Study on In2O3-SnO2 transparent and conductive films prepared by d.c. sputtering using high density ceramic targets

The influence of SnO₂ concentration in the target on the film characteristics was studied in order to make the useful database for the device design when low discharge voltage sputtering method and a high density In₂O₃-SnO₂ ceramic targets were used. In the case of the films deposited on unheated substrate, X-ray diffraction profile showed amorphous structure. Minimum resistivity of 358 μΩ cm was obtained by In₂O₃ film with mobility of 40.1 cm² (V s)⁻¹ and carrier density of 4.35E+20 cm⁻³. With the increase of SnO₂ contents, resistivity of the films increased because of the decrease in both carrier density and mobility. Whereas, the films deposited on heated substrates showed polycrystalline structure. Resistivity was reduced, ranging from 5 to 20 wt.% SnO₂, and minimum resistivity of 136 μΩ cm was obtained at 15 wt.% with mobility of 40.5 cm² (V s)⁻¹ and carrier density of 1.13E+21 cm⁻³. Transmittance and reflectance of these films strongly depend on carrier density.     

磁控溅射ITO薄膜的退火处理

采用直流磁控溅射方法在室温下玻璃基板上制备ITO(Indium tin oxide)薄膜,并在真空中不同温度(100℃~400℃)下退火处理.研究了退火对薄膜表面形貌、电光特性的影响.XRD测试发现薄膜在200℃退火后结晶,优选晶向为(222).随退火温度升高,方块电阻迅速下降,表面更加平整,薄膜在可见光范围平均透过率提高到85%.     

A study of deposition of ITO films on organic layer using facing target sputtering in Ar and Kr gases

In this study, the effects of sputtering gases on the damage to an organic layer (aluminum (III) bis(2-methyl-8-quninolinato)-4-phenylphenolate (BAlq)) were investigated in the deposition of indium-tin oxide (ITO) films by using a facing target sputtering (FTS) system. Only a small improvement in the PL intensity of the BAlq layer was observed when the sputtering gas was changed from Ar to Kr gas. It was also found that suppression of the high-energy γ-electron bombardment to the substrate is very important to reduce the damages in the BAlq layers. In addition, a remarkable improvement in the PL intensity was observed by the increase in the sputtering gas pressure from 0.3 to 1.3 Pa. These results suggest that bombardment of reflected neutral gas atoms is not the main source of the damage that BAlq layer has, but the bombardment of high-energy sputtered atoms plays an important role for the remnant damages caused by the sputter-deposition of the ITO film at a low gas pressure, since the decrease in the PL intensity was almost totally suppressed by increasing the sputtering gas pressure above 1.1 Pa. Finally, low-damage sputter-deposition of ITO film with low resistivity on BAlq layer was achieved by completely suppressing the bombardment of high-energy particles, including γ-electrons, negative oxygen ions and high-energy sputter-emitted particles.     

Structure and electrical properties of ITO thin films deposited at high rate by facing target sputtering

High rate deposition of ITO thin films at a low substrate temperature was attempted by using a facing target sputtering (FTS) system. Deposition rate as high as 53 nm/min was realized on polycarbonate film substrate of 80-μm thickness. When the film was deposited at a deposition rate above 80 nm/min, polycarbonate film substrate was thermally damaged. The film deposited by FTS has much smaller compressive film stress than the film deposited by conventional magnetron sputtering. The film stress was reduced significantly by increasing the sputtering gas pressure and stress-free films can be obtained by adjusting the sputtering gas pressure. This may be mainly caused by the fact that bombardment by high energy negative oxygen ions to substrate surface during deposition can be completely suppressed in the FTS. Film structure and electrical properties changed little with substrate position, and uniform films were obtained by the FTS.     

Fabrication of low resistivity tin-doped indium oxide films with high electron carrier densities by a plasma sputtering method

Tin-doped indium oxide (ITO) films fabricated on glass substrates using a hot-cathode plasma sputtering method exhibited low resistivity of 9.7 × 10⁻⁵ Ω cm, which is due to a high carrier density of 2.1 × 10²¹ cm⁻³. The change in the number of carriers, N, as a function of film thickness d, strongly suggests that oxygen extraction in the initial stages of ITO film growth on the glass substrate surface, creates oxygen vacancies as an electron carrier source for improvement in the resistivity of the films.     

