Solid-State Electronics 126 (2016) 170–174 Contents lists available at ScienceDirect Solid-State Electronics journal homepage: www.elsevier.com/locate/sse Ambient effect on thermal stability of amorphous InGaZnO thin film transistors Jianeng Xu, Qi Wu, Ling Xu, Haiting Xie, Guochao Liu, Lei Zhang, Chengyuan Dong ⇑ National Engineering Lab for TFT-LCD Materials and Technologies, Department of Electronic Engineering, Shanghai Jiao Tong University, Shanghai 200240, China a r t i c l e i n f o Article history: Received 17 March 2016 Received in revised form 7 August 2016 Accepted 9 August 2016 Available online 9 August 2016 The review of this paper was arranged by Dr. Y. Kuk Keywords: Amorphous InGaZnO (a-IGZO) Thin film transistor (TFT) Thermal stability Ambient gas a b s t r a c t The thermal stability of amorphous InGaZnO thin film transistors (a-IGZO TFTs) with various ambient gases was investigated. The a-IGZO TFTs in air were more thermally stable than the devices in the ambient argon. Oxygen, rather than nitrogen and moisture, was responsible for this improvement. Furthermore, the thermal stability of the a-IGZO TFTs improved with the increasing oxygen content in the surrounding atmosphere. The related physical mechanism was examined, indicating that the higher ambient oxygen content induced more combinations of the oxygen vacancies and adsorbed oxygen ions in the a-IGZO, which resulted in the larger defect formation energy. This larger defect formation energy led to the smaller variation in the threshold voltage for the corresponding TFT devices. Ó 2016 Elsevier Ltd. All rights reserved. 1. Introduction Amorphous InGaZnO (a-IGZO) thin film transistors (TFTs) have been considered one of the most promising candidates for use in next-generation displays including active-matrix liquid crystal displays (AMLCDs) and active-matrix organic light-emitting diodes (AMOLEDs); this is largely due to their high field-effect mobility, which is greater than that found in traditional hydrogenated amorphous silicon (a-Si:H) TFTs, and good large-area uniformity, which is superior to conventional polycrystalline silicon (p-Si) TFTs [1,2]. However, from a practical point of view, some critical issues, such as the instability of a-IGZO TFTs, still need to be resolved [3,4]. The thermal instability of a-IGZO TFTs caused by the prolonged temperature stressing is especially important for the display products that utilize these novel semiconductor devices [5–7]. Several research groups ascribed the negative threshold voltage shifts of the a-IGZO TFTs at high temperatures to the generation of oxygen vacancies [8–10]. The gas molecules in the surrounding atmosphere also play an important role [11,12]. Chang et al. observed the suppression of the thermal instability of the a-IGZO TFTs in the ambient air with respect to the a-IGZO TFTs in a vacuum [11]. Our group demonstrated that the passivation layers, which prevented the interaction between the active layers and the ⇑ Corresponding author at: 800 DongChuan Rd., Shanghai 200240, China. E-mail address: [email protected] (C. Dong). http://dx.doi.org/10.1016/j.sse.2016.08.001 0038-1101/Ó 2016 Elsevier Ltd. All rights reserved. ambient air, could markedly improve the thermal stability of the a-IGZO TFTs. We built a simple model to describe the related physical mechanism; for the sake of simplicity, only oxygen was considered in the discussion of the ambient effects [12]. However, the other ambient gases, such as moisture, nitrogen, and inert gases could also influence the instability of a-IGZO TFTs. Our recent studies confirmed this assumption and proved that moisture was the main origin of the storage instability for the a-IGZO TFTs at room temperature (RT) [13]. These facts inevitably make us wonder how the ambient gases exactly influence the thermal instability of a-IGZO TFTs. We believe the answer to this question might lead us to discover how to improve the thermal stability of these novel semiconductor devices. In this research, we measured the transfer characteristics of the a-IGZO TFTs in the temperature range of 323–473 K with various ambient gases including air, Ar, O2, N2, and H2O. Interestingly, O2, one of the main components of air, was the only gas that enhanced the thermal stability of the a-IGZO TFTs. 2. Experiment The inverted-staggered a-IGZO TFTs, as shown in Fig. 1(a), were fabricated on the substrates of n-type silicon wafers (gate electrodes) with 300-nm-thick layers of thermal SiO2 (gate insulators). After the substrates were thoroughly cleaned, the 50-nm-thick a-IGZO films were deposited as the