"Study of Indium Tin Oxide (ITO) for Novel Optoelectronic Devices"
Ph.D. thesis by Shabbir A Bashar


7. Conclusion



In order to investigate the use of optically transparent indium tin oxide (ITO), a range of technological steps were developed and optimised during the course of this study. These include reactive r.f. sputtering, reactive ion etching, careful optimisation for producing ideal Schottky contacts, annealing for producing good ohmic contacts using ITO and metal ohmic contacts on ITO itself. A number of novel optoelectronic devices were fabricated as a result including: transparent metal contact Schottky photo diode
[228], transparent gate HEMT (TG-HEMT) [79], transparent electrode VCSELs [88] and LEDs and transparent emitter contact HPTs [2] .



7.1 ITO Deposition

A reactive r.f. sputtering technique using an argon/oxygen mixture was utilized for the deposition of the Indium Tin Oxide films from a hot pressed target. A number of deposition parameters and their effects on the films were studied in detail. In particular the partial pressure of gaseous oxygen, PO2, in the plasma and the r.f. power, directly affecting the deposition rate, were found to be amongst the most influential. While the conductivity was found to be inversely proportional to the exponential of the PO2, the transparency reduced significantly in the absence of sufficient oxygen. The r.f. power was directly proportional to the film conductivity. These parameters were then optimised to maintain the desired combination of high transparency and conductivity properties of the films and to minimise sputter damage to the substrate material constituting the active device layers. The critical values for PO2 and the r.f. power used were 14e-3 (at a total pressure of approximately 10 mTorr) and 150W respectively.

Using this technique, highly conductive uniform ITO films were obtained. The as deposited sheet resistance, Rsh, was typically 340 W/ which reduced to 27 W/ after annealing. These values correspond to resistivities of 190e-4 Wcm and 15e-4 Wcm respectively and compare favourably to those in the literature. Above 90% transmittance was achieved for these ITO films over the 500nm to 2000nm wavelength range. This corresponds to 2.48eV to 0.62eV energy range which covers majority of the III-V compound semiconductors such as AlAs, AlGaAs, GaAs, InP and InGaAs as well as Si and Ge. For a typical ITO film, the value of the bandgap calculated from the transmission spectra was found to 3.8eV, which is in close agreement with previously published work.



7.2 ITO-based Microfabrication

Driven by the need to produce near micron structures with ITO films, a number of experiments were carried out to develop a suitable method for micro-pattering these films. Due to the energetic species inside the sputtering chamber, resulting in baking of the photoresist, liftoff lithography was rendered unsuitable. Wet chemical etching involving a number of chemicals, such as HCl, HNO3 etc., in various strengths as well as Zn dust as a catalyst were tried and were also found to be unsatisfactory for this delicate application. Finally a selective dry etching technique based on reactive ion etching (RIE) with Ar gas was developed; a 1000 thick layer of Al metal was used as the mask. As well as having a very good selective etch ratio of greater than 4:1 for Al:ITO, the use of Ar as the plasma gas is both cheaper and safer. Two micron fingers were successfully produced using this etching technique. The optimum r.f. power and the chamber pressure RIE system was found to be 100W and 11mtorr respectively.

Two distinct sets of post deposition annealing techniques were developed. One of these was to obtain an ITO/n-GaAs Schottky diode with rectifying contact with low series resistance while retaining the diode parameters for a good device. A two step process extended over several hours was used to ensure the reduction of ITO film resistivity and the recovery of sputter damage from the substrate without affecting the rectifying properties of the device. A five hour anneal at 240C followed by another five hours at 340C in a N2 ambient was found to produce these desired results.

The other annealing technique was developed to produce a heterojunction photo transistor with essentially an ohmic contact to the emitter cap layer. Given that the stringent requirement not to destroy a rectifying junction is no longer applicable, the realisation of an ITO ohmic contact proved to be more difficult than at first imagined. Traditional annealing techniques with RTA or dual alloying methods were unable to produce good uniform ohmic contacts. Thus a new technique involving a step-like annealing method was employed. Samples were at first gently heated at lower temperatures (240C) for relatively longer periods (3 minutes) and gradually the annealing temperature was increased to up to 500C where it was placed for a shorter time (1 minute); the sample was cooled using the reverse temperature/time combination.

Using both these techniques, the resultant ITO resistivity was found to be approximately 14e-4 Wcm. This compares well with the published data.

