模板效應對磁控濺鍍之氮化釩薄膜織構演變之影響

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研究生：	蘇禹徹 Su, Yu-Che
論文名稱：	模板效應對磁控濺鍍之氮化釩薄膜織構演變之影響 Template Effect on Texture Evolution of VN Thin Films Deposited by Unbalanced Magnetron Sputtering
指導教授：	黃嘉宏 Huang, Jia-Hong 喻冀平 Yu, Ge-Ping
口試委員:	李志偉 Lee, Jyh-Wei 呂福興 Lu, Fu-Hsing
學位類別：	碩士 Master
系所名稱：	原子科學院 - 工程與系統科學系 Department of Engineering and System Science
論文出版年：	2018
畢業學年度：	106
語文別：	英文
論文頁數：	81
中文關鍵詞：	氮化釩、介層、模板、織構
外文關鍵詞：	Vanadium, Nitride, Texture, Template
相關次數：	點閱：2 下載：0
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本研究目的是探討不同模板(釩和鈦)對於非平衡磁控濺鍍之氮化釩薄膜織構演變及其性質的影響。基本的構想是希望藉由織構為(0002)的鈦模板來改善具有(111)織構之氮化釩的微結構，並使其從zone-1結構變成較緻密之zone-T結構，進一步改善其機械性質。另一方面，由於釩晶體結構的(110)面與氮化釩的(200)面相似，所以釩模板或許可以使氮化釩薄膜之(200)面長得更好，並優化其性質。本研究利用平衡磁控濺鍍製備氮化釩試片。試片分成兩部分，第一部分試片的鍍膜參數為300℃、-70 V基板偏壓、氮流量由1.5 至 3.5 sccm；第二部分試片鍍製於室溫下且無基板偏壓，氮流量控制在12 sccm。每個參數條件的氮化釩薄膜皆分別鍍製單層、與在鈦及釩模板上。鍍膜後，測量其織構係數及薄膜性質。然而實驗結果卻與原先預期相反，鈦模板及釩模板皆可以提升氮化釩薄膜之(111)織構，而且微結構緻密程度隨著(111)織構增加而下降。釩模板提升氮化釩(111)織構的機制可能是藉由釩膜板讓氮化釩(200)面長得更好更平滑，進而使氮化釩(200)面上的吸附原子能遷移到(111)面上，而促進(111)織構成長。鈦模板僅能在高氮流量且低鍍率下透過局部磊晶的效果提升(111)織構。在性質方面，硬度及殘留應力皆隨(111)織構增加而下降，可能是氮化釩本質上偏好長(200)面，所以成長較不偏好的(111)織構會使結構變得較為鬆散，導致硬度及殘留應力下降。此外，鈦模板對氮化釩織構與性質的優化不如鈦模板對氮化鈦顯著，因此鈦模板雖然可以促進氮化釩(111)織構成長，卻不能明顯改善其微結構，因而無法提升薄膜機械性質。實驗結果亦發現，第一部分氮化釩試片的電阻與結晶度及化學計量比有關，第二部分氮化釩試片電阻較高則與其較為鬆散的zone-1結構有關。

The purpose of this study was to investigate the effect of different templates (V and Ti) on the texture evolution and the accompanying properties of VN thin films. Ti (0002) template was used to change the microstructure of (111)-textured VN thin films from zone I to zone T, and further improving the mechanical properties of the films. In contrast, the atomic configuration of V(110) is similar to that of VN(200), and thus V (110) template may facilitate the formation of VN(200) texture and improve the properties of the VN films. VN thin films were deposited by unbalanced magnetron sputtering. Specimens were divided in two groups, group I specimens were deposited with nitrogen flow rates ranging from 1.5 to 3.5 sccm and substrate bias of -70V at 300℃, and group II specimens were deposited at room temperature with a fixed nitrogen flow rate of 12 sccm and without bias. Each group contained single layer VN, VN with Ti template and with V template. After deposition, texture coefficient (TC) and film properties were measured. From the results, both Ti and V templates could enhance the growth of (111) texture, which was against the expected results, and the film structure became less dense with increasing TC(111). The enhancement of (111) texture by V template may be due to the formation of smooth VN(200) by the assistance of V template, which could not retard the migration of adatoms from (200) to (111), thus promoting the growth of (111) texture. On the other hand, Ti template only enhanced (111) texture by local epitaxy effect at low deposition rate and high nitrogen flow rate. Both hardness and residual stress of the VN films decreased with increasing TC(111), which should be resulted from less dense film structure caused by the unfavorable (111) texture. Unlike the case in introducing Ti template in TiN, using a Ti (0002) template may enhance the (111) texture but could not densify the (111) textured VN films and therefore could not improve the mechanical properties. Electrical resistivity of the VN films was related to crystallinity and stoichiometry of the group I specimens, while the high resistivity of the group II specimens was mainly due to the loose-packed zone-I structure.

