Leiste, H.

Seemann, K.

Seifert, H.J.

Strafela, M.

Ulrich, S.

Seifert, H. J.

KITopen

KIT – University of the State of Baden-Wuerttemberg and National Research Center of the Helmholtz Association Influence of the substrate topography on the constitution of Li-rich Li-Ni-Mn-Co-O thin film for battery application M. Strafela, K. Seemann, H. Leiste, H.J. Seifert, S. Ulrich  9-th Symposium on Vacuum based Science and Technology in conjunction with the 14-th Annual Meeting of the German Vacuum Society - DVG Conclusions and Outlook: 15 20 25 30 35 40 45 50 55 60 65Si110018017009012006011015014003 20 Pa10 Pa7 Pa2 Pa4 Pa0.5 Pa2 in deg.p = 0.2 PaBy increasing the surface area is it possible to improve the Li-diffusion rate or rate capability of Lithium-Ion batteries. The surface topography of stainless steel substrates are varied by sputter etching. Stainless steel substrates were sputter etched for  12 minutes at 500 W and between 30 minutes to 180 minutes at 900 W.  Li-rich Li-Ni-Mn-Co-O thin films are deposited onto these modified stainless steel substrates by non-reactive r.f. magnetron sputtering from a ceramic Li1.11(Ni0.37Mn0.19Co0.33)O1.77 target. Coating thickness is about 100 nm. In order to induce a transition of the crystalline films from a disordered to an ordered layered structure the films were post heat treated at 600 °C for one hour at 10 mPa in  Argon:Oxygen (80:20).   R.f. magnetron  sputtering: X-Ray diffraction as deposited XRD - Intensity in a.u. ICP-OES and CGHE analysis (before annealing) Raman-spectroscopy and X-ray diffraction - Li-Ni-Mn-Co-O thin films were successfully deposited on stainless steel with different surface topography. - By pre-deposition sputter etching the film roughness (RA) can be adjust between 8 nm to 44 nm. - Film roughness has no significant influence on other microstructural.  Film deposition Film roughness of selected films (7 Pa)    Pressure variation Ar-working gas pressure in Pa Ordered layered structure NMC 200 300 400 500 600 700 800480 Eg590 A1g12 min30 min 60 min120 min etching time 180 min  Raman - Intensity in a.u.Raman shift in cm-1200 300 400 500 600 700 800480 Eg590 A1g12 min30 min 60 min120 min etching time180  min  Raman - Intensity in a.u.Raman shift in cm-135 40 45 50 55 60 65 70 75 80 85180 min120 min etching time60 min30 min12 min(110)(018)(012)(01-1)SSSSSSSS  XRD - Intensity in a.u.2 in deg.SS35 40 45 50 55 60 65 70 75 80 85180 min 120 min etching time60 min30 min12 minSS SSSS(110)(012)(018)  XRD - Intensity in a.u.2 in deg.(01-1) SSAFM measurements As deposited films Heat treated films Pre-deposition etching time 12 min 30 min 60 min 120 min 180 min As deposited films Heat treated films  600 °C one hour 10 mPa Ar:O2 (80:20)  Film roughness (RA,  20µm x 20µm) of as deposited and heat treated films depending on the pre-depositon etching time.  Bevor deposition the substrates were sputter etched for 12 min with 500 W and between 30 min to 180 min with 900 W. µm µm µm µm µm µm µm µm µm µm Acknowledgment: The authors gratefully acknowledge the financial support by the Helmholtz-Portfolio-project  “Elektrochemische Speicher im System - Zuverlässigkeit und Integration“ 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 600 °C one hour 10 mPa Ar:O2 (80:20) 0 25 50 75 100 125 150 175 20001020304050607080   as dep. heat treated bevor dep.Ra in nmetching time in min.

Influence of the substrate topography on the constitution of Li-rich Li-Ni-Mn-Co-O thin film for battery application

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