磁控溅射制备增透ITO薄膜及其性能研究

用射频磁控溅射法在低温下制备了光电性能优良的ITO(In2O3:SnO2=1:1)薄膜。质量流量计调节氩气压强PAr为0.2～3.0Pa,氧流量fO2为0～10sccm,并详细探讨了溅射时PAr和fO2变化对ITO薄膜光学性能的影响。结果表明:fO2的改变引起薄膜中氧空位浓度变化而影响ITO薄膜折射率n;fO2对ITO靶材表面的溅射阀值和对Ar 散射而改变溅射速率。衬底表面粗糙度对ITO薄膜的折射率测量准确性有较大影响。PAr为0.8Pa,fO2为2.4sccm,薄膜厚度为241.5nm时,nmin=1.97,最大透过率为89.4%(包括玻璃基体),方阻为75.9?/□,电阻率为8.8×10-4?·cm。AFM分析表明薄膜表面针刺很少,表面平整(RMS=3.04nm)。     

溅射及RTA处理对ITO薄膜特性的影响

采用RF-磁控溅射生长铟锡氧化物薄膜(ITO),研究了生长条件、快速热退火(RTA)温度对薄膜的晶化情况、透过率、电导率以及表面形貌的影响.结果表明:改变In2-x3 (Snx4 ·e)O3制备过程中的氧含量使Sn4 ·e对电子束缚能力发生变化,过高的氧分压使费米能级EF降低,功函数Ws增大,氧气流量为2 ml/min、退火温度为450℃时薄膜电阻率最低为2.5×10-4 Ω·cm,透过率达88%以上.     

Improved ITO thin films with a thin ZnO buffer layer by sputtering

In this paper, we report a buffering method of improving the quality of ITO thin films on glass by r.f. magnetron sputtering. By applying a ZnO buffer before the ITO deposition in the same run of sputtering, ITO films showed single (111)-oriented highly textured structure, while ITO films showed mixed-oriented polycrystalline structure on bare glass. A design of experiment was taken out to minimize the resistivity of ITO films in the deposition parameter space (oxygen ratio, total gas pressure, and temperature). Resistance measurements showed that the ITO films with ZnO buffers had a remarkable 50% decrease of resistivity comparing to those without ZnO buffers at optimized deposition condition. Room-temperature Hall effect measurements showed that the decrease in resistivity comes from a large increase of mobility and a slight increase of carrier density after forming gas annealing. The ZnO/glass may be a good alternative substrate to bare glass for producing high quality ITO films for advanced electro-optic applications.     

室温直流磁控溅射制备ITO膜及光电性能研究

室温条件下,在玻璃衬底上,采用直流磁控溅射法制备了ITO膜.研究了溅射压强,氧流量和溅射功率等工艺参数对薄膜光电性能的影响.结果表明当Ar流量为44.2 sccm和溅射时间20 min等参数不变时,溅射气压0.7 Pa,氧流量0.62 sccm和溅射功率130 W为最佳工艺条件.并得到了电阻率5.02×10-4 Ω·cm,在可见光区平均透过率80%以上ITO薄膜.     

Effect of nitrogen flow rate on properties of nanostructured TiZrN thin films produced by radio frequency magnetron sputtering

The effect of nitrogen flow rate on structure and properties of (Ti,Zr)N thin films was investigated in the study. Two types of (Ti,Zr)N thin films were found with different nitrogen flow rates, one is the single-phase solid solution of (Ti,Zr)N that appeared for nitrogen flow rates of 2-7 sccm, the other one is the phase of both (Ti,Zr)N and TiZr mixture for the lower nitrogen flow rates of 1 sccm. The grain size of the films was also determined by X-ray diffraction, and the size was less than 20 nm. The (Ti,Zr)N films show excellent hardness ranging from 35.5 to 37.5 GPa with exhibiting (111) preferred orientation.     

磁控溅射制备ITO薄膜光电性能的研究

采用直流磁控溅射方法在玻璃基底上制备了ITO薄膜.分别用分光光度计和四探针仪测试了所制备ITO薄膜在可见光区域内的透过率和电阻率,研究了溅射气压、氧氩流量比和溅射功率三个工艺参数对ITO薄膜光电性能的影响.研究结果表明,制备ITO薄膜的最佳工艺参数为:溅射气压0.6 Pa,氧氩流量比1:40,溅射功率108 W.采用此工艺参数制备的ITO薄膜在可见光区平均透过率为81.18％,薄膜电阻率为8.9197×10-3Ω·cm.     