致謝……………….……………………………………………………………………………i
摘要……………………………………………………………………………………………ii
Abstract………………………………………………………………………………….…...iii
Content……………………………………………………………………………………….iv
List of Figures………………………………………………………………………...…….viii
List of Tables………………………………………........................………………….….…...x
Chapter 1  Introduction…………………….........................................................................1
Chapter 2  Literature Review………………………………………………………………3
2.1 Deposition Method…………………………………………………………………...3
2.2 Structure Zone Models…………………………………………………………….…3
2.3 Characteristics of VN………………………………………………………………...6
2.4 Superior Properties of VN……………………………………………………………8
2.5 Theories of Texture evolution for TMeN thin films…………………………….……9
2.5.1 Overall Energy Theory………………………………………................……..9
2.5.2 Competitive Growth Theory……………….....................................................9
2.6 Effects of Process Parameters on the Texture and Crystal Structure of
VN Thin films…………………………………………………………….………...11
2.7 Effect of Template…………………………………………………………………..12
2.8 Effect of Texture on Mechanical Properties………………………………………...14
2.8.1 Hardness………………………………………………………………….….14
2.8.2 Residual Stress………………………………………………………………15
2.8.3 Fracture toughness…………………………………………….……………..15
Chapter 3  Experimental Details……………………………………………………….…16
3.1 Specimen Preparation and Deposition Process……………………………………...16
3.2 Characterization of Composition and Film Structure………………………………..20
3.2.1 Chemical Composition……………………………………………………....20
3.2.2 Crystal Structure and Preferred Orientation……………………………...…..21
3.2.3 Cross-sectional Microstructure and Plan-View Morphology…………….…..22
3.2.4 Surface Roughness and Morphology………………………………....…...…23
3.3 Characterization of Film Properties………………………………………....………23
3.3.1 Hardness and Elastic Constant………………………………………….……23
3.3.2 Residual Stress…………………………………………………………….....24
3.3.3 Electrical Resistivity……………………………………………...............….26
3.3.4 Coloration……………………………………………………………………28
Chapter 4  Results…………………………………………….………..…….…29
4.1 Chemical Composition and Structure…………………………………………….…29
4.1.1 Chemical compositions………………………………………………………29
4.1.2 Cross-Sectional Microstructure and Surface Morphology…………………...35
4.1.3 Crystal Structure and Texture Evolution……………………………………..38
4.1.4 Surface Roughness………………………………...…………………………44
4.2 Properties……………………………………………………………………………45
4.2.1 Hardness and Elastic Constant……………………………………………….45
4.2.2 Residual Stress……………………………………………………………….47
4.2.3 Electrical Resistivity…………………………………………………………49
4.2.4 Coloration……………………………………………………………………51
Chapter 5  Discussion……………………………………………..……………………….52
5.1 Template Effect on Texture Evolution of VN Thin Films……………………....……52
5.1.1 Ti Template…………………………………………………………………..52
5.1.2 V Template…………………………………………………………………...56
5.2 Microstructure and Surface Morphology……………………………………………57
5.3 Effect of Template and Texture on Mechanical and Electrical Properties……………58
5.3.1 Hardness……………………………………………………………………..58
5.3.2 Residual Stress……………………………………………………………….60
5.3.3 Electrical Resistivity…………………………………………………………60
Chapter 6  Conclusions…………………………………………………………………....62
Reference…………………………………………………………………………………….63
Appendix A XPS spectra peaks integration results…………………….....………………71
Appendix B X-ray residual stress results………………………………………………….80



















