal that the lower liquidus temperature of the alloy has, the more tendency to form the spherical metallic glass powder by gas-atomization process. In parallel, the results of pulse laser re-melting test on the partially crystallized Ti42Zr35Ta3Si5Sn2.5Co12.5 alloy powder shows that a continuous fully amorphous alloy layer can be formed under proper laser re-melting condition. This implies that the Ti42Zr35Ta3Si5Sn2.5Co12.5 alloys which contain major microstructure of amorphous phase also can be formed a continuous fully amorphous alloy layer by laser re-melting. Therefore, Ti42Zr35Ta3Si5Sn2.5Co12.5 alloys are believed to be the promising alloy system and can be fabricated into spherical metallic glass powders for the application of additive manufacturing by selective laser melting method.

Table of Contents
摘要    I
Abstract    II
Acknowledgments    III
Table of Contents    IV
List of figures    VI
List of tables    IX
Explanation of Symbols    X
Chapter 1  Introduction    1
Chapter 2  Literature review    6
2.1 The characteristics of metallic glasses    6
2.2 Discovery of metallic glass    6
2.3 Glass-forming ability (GFA)    7
2.3.1 Component rule    8
2.3.2 Cluster unit    9
2.3.3 Deep eutectic point    10
2.3.4 Instability crystalline structure    11
2.4 Glass-forming ability index    13
2.4.1 Characteristic temperatures    13
2.4.2 Supercooled liquid region, ∆Tx=Tx -Tg    14
2.4.3 γ parameter    14
2.4.4 γm parameter    15
2.4.5 Reduce glass transformation temperature    15
2.5 Designing biocompatible for implant applications    15
2.5.1 Ti-based BMG for physical and chemical properties    16
2.5.2 Ti-based BMG for biological safety    18
2.5.3 Toxic element    18
2.5.4 The biological safety and GFA of alloying additions in Ti-based BMG    20
2.6 Open-cell bulk metallic glass foams (BMGFs)    22
2.7 Processing biomedical implant by additive manufacturing (AM)    22
2.7.1 Additive manufacturing (AM)    23
2.7.2 SLM of high cooling rate    24
2.7.3 SLM of hot tearing cracks    25
2.7.4 SLM of heat affect zone (HAZ)    26
2.7.5 Interaction between laser and metal powder beds    27
2.8 Processing metallic glasses by SLM    28
Chapter 3  Experimental procedures    29
3.1 Biocompatible Ti-based metallic glass with high GFA    29
3.2 Powder materials    30
3.3 SLM    30
Chapter 4  Results and discussion    31
4.1 Optimization of Ti-(Zr, Co, Sn)-Ta-(Si, P, B) amorphous alloy    31
4.1.1 Ti-Ta-(Zr, Si, Co) systems    31
4.1.2 Ti-Zr-Ta-(Si, Sn) systems    32
4.1.3 Ti-Zr-Ta-Co-(Si, B, P) and Ti-Zr-Ta-Sn-(Si, B, P) systems    32
4.1.4 Ti-Zr-Ta-(Co, Sn)-Si systems    33
4.2 real Tg    33
4.2.1 DSC curve of TiZr-based MG    34
4.2.2 Microstructure of Tg point    35
4.2.3 Reduce free volume    36
4.2.4 Kohlraush-Williams-Watts (KWW) relaxation function    36
4.2.5 Activation energy for structural relaxation    37
4.2.6 Incubation time    38
4.2.7 Other TiZr-based MG systems    39
4.3 Gas atomization process    39
4.4    Laser remelting-Line    41
Chapter 5  Conclusions    42
5.1 Biocompatible Ti-Zr-Ta-Si-Sn-Co with high GFA    42
5.2 Identify real Tg    42
References    43

