THIN FILM COMPONENTS FOR Li-ion MICROBATTERIES

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1 THIN FILM COMPONENTS FOR Li-ion MICROBATTERIES J. Přidal a, J. Prachařová a, J. Bludská b, I. Jakubec b a Institute of Physics, Academy of Sciences of the Czech Republic, Na Slovance 2, Prague 8, Czech Republic b Institute of Inorganic Chemistry, Academy of Sciences of the Czech Republic, Řež, Czech Republic The development of thin-film Li-ion microbatteries (MBs) aims at fabrication of MBs applicable on integrated circuits (IC). The operational acceptability is based on low power requirements of ICs and high energy density of MBs. An ideal MB should be inexpensive, compact, lightweight, and theoretically infinitely rechargeable. This contribution reports on preparation and properties of thin film components for all-solid-state MBs, namely LiCoO 2 cathodes and solid electrolytes. Experimental details All thin film components have been prepared by reactive RF magnetron sputtering system. The LiCoO 2 cathode thin films were sputtered on Si/SiO 2 and Si/SiO 2 /Ti/Au heated substrates in Ar/O 2 reactive atmosphere from 25 mm and 50 mm diameter targets () without any post-deposition annealing. The target to substrate distance was 20 mm and 40 mm for different diameters, RF power was 15 W for 25 mm target and 20, 60 and 80 W for 50 mm target. The targets were sintered from LiCoO 2 commercial powder (Aldrich), pressed into pellets under a pressure of 100 MPa and then sintered at C for forty hours. Samples of lithium phosphorous oxynitride (LiPON) electrolyte have been prepared from 50 mm diameter Li 3 PO 4 target on Si/SiO 2 and Si/SiO 2 /Ti/Au substrates by temperature 100 C. Target has been made from Li 3 PO 4 powder, which was pressed into pellet under pressure of 100 MPa and sintered at 750 C for 8 hours. Sputtering process has been carried out in reactive working gas mixture (Ar + N 2 ; N 2 content varying from 20% to 100%) by pressure about 2.5 Pa. The distance between target and substrate was 40 mm and used RF power was 60 W. The LiBO 2 thin films were sputtered on Si/SiO 2 /Ti/Au substrates in Ar/O 2 mixture at C. The RF power was 15 and 60 W for 25 and 50 mm target, respectively. The film thickness was measured on a partially masked film with a Alphastep profilometer. 3-1

2 LiCoO 2 cathodes The phase composition of the LiCoO 2 cathode films was investigated by reflection electron diffraction. It should be noted that this technique allows getting information from only thin surfaces layer ( 10 nm). The measurements were carried out at electron acceleration voltage of 75 kv with use of specialized electron diffraction equipment. The accuracy of this method was not very high, however it was enough to determine exactly all present phases in our samples. It has been found that surface phase composition was different from deeper film layers, which were earlier determined by X-ray diffraction. It has been observed, that on the surface of all the investigated films (deposition temperature T = 100, 200, 300, 400 and 500 C) the same Li 2 CO 3 phase is presented. The Auger analysis data showed, that carbon concentration decreases rapidly from surface into deeper layer and diminishes in 20 nm depth. Because we use turbomolecular pump and the composition measurement of residual gas in chamber doesn't show any presence of carbon, this allows us to propose the following explanation: CO 2 molecules, which are present in the ambient air, absorb on the film surface, react with Li 2 O and form Li 2 CO 3. Such chemical reaction suggests the presence of free unbound Li 2 O on the film surface. This Li 2 CO 3 layer can affect the transport properties of multilayer battery. Scanning Electron Microscope (Philips XL 30 CP, SE detector, accelerating voltage kv) and EDAX analysis was used to observe electrodes morphology and composition. However, the design of the microscope did not enable detection of lithium itself. Therefore, Atomic Absorption Spectrometer (Varian, Flame Atomization System) was used for the determination of Li and Co content in the LiCoO 2 thin films. It follows that neither substrate temperature nor substrate material have a significant effect on Li/Co atomic ratio (see Fig. 1) in films, prepared from 50 mm target. The main parameter influencing the film composition is the RF discharge power. However, there is not any simple relationship between Li/Co atomic ratio and the RF discharge power. The composition nearest to the stoichiometric one (Li/Co = 1) was observed for middle power 60 W. 3-2

3 2,6 2,4 2,2 60W, on Au 60W, on SiO2 20W, on Au 20W, on SiO2 80W, on Au 80 W, on SiO2 Li/Co atomic ratio 2,0 1,8 1,6 1,4 1,2 1, Deposition temperature [ C] Fig. 1 Dependence of Li/Co atomic ratio on deposition parameters The SEM pictures of LiCoO 2 cathode films have been obtained. On the same samples, AFM pictures have been scanned. We can assume, from comparison of these two methods, that all samples contain polycrystalline phase of LiCoO 2 compound, but the density of the crystallites is changing. The density of crystallites increases with increasing deposition temperature, typical SEM picture of LiCoO 2 surface is in Figure 2. The AFM measurements on the same films prepared on different substrates show considerable effect of substrate on film crystalinity and morphology. On the gold covered substrate, both the roughness and the size of crystallites are visibly higher than on SiO 2 or Si substrates. This result is in accordance with previous X-ray diffraction measurements. 3-3

