Letter pubs.acs.


Nanosoldering Carbon Nanotube Junctions by Local Chemical Vapor Deposition for Improved Device Performance
Jae-Won Do,†,⊥ David Estrada,†,∥,¶ Xu Xie,‡ Noel N. Chang,§ Justin Mallek,§ Gregory S. Girolami,§,⊥ John A. Rogers,‡,§,∥,⊥ Eric Pop,†,∥,⊥,□ and Joseph W. Lyding*,†,⊥

Department of Electrical and Computer Engineering, ‡Department of Materials Science and Engineering and Frederick Seitz Materials Research Laboratory, §Department of Chemistry, ∥Micro and Nanotechnology Laboratory, ⊥Beckman Institute for Advanced Science and Technology, University of Illinois at Urbana−Champaign, Urbana, Illinois 61801, United States
S Supporting Information *

ABSTRACT: The performance of carbon nanotube network (CNN) devices is usually limited by the high resistance of individual nanotube junctions (NJs). We present a novel method to reduce this resistance through a nanoscale chemical vapor deposition (CVD) process. By passing current through the devices in the presence of a gaseous CVD precursor, localized nanoscale Joule heating induced at the NJs stimulates the selective and self-limiting deposition of metallic nanosolder. The effectiveness of this nanosoldering process depends on the work function of the deposited metal (here Pd or HfB2), and it can improve the on/off current ratio of a CNN device by nearly an order of magnitude. This nanosoldering technique could also be applied to other device types where nanoscale resistance components limit overall device performance. KEYWORDS: Carbon nanotubes (CNT), nanosoldering, intertube junctions, electrical resistance, thermal resistance, local chemical vapor deposition (CVD)

ingle-walled carbon nanotubes (CNTs) can be thought of as one-dimensional cylinders of monolayer graphene. Semiconducting CNTs exhibit high carrier mobility1,2 and band gaps which vary inversely with diameter,3 whereas metallic CNTs can carry very high current densities.4 These properties make CNTs promising candidates as components in nanoelectronics.5,6 However, as-grown CNTs are a mixture of metallic and semiconducting types, which often hinders their practical applications. For instance, such mixtures do not have sufficiently high on/off current (ION/IOFF) ratios for low-power transistors, nor are they sufficiently metallic (i.e., independent of doping or gating) as interconnects. To address this challenge, there have been numerous attempts to eliminate metallic CNTs through electrical breakdown,7,8 diazonium functionalization,9,10 selective plasma etching,6,11 or by polymer wrapping and CNT sorting through ultracentrifugation.12 However, these methods require several postsynthesis processing steps that tend to contaminate or degrade the quality of the CNTs. An alternative approach is to find ways to enhance the performance of random networks of as-grown carbon nanotube networks (CNNs). Such networks are easy to fabricate and transfer to arbitrary substrates, which make them attractive for applications in integrated circuits and display drivers on flexible or transparent substrates, especially because CNNs have shown higher carrier mobility than organic or amorphous silicon thinfilm transistors.13,14 Sun et al.13 have recently improved the performance of CNN devices through control of the CNN
© 2013 American Chemical Society


morphology and have achieved ION/IOFF ratios of ∼106 and carrier mobilities of ∼20 cm2 V−1 s−1. One of the challenges associated with CNNs is that the performance and reliability may be limited by high electrical15−19 and thermal20−23 resistances of CNT−CNT internanotube junctions (NJs). Such resistances depend on the CNT−CNT separation and overlap, which affect the hopping probability of charge carriers and consequently the junction resistances.18,19 From an electrical point of view, the current transport is further limited by Schottky barriers at the junctions between metallic and semiconducting CNTs.24,25 These junction resistances are at least an order of magnitude higher than those of individual CNTs.15−17 Thus, local power dissipation at these junctions will dramatically degrade the overall device performance.21,26 To address this issue, several studies have sought to improve the junction resistance by depositing metal particles at the NJs using electron beam induced deposition27 and dip-pen nanolithography facilitated by atomic force microscopy (AFM).28 While elegant, these methods are slow, requiring one to locate individual junctions to deposit metal nanoparticles in a serial fashion. Other studies have shown improvements in the sheet resistance of CNNs by employing selective nucleation of fullerenes at the NJs29 and by treating CNNs with nitric acid and doping both the CNTs and the
Received: July 15, 2013 Revised: October 16, 2013 Published: November 11, 2013
dx.doi.org/10.1021/nl4026083 | Nano Lett. 2013, 13, 5844−5850