active layers and the J. Xu et al. / Solid-State Electronics 126 (2016) 170–174 171 respectively. A heating stage was used to modulate the measurement temperature (298–423 K) of the samples. Based on the measured transfer curves, the threshold voltage (Vth) was obtained from the gate voltage value (Vgs) where Ids/(W/L) = 100 nA. Here, Ids is the drain current of the TFT devices. In order to quantitatively characterize the thermal stability of the a-IGZO TFTs, we defined the essential term DVth as DVth = Vth(T) Vth(298 K), where T represents the ambient temperature. Apparently, smaller values of the DVth imply the improved thermal stability of the a-IGZO TFTs. 3. Results and discussion Fig. 1. (a) Schematic cross section of the inverted-staggered a-IGZO TFTs used in this study. (b) Schematic diagram of the unsealed probe station and electrical meters for the current-voltage (I-V) measurements. 200-nm-thick Indium Tin Oxide (ITO) films were prepared as the source/drain (S/D) electrodes by the magnetron sputtering technique. Patterned by shadow masks, the channel length (L) and width (W) of the devices were fixed to 250 lm and 1000 lm, respectively. Finally, the samples were annealed in air at 683 K for 1 h to improve their electrical properties. We measured the transfer characteristics (VDS = 10 V) of the devices in an unsealed probe station chamber using a Keithley 2636A parameter analyzer (Fig. 1(b)). It is worth noting that the chamber maintained the atmospheric pressure and room temperature and little gas circulation, which created the conditions strikingly similar to those of the natural atmosphere. We directly fed argon, nitrogen, and oxygen into the unsealed chamber, but injected the moisture by feeding the water molecules with the argon flow. The moisture content was quantitatively controlled by the water level in the container, i.e., the humidity in the chamber increased proportionally with the rise of the water level. We defined three water levels, low, middle, and high, and characterized them as ‘‘Low H2O”, ‘‘Middle H2O”, and ‘‘High H2O”, Fig. 2 shows the transfer characteristics of the a-IGZO TFTs at different temperatures in the ambient air. As shown in Fig. 2(a), the Vth of the transfer curves shifted negatively and the drain current increased gradually with the increasing temperature. This degradation was mainly associated with the generation of the oxygen vacancies [8–10] and/or the ambient effects [11,12]. The intrinsic excitation (i.e. the thermally generated electrons and holes) cannot work efficiently unless T > 473 K [12], so we ignored this mechanism. In addition, we observed the recovery process of the transfer characteristics when we shut down the heater, which resulted in the gradual fall of the temperature. Fig. 2(b) shows that both Vth and Ids recovered to the initial values within 90 min. The slow recovery process agreed well with the assumption that the ambient effects (instead of the intrinsic excitation) dominated the thermal instability of the a-IGZO TFTs observed in this study. Fig. 3 shows the DVth of the a-IGZO TFTs as a function of the temperature in the ambient argon, air, and nitrogen, respectively. For argon and nitrogen, their flow rates were fixed at 15 L per minute (LPM) to ensure that the original air in the unsealed chamber could be completely removed. It is generally believed that argon, a kind of inert gas, hardly interacts with semiconductors due to its inertness. Hence, the thermally induced DVth of the a-IGZO TFTs in the ambient argon was mainly associated with the inside generation of oxygen vacancies, i.e. the thermally excited oxygen atoms leaving their original sites, moving into the interstitial sites, and causing the vacancies with the remained free electrons at the corresponding sites [8–10]. Therefore, the Vth reductions observed at high temperatures for the a-IGZO TFTs in the ambient argon (as shown in Fig. 3) could be attributed to the additional generation of these free electrons along with the oxygen vacancies. For simplicity, we regarded the performance of the devices in argon as a reference to elucidate the ambient effects on the thermal stability Fig. 2. Transfer characteristics of the a-IGZO TFTs (a) at different temperatures and (b) in the recovery process in the ambient air. 172 J. Xu et al. / Solid-State Electronics 126 (2016) 170–174 Fig. 3. Temperature dependence of DVth for the a-IGZO TFTs in the ambient air, argon, and nitrogen. Fig. 4. Temperature dependence of DVth for the a-IGZO TFTs in the ambient argon (no H2O) and moisture. Here, the ‘‘Low H2O”, ‘‘Middle H2O”, and ‘‘High