Simulating mechanism at the atomic-scale for atomically precise deposition and etching
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1 SEMICON TechArena session on Advanced Materials 14 November 2017 Simulating mechanism at the atomic-scale for atomically precise deposition and etching Simon D. Elliott & Ekaterina
2 Outline Area-selective deposition of Si-based materials Mechanism of thermal ALE using F + Sn(acac) 2 2
3 Area-selective deposition of Si-based materials
4 Investigating routes towards the ALD of SiC
5 SiC thin film applications CVD/PECVD is unable to meet increasingly stringent conformality requirements in nanoelectronics fabrication. No known low temperature ALD process is suitable for highvolume manufacturing. SiC properties: Excellent barrier Low-k = 6-7 Low wet etch rate SiC applications: Si C 5
6 Do these precursors adsorb onto an SiC surface? Si 2 6 Si 4 Si 3 Cl C 2 2 CCl 4 CCl 3 DFT using VASP: PAW for core electrons, plane wave basis set to 400 ev cut-off for valence electrons, 8Å vacuum, slab 4 Si-C repeat units thick, 2x2x1 Monkhorst-Pack k-points.
7 Do these precursors adsorb spontaneously on -terminated SiC surface? Si 2 6 Si 4 Si 3 Cl C 2 2 (011) -SiC side view Cl Si C CCl 4 CCl 3 7
8 Do these precursors adsorb spontaneously on bare SiC surface with dangling bonds? Si 2 6 Si 4 Si 3 Cl C 2 2 Cl Si C CCl 4 CCl 3 (011) bare SiC side view 8
9 Adsorption of Si precursors on bare SiC Top view Side view silicon tetrachloride (SiCl 4 ) E ads = -1.8 ev disilane (Si 2 6 ) E ads = -4.3 ev Cl Si C silane (Si 4 ) E ads = -2.5eV 9
10 Adsorption of C precursors on bare SiC Top view Side view trichloromethane (CCl 3 ) E ads = -2.8 ev ethyne (C 2 2 ) E ads = -3.2 ev Cl Si C carbontetrachloride (CCl 4 ) E ads = -1.9 ev 10
11 All precursors adsorb spontaneously on bare surface, not on -terminated one disilane (Si 2 6 ) E ads = -4.3 ev Cl Si C ethyne (C 2 2 ) E ads = -3.2 ev 11
12 Kinetics of silane plasma reaction with -terminated SiC (011) -SiC Side view silyl (Si 3 ) silylene (Si 2 ) (011) -SiC Top view Cl Si C 12
13 Energy Kinetics of silane plasma reaction with -terminated SiC TS E a Reaction pathway Si C R - reactants TS - transition state P - products E a - activation energy 13
14 Kinetics of Si 3 with -SiC I R Si Si I Si R Si C Si (0 1 1) -SiC Si Si C Si (0 1 1) -SiC C 14
15 Kinetics of Si 2 with -SiC I I R Si Si C Si (0 1 1) -SiC Si C Si (0 1 1) -SiC C 15
16 Projected density of states Electronic structure of Si 2 with Si- orbitals in molecular model of R Si 2 I surface states on atom at Si- surface I At R: localisation of charge on surface when polarised by incoming Si 2 R TS P band energy, ev
17 Summary of silane PECVD onto SiC Both silyl and silylene show selectivity towards insertion into the Si- bond, rather than the C- bond Si - C - This reaction is not self-limiting and therefore it is not an ALD process 17
18 Outline Area-selective deposition of Si-based materials Mechanism of thermal ALE using F + Sn(acac) 2 18