Bearing in mind the need to form large metal pads for connection to external circuits, a set of experiments were performed to assess various metalisation schemes for making contacts to the ITO films themselves. These metalisation systems were Ni/AuGe/Ni/Au, Ni/Al and Ni/AuGe/Ni/Ti/Au; as well as the ohmic properties, mechanical adhesion was also a factor in these assessments. It was concluded that in the absence of an adhesion promoting layer such as Ni, the use of say only a layer of Au was unsuitable. Comparing the electrical properties of the three metalisation systems investigated, it is noticeable that their unalloyed characteristics were very similar (Rsk and rc in the region of 50W/ and 3e-4 Wcm2 respectively) despite the fact that the sheet resistances of the corresponding ITO material varies over a much greater range (1273 W/ to 665 W/). The Rsk after alloying for all three metalisations lie approximately in the range 1 to 2 W/ while rc lie in the range 3 to 8 e-5 Wcm2. Thus all three systems are equally suited for contacting ITO films as there is very little difference between them.



7.3 Optically Transparent Schottky Diodes

Following thorough cleaning and pre-metalisation chemical etch to the surface of MBE (Si) grown, n-GaAs wafers with ND = 1.4e16 cm-3, 1.75 mm thick active layers, near ideal Schottky diodes were produced using Au and Al as the metal contacts. The ideality factor, n, the barrier height, fbo, and the modified Richardson constant, A**, for the Au/n-GaAs devices were 1.04, 0.84 eV and 12.5e6 Am-2K-2; the corresponding values for the Al/n-GaAs diodes were 1.08, 0.77 eV and 16.0e4 Am-2K-2. These values for both sets of devices are in good agreement with the findings of other researchers. The Schottky diodes were also characterised over a wide temperature range to provide a thorough understanding of their d.c. performance. The results analysed using a simulation model involving the influence of various current transport mechanisms at different temperatures. Excellent agreement was found between the measured and the simulated data.

In the quest for replicating near ideal Schottky diodes with an ITO film replacing the conventional metal contact in the previous set of diodes, numerous experiments were performed to finally achieve the desired goal. As well as thoroughly cleaning the wafer prior to ITO deposition, a number of sputtering parameters had to be optimised. Some of these, such as r.f. power and PO2 and the relevant post-deposition annealing techniques, have already been discussed earlier. In addition, a thin layer of Indium metal, 100, deposited between the ITO and the semiconductor was found to be effective in shielding the substrate from sputter damage. Thus ITO/n-GaAs Schottky photo diodes were realised with the following characteristics: n = 1.1, f bo = 0.76 eV, dark current at -2V = 50 nA, series resistance = 25.8 W, responsivity to 780 nm radiation = 0.57 A/W and an external quantum efficiency, h = 91.5%. These are amongst some of the best results obtained thus far and compare better than many reported in the literature for similar devices. Thus near ideal, ITO/n-GaAs Schottky diodes with low leakage current, low series resistance and high responsivity have been fabricated on n-GaAs epitaxial layers.

The effect of mesa etching, r.f. power, use of a thin layer of indium and gradual annealing at 340C have been studied and optimised to produce near ideal photo diodes. Mesa etching significantly reduces the surface leakage current thus suppressing the dark current. Increasing the r.f. power reduces the sheet resistance of the ITO film but causes greater damage to the substrate; this damage can be minimised by depositing a thin layer of indium on the GaAs substrate prior to sputtering and the damage can be removed by gradual annealing.

A detailed C-V analysis was carried out to separate the effects of sputter damage from associated series resistance. It was concluded that sputtering causes two types of damage:

  1. donor like effect at the surface results from knocking of Arsenic atoms by relatively large Argon ions in the plasma
  2. damage induced traps due to high velocity particles penetrating deeper into the substrate are thought to be the cause of a progressively falling free charge carrier profile.
This requires further detailed study to understand both the cause and the nature of these defects.

These novel ITO/n-GaAs devices were then subject to cryogenic measurements similar to their conventional opaque counterparts. From the measurements, the modified Richardson constant, A**, for these devices were found to be 1.3e4 Am-2K-2, and to the best of our knowledge this is the first time it is being reported for ITO/n-GaAs devices produced by reactive r.f. sputtering.

Having thus obtained relatively large ITO/n-GaAs Schottky photo diodes, high speed diodes can be achieved by shrinking the active region; parasitic capacitances and leakage currents can be reduced by a combination of proton bombardment and mesa etch isolation techniques.