List of Figures
Fig. 1.1 (a) The atomic configuration of BCC(110) plane and NaCl (200) plane. (b) The atomic configuration of HCP (0002) plane and NaCl (111) plane…………………………………….3
Fig. 2.1 (a) SZM for thick evaporated metal coatings proposed by Movchan and Demchishin [23], and (b) SZM for sputtered metal coatings modified by Thornton [24]………… ....……5
Fig. 2.2 (a) SZM for RF sputtered coatings modified by Messier et al., by replacing the axe from argon pressure with substrate bias [25], and (b) SZM with generalized parameters modified by Anders [28] ………………………………………….…………...…...……….…6
Fig. 2.3 The V-N phase diagram[29]……………………………………………………......….7
Fig. 2.4 The crystal structure of VN………………………………………………...……….....7
Fig. 3.1 The schematic diagram of UBMS system……………………………………………17
Fig. 3.2 The flowchart of experimental procedures…………………………………………..18　
Fig. 3.3 Schematic diagram of laser curvature measurement apparatus …………………..….25
Fig. 3.4 Schematic diagram of four point probe…..………………………………………….26
Fig. 3.5 The schematic diagram of color space with L* a* and b* coordinates [68]…………..28
Fig. 4.1 AES depth profiles for specimens (a)VT3, (b)VV3, (c)VVR, and (d)VR. The compositions were calibrated by XPS and the depth was calibrated by the corresponding SEM image…………………………………………………………………………………………34
Fig. 4.2 SEM cross-sectional images of specimens V1, V2,V3, and VR…………....….……..36.
Fig. 4.3 SEM cross-sectional images of specimens VT1, VT2, VT3, and VTR……….…..…36
Fig. 4.4 SEM cross-sectional images of specimens VV1, VV2, VV3, and VVR……..…........36
Fig. 4.5 SEM surface morphology of specimens V1, V2, V3, and VR……………………....37
Fig. 4.6 SEM surface morphology of specimens VT1, VT2, VT3, and VTR…………………37
Fig. 4.7 SEM surface morphology of specimens VV1, VV2, VV3, and VVR………………..37
Fig. 4.8 The XRD patterns of (a) single-layer VN, and VN films with (b) Ti and (c) V templates……………………………………………………………………………………...40
Fig. 4.9 The texture evolution of the first group specimens VN with increasing nitrogen flow rats from 1.5 to 3.5 sccm………………………………………………..…………...…….....41
Fig. 4.10 Texture coefficient of (a)1-, (b)2-, (c)3-, and (d) R-series VN specimens……....…42
Fig. 4.11 The GIXRD patterns of (a) single layer VN, and VN films with (b) Ti and (c) V templates……………………………………………………………………………………...43
Fig. 4.12 The AFM images of Single layer VN……………………………………………….44
Fig. 4.13 The AFM images of VN with Ti template…………………………………………..44
Fig. 4.14 The AFM images of VN with V template…………………………..……….………44
Fig. 4.15 Hardness of (a)1-, (b)2-, (c)3-, and (d) R-series VN specimens………….…….…..46
Fig. 4.16 Hardness vs (111) texture coefficient of VN specimens…………………..…….….46
Fig. 4.17 Residual stress of (a)1-, (b)2-, (c)3-, and (d) R-series VN specimens……………...48
Fig. 4.18 The variation of residual stress with (111) texture coefficient for the VN specimens…………………………………………………………………………………….48
Fig. 4.19 Electrical Resistivity of (a)1-, (b)2-, (c)3-, and (d) R-series VN specimens………50
Fig. 4.20 The variation of electrical resistivity with (111) texture coefficient for the VN specimens…………………………………………………………………………………….50
Fig. 5.1 Comparison flow chart of single layer VN and VN with Ti template…………….....53
Fig. 5.2 Deposition rates of 1-, 2-, 3- and R-series specimens………………………………...56
Fig. 5.3 The SEM cross-sectional images of VV2 and VV3……………………..…….……...60
Fig. A.1 XPS spectra peaks integration of (a) V-2p (b) N-1s (c) O-1s for specimen V1…….71
Fig. A.2 XPS spectra peaks integration of (a) V-2p (b) N-1s (c) O-1s for specimen V2………72
Fig. A.3 XPS spectra peaks integration of (a) V-2p (b) N-1s (c) O-1s for specimen V3………73
Fig. A.4 XPS spectra peaks integration of (a) V-2p (b) N-1s (c) O-1s for specimen VT1……..74
Fig. A.5 XPS spectra peaks integration of (a) V-2p (b) N-1s (c) O-1s for specimen VT2……..75
Fig. A.6 XPS spectra peaks integration of (a) V-2p (b) N-1s (c) O-1s for specimen VT3……..76
Fig. A.7 XPS spectra peaks integration of (a) V-2p (b) N-1s (c) O-1s for specimen VTR….....77
Fig. A.8 XPS spectra peaks integration of (a) V-2p (b) N-1s (c) O-1s for specimen VV1……78
Fig. A.9 XPS spectra peaks integration of (a) V-2p (b) N-1s (c) O-1s for specimen VV2……79
Fig. B.1 AXS method X-ray residual stress plot of specimen V1……………………………..80
Fig. B.2 AXS method X-ray residual stress plot of specimen V3……………………………81
Fig. B.3 AXS method X-ray residual stress plot of specimen VT1………………………........82

 
List of Tables
Table 2.1 Characteristics of VN……………………………………………………………….8
Table 3.1 The deposition condition of Ti and V templates…………………………………..18
Table 3.2 The deposition condition of VN films…………………………………………….19
Table 3.3 The designation of specimens and the corresponding deposition condition….…..19
Table 3.4 The binding energies of VN, 〖"VN" 〗_"-s" , "V" _"2"  "O" _"3" , 〖"VO" 〗_"2" , "V" _2 "O" _5 for "V-" "2" _"p" , "N-" "1" _"s" , "O-" "1" _"s" [52-56]…………………………………………………………………………….………..21
Table 3.5 The correction factor for different d/s and d/a ratios [65]........................................27
Table 4.1 Summary of thickness, chemical composition, texture coefficient, FWHM, grain size and lattice parameter of VN films………………………………………………….……31
Table 4.2 Summary of hardness, elastic constant, residual stress, electrical resistivity, and roughness of VN films…………………………………………………………………….....32

                                

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