19 Thermal ALE processes to date S. George, Y. Lee & co-workers, Univ. Colorado: Al 2 O 3 with Sn(acac) 2 or Al(C 3 ) 3 ZrO 2 fo 2 ZnO via Al 2 O 3 ( conversion-etch ) These authors have also estimated thermodynamics of etching of GaN, InP, ZnS, GaAs, PbSe, CdTe using fluorinating agents F, SF 6, SF 4, ClF 3, NF 3, XeF 2 and F 2 and ligand exchange with -diketonate, alkyl, halide, cyclopentadienyl, silylamide, alkoxide and amidinate. 19 S. M. George & Y. Lee, ACS Nano. 2016, 10, , DOI: /acsnano.6b02991
20 Thermal ALE processes to date S. George, Y. Lee & co-workers, Univ. Colorado: Al 2 O 3 with Sn(acac) 2 or Al(C 3 ) 3 ZrO 2 fo 2 ZnO via Al 2 O 3 ( conversion-etch ) These authors have also estimated thermodynamics of etching of GaN, InP, ZnS, GaAs, PbSe, CdTe using fluorinating agents F, SF 6, SF 4, ClF 3, NF 3, XeF 2 and F 2 and ligand exchange with -diketonate, alkyl, halide, cyclopentadienyl, silylamide, alkoxide and amidinate. 20 S. M. George & Y. Lee, ACS Nano. 2016, 10, , DOI: /acsnano.6b02991
21 Schematic of proposed surface chemistry for Al 2 O 3 ALE showing (a) Sn(acac) 2 reaction and (b) F reaction. Published in: Younghee Lee; Jaime W. DuMont; Steven M. George; Chem. Mater. 2015, 27, DOI: /acs.chemmater.5b00300 Copyright 2015 American Chemical Society
22 ALE cycle F (g) Al 2 O 3 2 O (g) Al(acac) 3 (g) + Sn(acac)F (g) AlF 3 Al 2 O 3 Sn(acac) 2 (g) Mechanism proposed by Y. Lee; J. W. DuMont & S. M. George, Chem. Mater. 27, (2015).
23 ALE cycle F (g) AlF 3 Al 2 O 3 2 O (g) Al(acac) 3 (g) + Sn(acac)F (g) AlF 3 Al 2 O 3 Sn(acac) 2 (g) Mechanism proposed by Y. Lee; J. W. DuMont & S. M. George, Chem. Mater. 27, (2015).
24 ALE cycle 6 F (g) AlF 3 Al 2 O O (g) 2 Al(acac) 3 (g)? + 6 Sn(acac)F (g)? AlF 3 Al 2 O 3 6 Sn(acac) 2 (g) Mechanism proposed by Y. Lee; J. W. DuMont & S. M. George, Chem. Mater. 27, (2015).
25 ALE cycle F (g) AlF 3 Al 2 O 3 Al(acac) 3 (g) + Sn(acac)F (g) QUESTIONS ON MECANISM: AlF 3 Al 2 O 3 Sn(acac) 2 (g) 2 O (g) Are the proposed by-products thermodynamically favoured & kinetically accessible? Are other by-products possible? Are the reactions self-limiting? ow do the reagents adsorb? Can the measured coverage of fragments be rationalised? Mechanism proposed by Y. Lee; J. W. DuMont & S. M. George, Chem. Mater. 27, (2015).
26 Density functional theory calculations of the mechanism of F adsorption onto Al 2 O 3 26
27 Bare Al 2 O 3 surface 1x4 cell has surface area = 1.65 nm 2 (-2 1 0) surface of -Al 2 O 3 computed surface energy=1.3 J.m -2 (-2 1 0) (-2 1 0) Al O -Al 2 O 3 coordinates from G. Fomengia, RAPID project.
28 Adsorption of F onto surface (-2 1 0) Al O F
29 Adsorption of F onto surface Introduce F molecules to bare Al 2 O 3 surface: approach via -bonding of to surface-o followed by spontaneous dissociation into -O- and -Al-F F Al O (-2 1 0) Al O F
30 Adsorption of F onto surface Computed eight (-2 1 0) cells with F coverage ranging 2-11 F.nm -2 Shown here is (F) = 18 F/cell = 10.9 F.nm -2 F -Al-F -O- (-2 1 0) Al O F Density functional calculations using VASP program with PBE functional, plane waves, PAW cores and sparse k-point set. Geometry optimisation with bottom face of slab fixed.