Electrical and optical properties of Al-doped ZnO films deposited by hollow cathode gas flow sputtering

Al-doped ZnO (AZO) films were deposited on glass by hollow cathode gas flow sputtering using Zn-Al alloy targets. Sputtering power for all the depositions was fixed at 1500 W. Resistivities of 0.81-1.1 × 10^− 3 Ω cm were obtained for AZO films deposited at room temperature with an O₂ flow from 38 to 50 standard cubic centimetre/minute (SCCM), while static deposition rates were almost constant at 270-300 nm/min. On the other hand, lower resistivities of 5.2-6.4 × 10^− 4 Ω cm were obtained for AZO films deposited at 200 °C with an O₂ flow from 25 to 50 SCCM, while the static deposition rates were almost constant at 200-220 nm/min. Average transmittances in the visible light region were above 80% for both sets of films.     

Indium zinc oxide semiconductor thin films deposited by dc magnetron sputtering at room temperature

Amorphous indium zinc oxide (IZO) thin films were prepared on glass substrates by dc magnetron sputtering at room temperature. The resistivity of IZO films could be controlled between 3.8 × 10⁻³ and 2.5 × 10⁶ Ω cm by varying the oxygen partial pressure during deposition, while keep the average transmittance over 83%. With IZO films as channel layers, whose surface root-mean-square roughness was less than 1 nm, thin film transistors were fabricated at room temperature, showing enhanced mode operation with good saturation characteristics, mobility of 5.2 cm² V⁻¹ s⁻¹, threshold voltage of 0.94 V and on/off ratio of ∼10⁴.     

Properties of Ce-doped ITO films deposited on polymer substrate by DC magnetron sputtering

Ce-doped indium tin oxide (ITO:Ce) films were deposited on flexible polyimide substrates by DC magnetron sputtering using ITO targets containing various CeO₂ contents (CeO₂ : 0, 0.5, 3.0, 4.0, 6.0 wt.%) at room temperature and post-annealed at 200 °C. The crystallinity of the ITO films decreased with increasing Ce content, and it led to a decrease in surface roughness. In addition, a relatively small change in resistance in dynamic stress mode was obtained for ITO:Ce films even after the annealing at high temperature (200 °C). The minimum resistivity of the amorphous ITO:Ce films was 3.96 × 10^− 4 Ωcm, which was deposited using a 3.0 wt.% CeO₂ doped ITO target. The amorphous ITO:Ce films not only have comparable electrical properties to the polycrystalline films but also have a crystallization temperature > 200 °C. In addition, the amorphous ITO:Ce film showed stable mechanical properties in the bended state.     

Protective YSZ-based thin films deposited by RF magnetron sputtering

Protective Zr(Y)O_2−δ-based films sputter-deposited onto apatite-type lanthanum silicate ceramics were appraised for potential applications in solid oxide fuel cells with silicate-based solid electrolytes, where the performance may suffer from surface decomposition processes in reducing atmospheres. Dense and crystalline coatings were deposited using radio-frequency magnetron sputtering from an yttria-stabilized zirconia target. On the basis of microstructural analysis and profile measurements, a sputtering power of 300 W was selected in order to achieve deposition rates in the range 0.50-0.75 μm/h. The surface morphology studies using an atomic force microscope revealed typical film structures with small (<50 nm) grains. The polarization of model electrochemical cells with cermet anodes comprising Ni, yttria-stabilized zirconia and Ce_0.8Gd_0.2O_2−δ (50:30:20 wt.%), deposited onto the protective zirconia films, was found quite similar to that of copper-zirconia cermets without interlayers, suggesting that the electrochemical reaction is essentially governed by the oxygen anion transfer from zirconia phase and/or hydrogen oxidation in the vicinity of zirconia film surface.     