owing to its high work function and favorable interaction with CNT sidewalls. The process is repeated (4) at orthogonal directions to achieve CNT arrays with crossbar orientation. and (3) applying an elastomeric stamp to transfer the resulting CNT/Au/PI layer to a receiving substrate. the temperature rise of the NJs is significantly higher than the average device temperature. (a) Schematic diagram of a CNN device with red dots illustrating heated NJs under VDS. which acts as a global back-gate. 5844−5850 . which reduces their resistance and improves the overall CNN device performance. aligned CNTs were initially grown on quartz substrates by CVD methods described elsewhere33.32 In this study.35. (c) Schematic illustration of transferring aligned CNTs for crossbar devices as (1) aligned CNTs grown on quartz by CVD. the details of these improvements in terms of electronic properties specific to transistor applications.40 This change for our devices before and after oxygen desorption is shown by the transfer characteristics (IDS versus VGS with VDS = 50 mV) and band diagrams in Figure 2c.36 Figure 1c shows schematic illustrations of the preparation of the CNT crossbar devices.5 nm Ti (an adhesion layer for the SiO2 substrate) topped with 40−80 nm Pd. large area CNNs and CNT crossbar devices. which forms ohmic contacts to CNTs. followed by removal of the stamp and Au/PI layer.26.1021/nl4026083 | Nano Lett.37 Individual 5845 devices were then wirebonded to metal leads of a chip carrier.41 causing conversion to n-type behavior in high vacuum. Recent transport studies of CNNs have shown that.)41. We use test devices with two different geometries in our experiments.39 and in the Supporting Information.40 (It is well-known that devices made of as-grown CNTs exhibit p-type behavior in air due to oxygen adsorption along the CNT and at the CNT − metal contacts. Standard photolithography and electron beam evaporation were used to define metal electrodes. thereby passing currents through the CNT devices to desorb all remnant oxygen molecules. junctions. the latter consisted of 0. entire samples were first loaded and kept in a vacuum chamber (∼10−6 Torr or lower) for several hours. The net result is nanosoldering the NJs. during device operation.31 These findings indicate that nanoscale hot spots form at NJs throughout the CNN (Figure 1a).Nano Letters Letter Figure 1. followed by (2) deposition of a carrier film of Au and polyimide (PI) layers.42 Oxygen removal lowers the contact work function. After the samples were vacuum annealed and cooled to room temperature. The samples were vacuum annealed at 600 K for five minutes to desorb oxygen molecules from the CNTs and the metal electrodes.30 However. Additional details about our device fabrication can be found in our previous papers34. (b) False-colored SEM images showing (left) CNNs bridging the drain and source electrodes and (right) crossbar CNT test device.org/10. These additional heating steps were repeated until there was no discernible change in the transfer characteristics of the devices. the individually wirebonded devices were additionally heated by applying various voltages between the source and drain electrodes. such as mobility and ION/IOFF ratio.34 and subsequently transferred onto SiO2 (200 nm) with a highly doped Si substrate at orthogonal directions to achieve welldefined NJs.38. 2013. we utilize these nanoscale hot spots to locally deposit metals via chemical vapor deposition (CVD). as shown in Figure 1b. remained unexplored. In order to perform nanoscale CVD and nanosolder the NJs.26 For CNT crossbar devices. The oxygen removal step is carried out in order to clearly observe any change in the current transport in our device that may arise from nanosoldering the NJs.doi. Figure 2a shows the process flow for nanosoldering the NJs and Figure 2b shows the schematic diagram of our vacuum system for the CVD reactions. After the transfer dx. The CNNs were grown by CVD of methane gas with ferritin catalysts on SiO2 (90 or 300 nm) with a highly doped Si substrate. a conclusion that is supported by recent simulations. 13.