31 Adsorption of F onto surface Computed eight (-2 1 0) cells with F coverage ranging 2-11 F.nm -2 Shown here is (F) = 18 F/cell = 10.9 F.nm -2 F -Al-F -O- (-2 1 0) Average adsorption energy E ads = -1.2 ev/f E ads = -1.1 ev for -bonding of molecular F E ads = -2.1 ev for dissociative adsorption into O- + Al-F Al O F Multi-layers of molecular F
32 Adsorption of F onto surface Computed five (1 0 0) cells with F coverage ranging 6-18 F.nm -2 Shown here is (F) = 6 F/cell = 9.2 F.nm -2 F -Al-F -O- Al O F (1 0 0) Average adsorption energy E ads = -1.5 ev/f E ads = -1.1 ev for -bonding of molecular F E ads = -2.2 ev for dissociative adsorption into O- + Al-F
33 2 O by-product -O 2 Molecular 2 O can form spontaneously (1 0 0) Compute E des =+0.2 to +0.8 ev/ 2 O < T S des =1.0 ev/ 2 O at 250 C 2 O can desorb But some O may persist at surface? Possible reaction O + acac acac (g) + oxide growth? Al O F
34 AlF x by-product or saturating layer? -Al-F Driving force towards Al-F bonds but not AlF 3 molecules. (1 0 0) -AlF 2 -Al-F-Al- -Al-F-Al- -Al-F Al O F (-2 1 0)
35 AlF x by-product or saturating layer? -Al-F-Al- -Al-F Driving force towards Al-F bonds but not AlF 3 molecules. (1 0 0) Compute E des (AlF 3 )= +4.4 ev/alf 3 >> T S des no desorption of AlF 3 (Al 2 F 6 dimer is 2 ev more stable still not enough to allow desorption). This means that the surface coating of AlF x prevents further adsorption of F Self-limiting etch reaction by F A co-reagent is therefore needed to remove residual F and Al from the surface, i.e. Sn(acac) 2.
36 Coverage of F and etch rate Excluding molecular F, maximum computed coverage of dissociated F in large (-2 1 0) cell is sat (F) = F.nm -2. Assume dissociated F is the self-limiting intermediate. Assume that residual O does not combine with acac in ALD-like reaction. Instead, assume that 2 O is the only O product. Al 2 O 3 :F = 1:6 ence maximum Al 2 O 3 etched per cycle is (etch) = -1/6. sat (F) = Al 2 O 3.nm -2 = Al 2 O 3.cm -2 = ng.cm -2. Experimentally S. George reports ng.cm -2.cycle -1 at 250 C and 1.5 Torr. Computed coverage is consistent with experiment.
37 Adsorption of Sn(acac) 2 onto surface DFT calculations show no spontaneous Sn F interaction Barrier exists towards adsorption / ligand exchange acac acac Sn: F Al (-2 1 0) Can derive overall thermodynamics ( E) for this pulse without computing constituent reaction steps for ligand exchange. Al O F
38 Ligand exchange by-products E at T=0 K (ev/al 2 O 3 ) for F pulse, Sn pulse and entire cycle Possible etch reactions Cl Br I Al 2 O 3 +6F+6Sn(acac) 2 2Al(acac) 3 +6Sn(acac)F+3 2 O Al 2 O 3 +6F+2Sn(acac) 2 2Al(acac)F 2 +2Sn(acac)F+3 2 O F pulse entire cycle Sn Pulse Al 2 O 3 +6F+Sn(acac) 2 2Al(acac)F 2 +SnF O Both pulses should show favourable thermodynamics in order for the entire ALE process to be viable.
39 Ligand exchange by-products E at T=0 K (ev/al 2 O 3 ) for F pulse, Sn pulse and entire cycle Possible etch reactions Cl Br I Al 2 O 3 +6F+6Sn(acac) 2 2Al(acac) 3 +6Sn(acac)F+3 2 O Al 2 O 3 +6F+2Sn(acac) 2 2Al(acac)F 2 +2Sn(acac)F+3 2 O Al 2 O 3 +6F+Sn(acac) 2 2Al(acac)F 2 +SnF O Most thermodynamically favourable to fully exchange three acac to Al Statistically more likely to just exchange one acac to Al and one F to Sn Unfavourable to donate two F to Sn Al(acac)F 2 and Sn(acac)F are the most likely by-products. alogenated (-2 1 0) surface with 3.6 X/nm 2 at end of X pulse used as basis for E per pulse.