7.4 Transparent Gate HEMTs

As an extension of the work with ITO/n-GaAs Schottky diodes, a set of novel pseudomorphic HEMTs with a transparent gate (TG-HEMT) were fabricated using transparent indium tin oxide for the first time. These AlGaAs/InGaAs/GaAs pseudomorphic HEMTs (pHEMTs) with ITO gate electrodes have an optical responsivity greater than 5A/W corresponding to an external quantum efficiency of greater than 800% for an incident radiation of l= 780nm. A set of conventional devices were also fabricated for comparison using opaque Ti Schottky gates. This was performed in collaboration with another researcher in the group to demonstrate the viability of such devices and greater detail is available in [229] .



7.5 Optically Transparent ITO Ohmic Contacts

The next part of this thesis involved the fabrication of good ITO ohmic contacts to highly conductive n and p type layers (ND = 5e18 cm-3, NA = 5e19 cm-3) of GaAs and n-type InGaAs layers (ND = 3e18 cm-3). The objective was to realise good transparent contacts to the emitter of HBTs for vertical illumination of an optical signal. The TLM method was used for assessing the quality of these contacts. In each of these cases, the transparent ohmic contacts were compared to ohmic contacts made from conventional metals on the same substrates to enable a direct comparison to be made.

For the ITO/n+-GaAs contacts, the insertion of a thin layer of In metal between the semiconductor and the transparent film was found to be very effective in enhancing the ohmic properties of the contact. Although initially this reduced the transparency to nearly 60%, this parameter was restored to above 90% following the ohmic contact annealing scheme discussed earlier. It is believed that In acts as a doping species in n-type GaAs thereby reducing the specific contact resistance. The best transfer resistance, Rt, and the specific contact resistances, rc, achieved in each case were as follows: Rt = 0.68 Wmm, rc = 1.2e-4 Wcm2 (n+-GaAs); Rt = 0.49Wmm, rc = 7.6e-5 Wcm2 (In/n+-GaAs). Thus the superior quality of the ITO/In/n+-GaAs over the ITO/n+-GaAs ohmic is clearly demonstrated [230]. The corresponding values for the conventional contacts realised using the Ni/AuGe/Ni/Au metalisation system, were as follows: Rt = 0.10Wmm, rc = 3.1e-5 Wcm2.

The values achieved for these parameters in case of the ITO/p+-GaAs contacts and their conventional counterparts fabricated using Au/Zn/Au metalisation system were Rt = 0.55Wmm, rc = 3.2e-5 Wcm2 (ITO); and Rt = 0.07Wmm, rc = 5.1e-6 Wcm2 (conventional) respectively. Although comparably good transparent ohmic contacts were achieved on p+-GaAs substrates, the increased difference between the transparent and their opaque counterparts is attributable to the absence of any obvious dopant species in the ITO contacts. Despite this absence, the main reason behind realising good p-type transparent ohmic contacts is likely to be due to the high substrate doping alone.

The results for the ITO/n+-InGaAs contacts and their conventional counterparts were as follows: Rt = 0.37Wmm, rc = 7.1e-5 Wcm2 (ITO); and Rt = 0.10 Wmm, rc = 3.1e-5 Wcm2 (conventional).

A brief surface morphology examination of the ITO contacts and subsequent comparison with the conventional metal contacts revealed some interesting results. It was seen that there was significant "balling-up" on the surface of the conventional contacts to the n+-GaAs substrates. The diameter of an average "mound" is approximately 5mm - comparable to, if not larger than, the dimensions involved in emitter finger widths of microwave HBTs. This effect is reduced but nevertheless it is still present in the p-type contact. By contrast, the metal on the ITO/n+-GaAs surface was smooth suggesting that there is no liquid phase reactions involved in the latter ohmic contact and ITO acts like a capping (such as Ti/Au) or a diffusion barrier (such as ZrB2) layer preventing the intermixing of the top-most Au layer with the substrate causing the balling effect. Its demonstrated excellent surface morphology and edge definition is an added advantage in the fabrication of small geometry optoelectronic devices. This observation is further correlated by the fact that Sn present in ITO is also known to take part in solid phase reactions to n-GaAs in the formation of good ohmic contacts. However, like other solid phase schemes, such as Pd/Ge or Pd/Sn, the resistance is higher than that obtained for the Ni/AuGe/Ni/Au liquid phase n-type contact.