we take ION at a constant 5846 VGS overdrive from the forward sweep (VGS − VTH.44 respectively. like Pd. These results indicate that the ION was improved by a factor of ∼6. the samples were removed from the vacuum system and exposed to the ambient atmosphere for sufficient time (over 24 h) to allow readsorption of oxygen molecules. In order to calculate the ION/IOFF ratio. Corresponding energy band diagrams at the metal−CNT interface are shown in the insets of each graph. leading to ION/IOFF ratio improvement by a factor of ∼8.52. The approximate CVD reactions of each precursor are given by the following equations43.42. (a) Process flow for nanosoldering NJs.47 Note that for devices with IOFF lower than the measurement limit. The two false-colored electrodes in red were used to pass current through the CNTs and electrodes in blue were left floating. either C5H5PdC3H5 or Hf(BH4)4. Please refer to Figure S2b in dx. Both precursors have relatively high-vapor pressures (∼30 Torr at 25 °C for C5H5PdC3H5 and ∼15 Torr at 25 °C for Hf(BH4)4).REV = 0. the IOFF was found by averaging currents in the regions with fluctuations in the off state below VTH. we varied the applied voltages over specific time periods to deposit Pd or HfB2 at the locally heated NJs. the improvement in ION is indicative of an increase in the average device mobility by a factor of ∼6. The ION/IOFF ratios were subsequently measured to monitor changes resulting from metal deposition. the background pressure of the CVD chamber was about 1−5 × 10−6 Torr. 2013. 5844−5850 . 13. We also note that there was no significant effect on the threshold voltage hysteresis (ΔVTH.1021/nl4026083 | Nano Lett. The arrows indicate the VGS sweep direction. Figure 3b shows the transfer characteristic curves before and after Pd deposition for the device shown in Figure 3a. Note that positive VGS is used while varying VDS in order to pass a high current because devices are now n-type. while the IOFF (averaged in the regions indicated by black arrows) was lowered by a factor of ∼1. Finally.43. characteristics stabilized. The left inset depicts hole injection into the CNT when a high work function metal. was introduced into the chamber until a total pressure of about 10−4 Torr was achieved to deposit Pd and metallic HfB2.Nano Letters Letter Figure 2.FWD − VTH. they were kept in sealed stainless steel and glass containers under argon and stored in an ice bath or in a refrigerator at −20 °C until use.doi. (c) Transfer characteristics of a CNN device (left) in air and (right) in vacuum after oxygen removal steps from the device. contacts the CNT and the device is operated in air with VGS < 0 V (p-type behavior). suggesting that Pd nanosoldering does not introduce new trap states near the CNT-SiO2 interface. and VDS was applied from 5 to 35 V for three seconds. Once the pressure in the CVD chamber stabilized. if we assume the current paths between source and drain electrodes remain unchanged (at a constant VGS overdrive) before and after Pd deposition.015 V). Figure 3a shows scanning electron microscope (SEM) images of a CNT crossbar device with well-defined NJs before and after Pd deposition. a singlesource CVD precursor.43.46 After introduction of the precursors into the chamber.2 Thus.45 C5H5PdC3H5 (g) → Pd (s) + C5H5C3H5 (g) Hf(BH4)4 (g) → HfB2 (s) + B2H6 (g) + 5H 2 (g) (1) (2) Because the precursors are air sensitive. The right inset depicts electron injection into the CNT when the oxygen molecules are desorbed off from the metal surface and CNTs in vacuum and VGS > 0 V is applied (n-type behavior). VGS was applied up to 15 V in order to “turn on” both metallic and semiconducting CNTs.org/10. The ION/IOFF ratios were again measured to assess the effects of nanosoldering the NJs on the p-type characteristics of the devices. (b) Schematic diagram of vacuum system for our nanoscale CVD process.FWD = −10 V) and take IOFF as the minimum IDS from the same transfer curve (see Supporting Information) in order to better compare performance of different devices by comparing them at similar charge densities and to reduce variability due to VTH shift.