4 Fig. 2 SEM picture of surface of LiCoO 2 sample, prepared by 300 C In situ emission spectroscopy was used under various deposition conditions as discharge plasma diagnostics (Triax 550 JY, CCD detector). Plasma composition was investigated during reactive sputtering of the LiCoO 2 target. For all selected deposition conditions strong Li lines were identified in the spectra. The most intensive line was Li resonant line (670.8 nm). Less intensive Li lines at and nm were found as well. Cobalt lines as Co (384.5 nm) and Co (387.3 nm) were identified in spectra. These results have shown that significant amount of growth components of films are sputtered from the LiCoO 2 target as Li and Co single atoms. The atoms move to a substrate surface where they react with oxygen. The probability of oxidization in the plasma volume is insignificant. Cyclic voltammetry and charge/discharge measurements were carried out on LiCoO 2 electrodes prepared at temperatures from 200 to 500 C. The effect of preparation temperature on electrochemical properties of samples was investigated. Results of charge /discharge measurements are given in the following Table I. Surprisingly good properties were displayed on a cathode prepared at 200 C that absolved 10 cycles and in each of them the capacity reached 140 mah/g. In the case of K2, K5 and K6 electrodes the cut off was given by 4.5 V. This potential value was never reached on K4 and K13 electrodes, where the cut off was given by the time of 125 h. Therefore the capacities have been not evaluated. 3-4

5 Table I. Results of measurements on LiCoO 2 samples (Charge/Discharge: V; constant current-constant voltage method) Sample Temperature [ 0 C] Thickness [µm] Current [ma] Capacity [mah/g] Number of cycles K K Damaged by experiment K ? 3 K6 400 > K K ? 3 Electrolytes LiPON films were explored by AFM microscope, to find the influence of substrate and working gas composition on surface morphology. For this purpose, the films were prepared on two types of substrate, first with SiO 2 upper layer and second with gold layer, and by gas composition: 100% N 2, 80 % N 2,.., 20 % N 2 (the rest argon). 5.0E+6 -Z Im /Ohm.cm 2 / 4.0E+6 3.0E+6 2.0E+6 1.0E+6 0.0E+0 0.0E+0 4.0E+6 8.0E+6 1.2E+7 Z Re /Ohm.cm 2 / Fig. 3 Impedance characteristic of electrolyte sample E20 3-5

6 No visible effect of substrate was observed, the morphology was the same for both substrate materials. Still, the effect of working gas composition is significant. In the first case (deposition in pure N 2 ), the film surface roughness is higher, which can increase the probability of shortcuts. The presence of two phases is possible in this case, while the second case (deposition in 20% N 2 /80% Ar) looks more uniform and with only one phase. The a.c. admittances were measured using PAR 263 equipped by a lock-in amplifier. The preview of some results gives Table II, the example of impedance characteristic is shown in Fig. 3. The marked decrease in resistivity values measured on P13, E19 and E20 samples in the region of high frequencies indicate prevailing ionic contribution in these mixed conductors. The good impedance properties of LiPON sample deposited by 20% N 2 correspond to good surface morphology. Table II: A.c. resistivity of some electrolyte samples Sample Target Atmosphere D [nm] Frequency [Hz] RE [Ω] P13 Li 3 PO 4-50 mm 80% Ar / 20% N 2-15m k 442 P14 Li 3 PO 4-50 mm 40% Ar / 60% N 2-100m k 1.9 PB4 LiBO 2 50 mm 80% Ar / 20% O m 15 75k 15 PB5 LiBO 2 50 mm 80% Ar / 20% O m 56k E4 LiBO 2 25 mm 80% Ar / 20% O m k 3.8 E20 LiBO 2 25 mm 80% Ar / 20% O m k E19 LiBO 2 25 mm 80% Ar / 20% O m k 120 E18 LiBO 2 25 mm 80% Ar / 20% O m k 8.0 Conclusions The main parameter which affects the composition of sputtered LiCoO 2 films is the RF discharge power. Significant amount of growth components are sputtered from the LiCoO 2 target as Li and Co atoms. Mechanism of sputtering of more complex Li and Co compounds directly from the target is not clear yet. Further investigation should reveal these phenomena in more detail. We suppose that strong presence of eroded Li-atoms in the volume of the magnetron discharge is correlated with excess of Li in most deposited samples. Good capacity 3-6

7 of low temperature samples, despite they have lower crystallization, is very important for further use in semiconductor integrated circuits, where the temperature is often the main limiting factor. The prevailing ionic conductivity was found for some thin films of Li electrolytes deposited by RF sputtering. The high resistance in low frequency region indicates leak-free electronically insulating films suitable for further use in microbattery construction. Acknowledgement We thank to Dr. Z. Malkova for Atomic Absorption measurements of cathode films and to Dr. Z. Hubicka for emission spectra evaluation. The support of SfP NATO Programme (SfP /LiBatIC) is gratefully acknowledged. 3-7

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