List of figures
Figure 1. Illustration of biomedical implants and devices made out of BMGs. (a) commercial martensitic steel surgical blade coated with Zr53Cu30Ni9Al8 BMG film (top) and Zr53Cu30Ni9Al8 BMG surgical lade (down), (b) BMG medical stapling anvils, (c) open-cell BMG foams implant. [Maker: NCU HPAL Lab.]    53
Figure 2. Mechanisms for the multicomponent alloys which satisfy the three empirical rules.    53
Figure 3. Schematic illustrations of the structural features of cluster unit of glassy alloys.    53
Figure 4. DSC curves of of the Cu41.5Zr42Al8Ag8Si0.5 BMG with a diameter of 4 mm.    54
Figure 5. Schematic T-T-T curves for two different alloys. Cooling rate: Rc2 > Rc1    54
Figure 6. The atomic arrangements of (a) crystal of long-range order and (b) amorphous of short-range order.    54
Figure 7. Human bone structure.    55
Figure 8. Illustration of an AM (a) powder bed system, (b) wire feed system, and (c) powder feed system.    55
Figure 9. Tensile engineering stress-strain curves, two different types of SLM machines were used and named as ‘Concept’ and ‘Fraunhofer’, respectively.    55
Figure 10. AM of metal alloys via selective laser melting. (a, c) Many alloys including Al7075 tend to solidify by columnar growth of dendrites in the strong temperature gradient process, resulting in cracks due to solidification shrinkage. (b, d) Suitable nanoparticles can induce heterogeneous nucleation and facilitate equiaxed grain growth, thereby reducing the effect of solidification strain.    56
Figure 11. Thermal profile of a single layer of Ti-6Al-4V during AM.    56
Figure 12. (a) Optical micrographs of the solidified melt track within a powder layer, (b) Schematic depicting the action of evaporated metal flux on the flow pattern of the surrounding Ar gas and displacement of particles in the powder bed.    56
Figure 13. The formation mechanism of denudation zone.    57
Figure 14. A time series of track cross sections for a fixed position with the laser moving out of the plane. It can divide into the indentation formation, the indentation collapse, formation of a pore, and the cooling as the melt solidifies.    57
Figure 15. High-speed images of spattering with schematic illustration of spatter formation [120].    58
Figure 16. Composition dependence of (a-1) liquidus temperature, Tl and (a-2) supercooled liquid region, ∆Tx for Ti42ZrwTa3SixCoz quinary alloys, (b-1) Tl and (b-2) ∆Tx for Ti42ZrwTa3SixSny quinary alloys. C and N marker in the circle index the crystal and nanocrystal for microstructure ribbon at the same experiment parameter, respectively.    58
Figure 17. HT-DSC (a) and DSC (b) curves for Ti42Zr35Ta3Si5SnyCoz. (y+z=15 in at %) glassy alloy ribbons, respectively.    59
Figure 18. DSC trace scanned at 0.67 K/s of (A) the Ti42Zr35Ta3Si5Sn2.5Co12.5 as-quench alloy ribbon with a thickness of 25 μm, (B) the sample is reheated again, (C) is difference in heat flow signals between the (A) and (B).    59
Figure 19. (a) XRD of the isothermal annealed Ti42Zr35Ta3Si5Sn2.5Co12.5 alloy ribbons (Holding time = 3 min), (b) bright field TEM image and selected area diffraction pattern of the sample annealed at 761 K (top of first peak) for 3 min.    59
Figure 20. DSC plots of the Ti42Zr35Ta3Si5Sn2.5Co12.5 alloy ribbons annealed at different annealing conditions; DSC heating rate is 0.67 K/s.    60
Figure 21. (a) Variation of the enthalpy difference with the annealing time in isothermal annealing (713 K) and (b) KWW-exponent β in the vicinity of first peak for the Ti42Zr35Ta3Si5Sn2.5Co12.5 alloy ribbon.    60
Figure 22. The activation energy of cooperative motion of cluster estimated by Arrhenius plots as a function of temperature for the Ti42Zr35Ta3Si5Sn2.5Co12.5 alloy ribbon.    60
Figure 23. (a) Incubation time as a function of isothermal annealing temperature and (b) real Tg at heating rate of 0 K/min for the Ti42Zr35Ta3Si5Sn2.5Co12.5 alloy ribbon.    61
Figure 24. DSC plots of as-quench TiZr-based metallic glass ribbon with a thickness of 25 μm.    61
Figure 25. The morphologies of atomized alloy powder observed by SEM; (a) Ti42Zr40Ta3Si7.5Sn7.5, (b) Ti42Zr32.5Ta3Si7.5Co15, (c) Ti42Zr35Ta3Si5Sn7.5Co7.5 and (d) Ti42Zr35Ta3Si5Sn2.5Co12.5.    62
Figure 26. Cross-sectional metallographs of the atomized Ti42Zr35Ta3Si5Sn2.5Co12.5 alloy powder.    62
Figure 27. Plots of particle size distribution of as-atomized Ti-based alloy powders; (a) Ti42Zr40Ta3Si7.5Sn7.5, (b) Ti42Zr32.5Ta3Si7.5Co15, (c) Ti42Zr35Ta3Si5Sn7.5Co7.5 and (d) Ti42Zr35Ta3Si5Sn2.5Co12.5.    63
Figure 28. XRD patterns of atomized alloy powders for different particle size range; (a) Ti42Zr40Ta3Si7.5Sn7.5, (b) Ti42Zr32.5Ta3Si7.5Co15, (c) Ti42Zr35Ta3Si5Sn7.5Co7.5 and (d) Ti42Zr35Ta3Si5Sn2.5Co12.5, (e) four kind of alloy ribbons with thickness 50 um    64
Figure 29. DSC curves of gas-atomized powders with different size and ribbon (Ti42Zr35Ta3Si5Sn2.5Co12.5).    64
Figure 30. SEM images of the alloy lines formed after laser re-melting at different beam size (a) 100 um, (b) 200 um for Ti42Zr35Ta3Si5Sn2.5Co12.5.    65

List of tables
Table I. Summary of biomedical Ti-based BMG systems and their mechanical properties.    66
Table II. Summary of metal-based BMG systems.    66
Table III. Selected alloys commercially used in AM processing.    66
Table IV. Thermal parameters of the Ti-Zr-Ta-Si-Co metallic glasses.    67
Table V. Thermal parameters of the Ti-Zr-Ta-Si-Sn metallic glasses.    68
Table VI. Thermal parameters of the Ti-Zr-Ta-(Co, Sn)-(Si, B, P) metallic glasses.    69
Table VII. Thermal parameters of the Ti-Zr-Ta-Co-Sn-Si metallic glasses.    70
Table VIII. Parameters according to the KWW relaxation function fitted to data with τ and β.    72
Table IX. Thermal properties of TiZr-based metallic glass alloy ribbon.    72
Table X. Alloy line formation and line width by a function of power and scanning speed for beam size 200μm.    73
Table XI. Alloy line formation and line width by a function of power and scanning speed for beam size 100μm.    74
 

                                

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