is used to connect two semiconducting CNTs at a NJ with Pd electrodes and (bottom) back-to-back pnp junctions when low work function metal. Pd is used for both the source and drain electrodes. Instead.52 Once 5847 Figure 4. Please refer to Figure S2b in the Supporting Information for n-type transfer characteristic curves in vacuum. We note that even though a large improvement in the ION/IOFF ratio was observed.4.1021/nl4026083 | Nano Lett. We attribute the increase in ION to higher charge carrier hopping probability at the NJs. In the devices we studied. Post characterization with SEM and AFM (see Figure S5 in Supporting Information) indicate that Pd nanoparticles from sub-10 nm to over 30 nm in size were deposited on the NJs.Nano Letters Letter Figure 3. like Pd. Energy band diagrams at the metal−CNT interface showing (a) (top) back-to-back p-type junctions when high work function metal. the nanosoldering was deliberately carried out with high currents for longer times (up to 30 s) on other similar devices to deposit a larger amount of Pd. Figure 4 shows the schematic band diagrams for nanosoldered NJs between semiconducting CNTs. their resistance decreases and they cool. thus stopping the nanosoldering process. a slight increase in contrast along some CNTs near the NJs was observed after Pd deposition as can be seen in Figure 3a. and the CNTs form percolation paths between the two electrodes. the IDS−VGS characteristics remained about the same or even degraded after these control experiments (see Supporting Information). As Pd is deposited at the NJs. The decrease in IOFF may result from a heightened Schottky barrier for electrons in the off state. For a majority of devices we tested. On a single device. 2013. In order to confirm that Pd was deposited on the NJs.51.1−5. before and after Pd deposition. The red and blue arrows indicate the VGS sweep direction. nanosoldering the NJs with Pd will also induce p-type behavior at these NJs. These experiments allowed us to test the possibility that the improvement in device performance was due to factors other than nanosoldering. Additional control experiments were performed on similar crossbar and CNN devices that were annealed in vacuum and subjected to the similar set of deposition conditions without actually introducing any precursor into the chamber. Blue electrodes were left floating. (a) (Left) SEM image of crossbar CNT device before Pd deposition where current was passed between the two false-colored red electrodes to heat the NJs. 5844−5850 . The right-hand images are magnified views of the region indicated by the yellow dotted box. the area available for carrier flow is increased and the energy barrier is lowered.org/10. we saw an ION/IOFF ratio improvement of a factor of ∼2. the Supporting Information for n-type transfer characteristic curves in vacuum. Note that the IOFF was found by averaging the current in the regions indicated by black arrows. possibly due to the elimination of contaminants on CNTs or thermal annealing dx. (Right) Zoomed-in NJs indicated by yellow dotted box in the left image (top) before and (bottom) after Pd deposition showing traces of Pd along CNTs near the NJs. these NJs are soldered. and semiconducting-metallic CNTs.)48−50 Therefore. (b) (Left) linear and (right) log scale transfer characteristics of the CNN device before and after Pd deposition with VDS = 1 V.9 eV. 13. like HfB2. (b) Energy band diagrams when (top) Pd and (bottom) HfB2 are used to connect two metallic CNTs at a junction. and the lowered Schottky barrier at the valence band edge and increased Schottky barrier for electrons in the off state will lead to a large improvement in the overall device performance. metallic CNTs. and thus lowered junction resistance.doi. we did not find any large Pd particles after nanosoldering (see Figure 3a). (c) Energy band diagrams showing (top) p-type junction when Pd is used to connect metallic and semiconducting CNTs at a NJ and (bottom) pn junction when HfB2 is used to connect CNTs. CNT contacts to Pd electrodes induce p-type behavior at the source and drain because Pd has a high work function (ΦPD = 5. We speculate that only a very small amount of Pd is needed to connect the CNTs at the NJs because Pd is known to wet CNTs very well. The deposited material was also verified to be Pd by elemental analysis using energy dispersive X-ray spectroscopy (EDS). is used to connect CNTs.

