Surface Chemistry of Copper Precursors
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1 Surface hemistry of opper Precursors in onnection with Atomic Layer Deposition (ALD) Processes Qiang Ma, Roy G. Gordon 1, and Dept. hemistry, University of alifornia, Riverside, A 92521, USA Phone: 1 (951) Fax: 1 (951) zaera@ucr.edu 1 Dept. hemistry, Harvard University ambridge, MA ALD International onference Boston, June 28,
2 Introduction Atomic Layer Deposition ALD: Separate chemistry into two self-limiting and complementary reactions for more control H H H2 H H H 2 H 2 H H H 2 H2 H H 2 H opper Acetamidinate: Promising ALD precursor F. Zaera, J. Mater. hem., 18, (2008). 2
3 Amidinate Thermal hemistry Stepwise Decomposition, TPD on 220 K Molecular desorption 300 K s But H (H3 )=H 405 K Additional dehydrogenation Acetonitrile, amido group? 480 K β-hydride elimination to butene Q. Ma, H. Guo, R. G. Gordon, F. Zaera, hem. Mater., 22(2), (2010). Q. Ma, H. Guo, R. G. Gordon, F. Zaera, hem. Mater. (2011). 3
4 Amidinate Thermal hemistry Dimer Dissociation upon Adsorption H 2 H 2 H H H H 2 H H 2 < 150 K Dissociative adsorption H2 H 2 H H Q. Ma, H. Guo, R. G. Gordon, F. Zaera, hem. Mater. (2011). 4
5 Amidinate Thermal hemistry First Bond Dissociation, T ~ 200 K H 2 H 2 H H bond scission 200 K 3 H 2 H H H H H Q. Ma, H. Guo, R. G. Gordon, F. Zaera, hem. Mater. (2011). 5
6 Amidinate Thermal hemistry -sec-butylacetamidine Formation Molecular Desorption -sec-butylacetamidine H 2 3 H 2 H H H H (ads) 300 K +H 310 K 3 H 2 H H H H H Q. Ma, H. Guo, R. G. Gordon, F. Zaera, hem. Mater. (2011). 6
7 Amidinate Thermal hemistry Reduction ev ev opper reduction occurs as -secbutylacetamide desorbs K ev ev Q. Ma, H. Guo, R. G. Gordon, F. Zaera, hem. Mater. (2011). 7
8 Amidinate Thermal hemistry High Temperature onversion, 1s and 1s XPS ev ev ev ev H H 2 H 400 K Acetonitrile H ev ev H = H M. Xu, H. Tiznado, B.-. Kang, M. Bouman, I. Lee, F. Zaera, J. Kor. Phys. Soc., 51(3), (2007). Q. Ma, H. Guo, R. G. Gordon, F. Zaera, hem. Mater. (2011). 8
9 Amidinate Thermal hemistry Butene Formation and Further Dehydrogenation Butene H=H H K 405 K Acetonitrile = H 2 H H Q. Ma, H. Guo, R. G. Gordon, F. Zaera, hem. Mater. (2011). 9
10 Amidinate Thermal hemistry Proposed Mechanism H 2 H 2 H H H H 2 H H 2 H2 H 2 H H Dissociative adsorption H 2 < 150 K (ads) Several intermediates form vs. T Some may desorb molecularly, but by ~ 480 K dehydrogenation is irreversible -sec butylacetamidine H 300 K H 2 H H 310 K K H K H H H H H ~500 K (ads) (ads) (ads) (?) = H 2 H 3 (?) 405 K Acetonitrile opper reduction (I) (0) Q. Ma, H. Guo, R. G. Gordon, F. Zaera, hem. Mater. (2011). Butene H=H 480 K H H 2 H 10
11 Amidinate Uptake Effect of Temperature and Hydrogen Fast and continuous uptake above 460 K. Possible VD. Deposition of impurities. Butene desorption Extensive dehydrogenation Uptake past monolayer above 400 K Acetonitrile formation o uptake below 300 K -sec-butylacetamidine desorption o appreciable changes seen with hydrogen surface presaturation Q. Ma, H. Guo, R. G. Gordon, F. Zaera, hem. Mater., 22(2), (2010). 11
12 Amidinate Uptake Growth Rate, LEIS i Θ = 0.85 Saturation at ~ 15 L Some surface uncovered upon annealing ~ 3 ycles/ ML in ALD mode Q. Ma, H. Guo, R. G. Gordon, F. Zaera, hem. Mater., 22(2), (2010). 12
13 Amidinate Thermal hemistry Proposed Mechanism H 2 H 2 H H H H 2 H H 2 H2 H 2 H H Dissociative adsorption H 2 < 150 K (ads) Several intermediates form vs. T Some may desorb molecularly, but by ~ 480 K dehydrogenation is irreversible -sec butylacetamidine H 300 K H 2 H H 310 K K H K H H H H H ~500 K (ads) (ads) (ads) (?) = H 2 H 3 (?) 405 K Acetonitrile opper reduction (I) (0) Q. Ma, H. Guo, R. G. Gordon, F. Zaera, hem. Mater. (2011). Butene H=H 480 K H H 2 H 13
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