H2O” are the various water levels, as shown in Fig. 1(b). of the a-IGZO TFTs. Then, as shown in Fig. 3, the ambient air apparently improved the thermal stability of the devices. Although Chang et al. [11] reported a similar result, it is still unknown which gas (i.e. nitrogen, moisture, or oxygen) was responsible for this improvement. In this study, we measured the temperature dependence of DVth on the ambient nitrogen, moisture, and oxygen. As shown in Fig. 3, the temperature dependence of DVth on the ambient nitrogen exhibited a similar tendency with that found with the ambient argon, indicating that nitrogen hardly interacted with the back channels of the devices, even at high temperatures. This was consistent with the results for the a-IGZO TFTs under both the bias stresses and ambient nitrogen [14]. Next, we measured the thermal stability of the a-IGZO TFTs in the ambient moisture. Fig. 4 shows the DVth of the a-IGZO TFTs as a function of the temperature under the ambient ‘‘Low H2O”, ‘‘Middle H2O”, and ‘‘High H2O” conditions, respectively. For comparison, the figure also shows the case in the ambient argon (no H2O). Fig. 4 indicates that the Vth reduction under the ‘‘Low H2O” conditions exhibited a similar tendency to that found with the argon gas (no H2O). Even when the moisture content increased (‘‘Middle H2O”/‘‘High H2O”), the DVth still remained almost the same. It seemed that the a-IGZO TFTs at high temperatures were not sensitive to the moisture, a result that was quite different from our pervious study that showed the a-IGZO TFTs stored at RT were fairly sensitive to the ambient moisture [13]. Based on the aforementioned investigations, we examined the physical mechanism concerning the effect of the ambient moisture on the thermal stability of the a-IGZO TFTs by comparing the cases at RT and a high temperature. Fig. 5(a) shows the mechanism of the moisture adsorption for the a-IGZO TFTs at RT. The surrounding moisture was easily adsorbed onto the back channel surface, which donated electrons to the a-IGZO in a form of H2O = H2O+ + e, and thus led to the gradual negative shift of the Vth for the devices stored at RT until the system reached equilibrium [13,15]. However, when the a-IGZO TFTs were heated, as shown in Fig. 5(b), apart from the inside generation of the oxygen vacancies, the high temperature suppressed the moisture adsorption onto the a-IGZO films; as a result, the moisture donated few electrons to the active layers of the a-IGZO TFTs. Fig. 5(c) shows that even with the increase in the moisture content, the moisture adsorption effect was still negligible. So, the negative Vth shifts of a-IGZO TFTs at a high temperature in the ambient moisture were mainly caused by the inside generation of the oxygen vacancies rather than the extra electrons donated by the ambient moisture. Therefore, the ambient moisture did not influence the thermal stability of the a-IGZO TFTs. Neither nitrogen nor moisture was proven to significantly influence the thermal stability of the a-IGZO TFTs. We therefore assume that oxygen should exhibit different performance, which was confirmed by the following experimental results. Fig. 6 shows the temperature dependence of DVth for the a-IGZO TFTs in the ambient oxygen with different flow rates; we include the results for the ambient argon for comparison. One may observe much smaller Vth reductions with the increase in the surrounding oxygen content. For example, the DVth at 423 K improved to only 7 V when the oxygen flow rate increased to 15 LPM. It seemed that the a-IGZO TFTs at high temperatures were fairly sensitive to oxygen, contrary to what our pervious results indicated (i.e. the a-IGZO TFTs stored at RT were insensitive to the ambient oxygen [13]). Since the thermal instability of the a-IGZO TFTs was closely connected to the oxygen content in the surrounding atmosphere, Fig. 5. Schematic diagram of the a-IGZO films in the ambient moisture (a) without heating, (b) with heating (little H2O), and (c) with heating (more H2O). J. Xu et al. / Solid-State Electronics 126 (2016) 170–174 Fig. 6. Temperature dependence of the DVth for the a-IGZO TFTs in the ambient argon and oxygen with different flow rates. Fig. 7. Experimental plots and the proximate straight lines for ln(|DVth|) e/kBT in the temperature range of 323–423 K for the a-IGZO TFTs in the ambient argon with a flow rate of 15 LPM or the oxygen with the flow rate of 5, 10, and 15 LPM, respectively. Inset: the dependence of the defect formation energy W on the different gases in the surrounding atmosphere. investigating the exact physical essence