40 ALE cycle 6 F (g) AlF 3 Al 2 O O (g) 2 Al(acac)F 2 (g) + 2 Sn(acac)F (g) AlF 3 Al 2 O 3 2 Sn(acac) 2 (g)
41 Effect of entropy on etching E at T=0 K (ev/al 2 O 3 ) for F pulse, Sn pulse and entire cycle Possible etch reactions Cl Br I Al 2 O 3 +6F+6Sn(acac) 2 2Al(acac) 3 +6Sn(acac)F+3 2 O Al 2 O 3 +6F+2Sn(acac) 2 2Al(acac)F 2 +2Sn(acac)F+3 2 O Al 2 O 3 +6F+Sn(acac) 2 2Al(acac)F 2 +SnF O alogenated (-2 1 0) surface with 3.6 X/nm 2 at end of X pulse used as basis for E per pulse.
42 Effect of entropy on etching Possible etch reactions Cl Br I Al 2 O 3 +6F+6Sn(acac) 2 2Al(acac) 3 +6Sn(acac)F+3 2 O Al 2 O 3 +6F+2Sn(acac) 2 2Al(acac)F 2 +2Sn(acac)F+3 2 O Al 2 O 3 +6F+Sn(acac) 2 2Al(acac)F 2 +SnF O G at T=250 C, p=1.5 Torr (ev/al 2 O 3 ) for F pulse, Sn pulse and entire cycle The overall ALE energetics are relatively insensitive to temperature, but +0.4 the energetics of each pulse are affected strongly: F pulse deposits F entropy cost Sn pulse removes F entropy gain Temperature drives the Sn pulse via (i) entropy of by-products and (ii) thermally-activated ligand exchange reactions. alogenated (-2 1 0) surface with 3.6 F/nm 2 at end of F pulse used as basis for E per pulse. Calculation of S assumes entropy of solid surface and etched material is zero.
43 Etching other metal oxides 43
44 Various metal oxide substrates Overall E at T=0 K (ev/m 2 O n ) Etch reaction M 2 O n + 2nF + 2Sn(acac) 2 2M(acac)F n-1 + 2Sn(acac)F + n 2 O - rutile monocl. monocl. - rutile Al 2 O 3 TiO 2 ZrO 2 fo 2 SiO 2 SnO TiO 2 is the easiest to etch with F+Sn(acac) 2, followed by ZrO 2 =fo 2. Al 2 O 3 =SiO 2 are predicted to show similar overall thermodynamics. But S. George was not able to etch SiO 2 and suggested that this was due to strong Si-F resisting ligand exchange with co-reagent, i.e. E(co-reagent)>0. SnO 2 is the hardest to etch; maybe one of its constituent pulses will also have E(pulse)>0, preventing etching. 44
45 Various metal oxide substrates Overall E at T=0 K (ev/m 2 O n ) Etch reaction M 2 O n + 2nF + 2Sn(acac) 2 2M(acac)F n-1 + 2Sn(acac)F + n 2 O - rutile monocl. monocl. - rutile Al 2 O 3 TiO 2 ZrO 2 fo 2 SiO 2 SnO Saturating coverages, not thermodynamics, determine etch rates. S. George proposes that unreacted acac ligands block sites for fluorination and reduce etch rates. It is also possible that unreacted acac consume the protons from F that would otherwise etch away O as 2 O. Published in: Younghee Lee; Craig uffman; Steven M. George; Chem. Mater. 2016, 28, , DOI: /acs.chemmater.6b02543 Copyright 2016 American Chemical Society Film thickness versus number of F and Sn(acac) 2 reaction cycles at 200 C for a variety of materials. 45
46 Conclusions: mechanism of thermal ALE F pulse: Dissociation of F on the alumina surface is spontaneous and self-limiting, with desorption of 2 O as by-product. More thermodynamically favourable for TiO 2, ZrO 2 and fo 2. The saturating coverage of dissociated F gives an etch rate consistent with experiment. Sn(acac) 2 pulse: There is a kinetic barrier to adsorption and ligand exchange. Temperature drives the desorption of halogenated by-products. Most likely by-products are SnF(acac) and AlF 2 (acac).
47 Atomic-scale calculations can give mechanistic insights into surface chemistry of selectivearea PECVD and thermal ALE. 47
48 Tyndall National Institute, Lee Maltings, Dyke Parade, Cork, Ireland. T12 R5CP t: e: tyndall.ie
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