7.6 Optically Transparent HPTs

The penultimate part of the study concerned the study of heterojunction bipolar transistors fabricated on three different material systems: AlGaAs/GaAs, InGaP/GaAs and InP/InGaAs respectively [231]. This was followed by realisation of their counterparts fabricated using transparent ITO as the emitter contact. The measured electrical (d.c.) properties of the HBTs were then analysed. At first a comparison between the opaque and transparent set of devices was made; this was followed by a comparison between the HBTs fabricated from the different material systems. This electrical performance analysis was followed by an extensive study of the suitability of these devices as phototransistors [232]; a very brief demonstrational work was performed to compare the results of vertical illumination versus edge illumination.

One of the consistent findings from the electrical study was that the emitter series resistance for the ITO emitter contact devices was higher than those with conventional metal contacts. This directly affected a number of other parameters of the transparent emitter contact transistors such as the offset voltage which was higher compared to their conventional counterparts. Further investigation revealed that the high series resistance could not be attributed to the resistance of the ITO layer or to the cap layer resistance alone. It also became apparent that the total contact resistance of the conventional devices also had other resistive components, albeit much less significant in comparison to the r.f. sputtered contacts. The additional resistance in the transparent contact must therefore be due to some sputter induced damage to layers deeper than the cap layer. It was also observed that the thin layer of In helps reduce this effect because preliminary devices without this intermediate metallic film had even larger Ree'. More detailed study is necessary to investigate this source of resistance and further reduction in the emitter resistance may be achieved by using a thicker layer of indium without causing significant reduction to the transmittance of the ITO contact.

A study of the Gummel plot showed that the overall reduction in Ic vs. Vbe in comparison with the metal contact devices again points to the likelihood of possible damage caused to the emitter layer during r.f. sputtering which was not fully recovered during the ohmic contact annealing. This deep damage results in an increased base ideality factor suggesting increased SCR recombination at the base-emitter junction and also possibly greater base bulk recombination; As a result, the measured d.c. gain, b is consistently lower for the ITO emitter contact devices.

A study involving the C-V measurements on both these sets of devices suggested that there was a noticeable change on the doping profiles of emitter layers in the HBTs due to r.f. sputtering and that this does indeed give rise to a donor like effect in the affected regions. Recall, this is consistent with the findings of the work on the ITO/n-GaAs Schottky photo diodes. Furthermore, as there is no significant change in the collector doping profile, it was assumed that the sputtering effects are confined before the collector layer. Since the C-V profiling technique cannot yield the doping profile of the already highly doped p+ GaAs base region, it is not possible to make definite conclusions based on these measurements about the effects of r.f. sputtering on that region.

A final feature of this work is the relationship between the effect of r.f. sputter induced damage on the base-emitter interface and the depth of this junction from the surface of the wafer. For example in the work with the InGaP/GaAs HBTs, it was seen that the base ideality factor for ITO contact devices fabricated on a wafer with a shallower base of 2725 (this figure being the sum of the cap and the emitter layers) is 1.25 in comparison to 1.09 of their opaque counterparts indicating presence of sputter induced damage giving rise to increased SCR recombination at the heterojunction; in contrast, the difference in the nIb between ITO and metal contact devices is insignificant for the wafer with the deeper base of 5000. These results were also consistent with the work on the AlGaAs/GaAs HBTs on two wafers with slightly different structures. The depth of the base/emitter hetero-interface for the InP/InGaAs was 4000 and thus the damage sustained is less than in devices with shallower base/emitter junctions. Recall, that the effect of sputter damage was not noticeable for the base interfaces deeper than 5000.

Like their InGaP/GaAs counterparts, the InP/InGaAs material system also offers the advantages associated with selective etching during device fabrication resulting in uniform device characteristics across the wafer; this desirable property is reduced in case of the AlGaAs/GaAs HBT fabrication where no suitable selective etchants are available. The InP/InGaAs HBTs fabricated in this study, a low common emitter offset voltage (measured when Ib ~ Ic ~ 0) of 61mV and collector/emitter breakdown voltage of 5.5V were observed. However, it was evident from the output characteristics that InP/InGaAs HBTs have rather poor saturation characteristics with high output conductance unlike the complete saturation observed in typical GaAs-based devices. This is due to the high multiplication factor and the low breakdown voltage associated with the low band gap of the InGaAs material.

In order to compare the turn on voltages, Vt, of the AlGaAs/GaAs HBTs, with typical InGaP/GaAs and InP/InGaAs HBTs, the collector currents of three devices with same geometries but different material systems were plotted as a function of base emitter voltage with Vbc = 0. It is seen that the InP/InGaAs HBTs exhibit a lower turn on voltage (0.2eV) compared to GaAs-based HBTs (0.8eV). This clearly demonstrates the advantage of InP- based HBTs for low power circuit applications, such as mobile telecommunications [199].