of the oxygen vacancy formation during the thermal stability tests became necessary. Here, we employed a theoretical analysis based on the model proposed by Takechi et al. [9], where the temperature dependence of DVth can be expressed as the following equation: lnðjDV th jÞ ¼ W Cg ; ln 3kB T 2 e t IGZO C 1 ð1Þ 173 where W stands for the defect formation energy, kB is the Boltzmann constant, Cg is the capacitance of the gate insulator per unit area, e is the electronic charge, tIGZO is the thickness of the a-IGZO layer, and C1 is the constant related to the entropy for the formation of one vacancy and two free electrons. By using the experimental data (shown in Fig. 6) and the least square method to fit these points, we extracted W and C1 from the slope and the intercept of the straight lines expressed by Eq. (1), as shown in Fig. 7. Here, the defect formation energy W rather than C1 was calculated since the later was beyond the scope of this article. As shown in the inset of Fig. 7, the experimental plots led to the proximate straight lines with W of 0.696, 0.750, 0.786, and 0.831 eV when the argon flow rate was fixed at 15 LPM or the oxygen flow rate was fixed at 5, 10 and 15 LPM, respectively. The defect formation energy clearly increased with the rise in the ambient oxygen content. It is well known that the electron concentration in a-IGZO is closely related to the concentration of the oxygen vacancies determined by the defect formation energy W [9,16]. Generally speaking, the higher W values lead to the smaller variations in the carrier concentration. Therefore, a conclusion might be that the higher ambient oxygen content could result in the larger defect formation energy in the a-IGZO films and thus lead to a smaller variation in the carrier concentration and DVth value. Why did the higher ambient oxygen content cause the larger defect formation energy in the a-IGZO? We discuss the related physical mechanism based on some earlier reports in the literature [11,13,17–19]. Since the a-IGZO TFTs were fabricated and stored in the ambient air, the oxygen molecules were adsorbed onto the back channel surface, as reported by several researchers [17–19]. The adsorbed oxygen on the back channel surface existed as O or O 2 , indicating that the adsorbed oxygen could accept electrons from the back channel and cause a positive shift of Vth [17,18]. Our pervious results proved that this oxygen adsorption would achieve saturation at RT, as shown in Fig. 8(a); it was characterized by the phenomenon in which the oxygen molecules could no longer be adsorbed onto the back surface anymore with the further increase in the ambient oxygen content [13]. When the a-IGZO TFTs were heated, a large amount of oxygen vacancies were generated by thermal excitation, which led to the large negative Vth shifts as the temperature increased. Apart from the inside generation of the oxygen vacancies, the recombination of the oxygen vacancies and oxygen ions was accelerated at high temperatures in the ambient oxygen [11]; this process could be divided into two steps, as shown in Fig. 8(b). First, the saturation of the oxygen adsorption was broken at high temperatures and more oxygen molecules were adsorbed onto the back channel surface, which additionally accepted electrons and created the oxygen ions (O or O 2 ). It is likely that the oxygen ions existed as O at high temperatures, and the related reaction can be described as O2 + 2e = 2O [19]. Second, the thermally excited oxygen vacancies recombined with the oxygen ions in the a-IGZO films, which can be described as Metal-V+o + O = Metal-O, where Metal-V+o and Fig. 8. Schematic diagram of the a-IGZO films in the ambient oxygen (a) without heating, (b) with heating (little O2), and (c) with heating (more O2). 174 J. Xu et al. / Solid-State Electronics 126 (2016) 170–174 Metal-O stand for the oxygen vacancy and the recovered oxygen atom, respectively. In addition, the higher oxygen content in the ambience accelerated this recombination process, indicating that more oxygen atoms might turn into oxygen ions and then recombine with the oxygen vacancies as the ambient oxygen flow rate increased, as shown in Fig. 8(c). Therefore, the generation of oxygen vacancies in the a-IGZO films at high temperatures needed more energy (a higher W value) if the devices were exposed to more oxygen molecules. In other words, the higher ambient oxygen content made the thermal generation of the oxygen vacancies in the active layers more difficult, resulting in more thermally stable a-IGZO TFTs. 4. 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