Characterization of iridium oxide thin films deposited by pulsed-direct-current reactive sputtering

Thin films of iridium oxide were deposited on silicon and borosilicate glass substrates by pulsed-direct-current (pulsed-DC) reactive sputtering of iridium metal in an oxygen-containing atmosphere. Optimum deposition conditions were identified in terms of plasma pulsing conditions, oxygen partial pressures, and substrate temperature. The films were characterized by X-ray diffraction, X-ray photoelectron spectroscopy, Raman spectroscopy, and Rutherford backscattering spectroscopy. According to the results, it was possible to obtain films that are near-stoichiometric, smooth and uniform in texture. The films deposited without substrate heating were amorphous, and those deposited at substrate temperatures above 300 °C were found to have a homogeneous polycrystalline structure. The results also showed that pulsed-DC sputtered iridium oxide films were smoother and had lower micro-inclusions density than DC-sputtered films obtained under otherwise similar deposition conditions. This improvement in the film quality is at the expense of a tolerable decrease in the deposition rate.     

ZnO掺杂Li+陶瓷靶及溅射膜制备工艺研究

利用固相反应成功地制备了直径为70mm,厚度为10～15mm的掺杂Li离子ZnO陶瓷靶材.研究了不同摩尔浓度的Li离子掺杂靶材,并对其绝缘电阻与损耗进行了分析比较,最终确定Li离子的最佳掺杂量为2.2l%(摩尔分数).同时通过在不同温度烧结试验、不同成型压力试验确定了ZnO靶材制备的最佳工艺,并通过所制备的ZnO-Li0.022陶瓷靶,采用RF射频磁控溅射技术在Si(100)、玻璃(载玻片)、及Pt(111)/Ti/SiO2/Si(100)基片上制备出高度c轴(002)择优取向、均匀、致密的ZnO薄膜.     

Cu2O thin films deposited by reactive direct current magnetron sputtering

The Cu₂O thin films were prepared on quartz substrate by reactive direct current magnetron sputtering. The influences of oxygen partial pressure and gas flow rate on the structures and properties of deposited films were investigated. Varying oxygen partial pressure leads to the synthesis of Cu₂O, Cu₄O₃ and CuO with different microstructures. At a constant oxygen partial pressure of 6.6 × 10^− 2 Pa, the single Cu₂O films can be obtained when the gas flow rate is below 80 sccm. The as-deposited Cu₂O thin films have a very high absorption in the visible region resulting in the visible-light induced photocatalytic activity.     

A study of amorphous and crystalline phases in In2O3-10 wt.% ZnO thin films deposited by DC magnetron sputtering

We report on the processing, phase stability, and electronic transport properties of indium oxide (In₂O₃) doped with 10 wt.% zinc oxide (ZnO) deposited to a thickness of 100 nm using DC magnetron sputter deposition at room temperature and 350 °C. We compare the optimum oxygen content in the sputter gas for pure In₂O₃ and doped with (i) 10 wt.% ZnO and (ii) 9.8 wt.% SnO₂. Amorphous IZO films were annealed at 200 °C in air and N₂/H₂ and resistivity, Hall mobility, and carrier density along with molar volume change were monitored simultaneously as a function of time at temperature. We report that annealing the amorphous oxide in air at 200 °C does not lead to crystallization but does result in a 0.5% decrease in the amorphous phase molar volume and an associated drop in carrier density. Annealing in forming gas leads to an increase in carrier density and a small decrease in molar volume. We also report that when annealed in air at 500 °C, the amorphous IZO phase may crystallize either in the cubic bixbyite or in a recently observed rhombohedral phase.     

Effect of the oxygen flow on the properties of ITO thin films deposited by ion beam assisted deposition (IBAD)

ITO films were deposited onto glass substrates by ion beam assisted deposition method. The oxygen ions were produced using a Kaufman ion source. The oxygen flow was varied from 20 until 60 sccm and the effect of the oxygen flow on properties of ITO films has been studied. The structural properties of the film were characterized by X-ray diffraction and atomic force microscopy. The optical properties were characterized by optical transmission measurements and the optical constants (refractive index n and extinction coefficient k) and film thickness have been obtained by fitting the transmittance using a semi-quantum model. The electrical properties were characterized by Hall effect measurements. It has been found that the ITO film with low electrical resistivity and high transmittance can be obtained with 40 sccm oxygen flow (the working pressure is about 2.3 × 10^− 2 Pa at this oxygen flow).