From a comparison of the respective gain plots of the devices on different material systems, it was evident that while the AlGaAs/GaAs b varied with Ic, the InGaP/GaAs showed little change with respect to Ic and the InP/InGaAs gain is almost independent of the collector current. This was attributed to the influence of various recombination processes in the base-emitter junctions of these devices and also the lower surface recombination velocity associated with the InGaAs material.

Optical output results showed that there is no degradation of the active substrate layers or the device characteristics as a result of r. f. sputtering used in the ITO deposition. It was also shown that a HPT can be controlled both optically and electrically or by a combination of both sources representing the potential to use a single device for the simultaneous detection and amplification of an optical signal as well as its subsequent coupling with an electrical signal in a single device. Much of the optical characterisation work was based only on the InP/InGaAs devices.

A notable feature of the output characteristic of the InP/InGaAs HBTs with ITO emitter contacts was the significant reduction in the collector offset voltage optical output of the photo transistor to 15mV from 60mV in its electrical mode of operation. This reduction is related to the absence of the finite base resistance in case of the optical mode where no active base contact is required.

In order to understand the relationship between the optical gain and the d.c. current gain, the responsivity of the base-collector p-n junction diode was measured and compared with the responsivity of the device operating under the three terminal device mode. A plot of the ratio of the responsivity of the InP/InGaAs HPT to the responsivity of the base-collector photo diode vs. optical power at l = 780 nm showed that this is approximately equal to b, in agreement with conventional analysis of photo transistor operation. Similar measurements were made for a set of AlGaAs/GaAs HPTs and found to confirm the relationship between the optical gain, the electrical gain b and the photo diode responsivity at a given wavelength.

The optical characterisations also involved the measurement and analysis of the spectral response of these novel HBTs with ITO emitter contacts over the relevant wavelength ranges. The AlGaAs/GaAs devices showed an operational range spanning over l = 450 to 900 nm while for the InGaAs/InP devices this was from 800nm to 1700 nm.

In both cases, the long wavelength cut-off is determined by the absorption edge of the narrow- bandgap base and collector. For In0.53Ga0.47As this corresponds to a wavelength of approximately 1650 nm. At shorter wavelengths (< 950 nm), the photoresponse is limited by absorption in the InP emitter as well as the ITO transmission and the monochromator grating efficiencies. The dip in the spectral response at around 1400nm corresponds to atmospheric absorption of radiation from the monochromator and is not a reflection of the device characteristic. This atmospheric absorption in the wavelength range 1340-1450nm is most likely due to moisture and CO2. The suitability of the InP/InGaAs devices for operation at 1310 nm and 1550 nm wavelengths was clearly demonstrated.

Finally, initial experiments comparing the benefits of edge coupling versus top coupling showed that up to 40% of the incident beam is lost in the former mode. Device structures need to be redesigned to suit the edge coupling mode. Further work is required to provide more quantitative analysis.



7.7 Spectral Response Model

A spectral response model was developed for the first time to understand, analyse and finally to optimise the performance range of these HBTs [233]. Device parameters such as the doping concentrations, the ITO and the semiconductor layer thickness as well as the material properties such as the absorption coefficients, a, the refractive indices, n, and the generation efficiency were used from the literature for the purpose of simulation. A 100% collection efficiency was assumed for any electron-hole pairs photo generated inside the depletion region or within a diffusion length in the neutral material. The spectral responses of the ITO/n-GaAs Schottky diodes and the AlGaAs/GaAs, InP/GaAs phototransistors are simulated and compared to measured data for the first time. In all cases, very good correlation between the model and the measured results were obtained [204].

The results presented in this thesis provide valuable insight into the use of optically transparent ITO for use in a wide range of optoelectronic devices as well as the respective optimisation. A list of publications arising from this work is presented in Appendix A.


1998: Shabbir A. Bashar (in accordance with paragraph 8.2d, University of London Regulations for the Degrees of M.Phil. and Ph.D., October 1997). The Copyright of this thesis rests with the author, and no quotation from it or information derived from it may be published without the prior written consent of the author.
Title Dedication Acknowledgements Abstract Symbols Contents

This page is hosted by Dr. Shabbir A. Bashar, e-mail: shabbir@betelco.com