we were able to nanosolder this same device with Pd after the control experiment and improve the ION by a factor of ∼5.. charge transfer occurs from the metal to the CNT and creates a Schottky barrier at the valence band edge. 5844−5850 .org/10. For more details on these devices. Pd.g. Note that there was little change on the threshold voltage hysteresis (ΔVTH. By matching the work function of the electrode with the metallic nanosolder (e. dx.doi. In conclusion. Thus the decreased IOFF after Pd deposition in our devices suggests that nanosoldering Pd is indeed playing a role at the NJs. we improved the ION/IOFF ratio of our devices by nearly an order of magnitude. we achieved nanoscale CVD of metallic nanoparticles at NJs by passing current through devices like CNNs and CNT crossbars to selectively heat the NJs. the resistance will not drop as much due to the work function mismatch and the poor interface between HfB2 and CNTs (compared to Pd which wets CNTs very well) and thus the nanosoldering process will continue.Nano Letters of the contacts from the heat generated during current flow. The stable current during the device operation and consistent transfer curves in Supporting Information Figure S3 show that our technique does not suffer from stability issues such as electromigration or oxidation. and the next most-resistive NJs will undergo nanosoldering. we have not observed any device for which IOFF decreases after a control experiment conducted without the CVD precursor.2 We tested several other devices with similar channel geometries. We believe that when HfB2 is deposited at these NJs. The self-limiting nature of the nanosoldering process means that the NJs cool as they are soldered. Figure 6c shows a histogram that summarizes the degree of improvement in the ION/IOFF ratio (ION/IOFF. (b) Energy dispersive X-ray spectroscopy (EDS) spectra from HfB2 deposited on NJs (red) and on CNTs in the same device where no HfB2 was deposited (blue). and found the device performance either showed less improvement or could even be degraded (see Supporting Information for more data).REV = 0. please refer to Figure S4 in Supporting Information. 13. making much larger islands. 2013.9 while decreasing the IOFF by a factor of ∼1. we then used the precursor Hf(BH4)4 to deposit HfB2 at the NJs.4. by using Pd).25 (see Supporting Information).FWD − VTH. We chose the precursor Hf(BH4)4 because the resultant HfB2 has a high melting point (3250 °C) and excellent electrical properties:43 a resistivity of ∼15 μΩ·cm and a low work function (ΦHfB2 ≈ 3. EDS measurements confirm the presence of hafnium: the red curve in Figure 5b shows the EDS spectrum obtained from a bright island formed at a NJ. When a low work function metal comes in contact with a semiconducting CNT. Figure 6b shows the transfer characteristics of this device before and after HfB2 deposition where the ION/IOFF ratio was improved by ∼24% using our nanosoldering technique. In order to clarify the effect of the nanosolder work function. leading to the overall performance improvement of another factor of ∼8.BEFORE) for the control. (a) SEM images of CNNs (left) before and (right) after nano-CVD of HfB2. Notably.AFTER/ ION/IOFF. large HfB2 particles were visible after nanosoldering the junctions (see Figures 5 and 6). suggesting that HfB2 nanosoldering does not introduce new trap states. We also note that. inducing n-type behavior at the contact as shown in Figure 4. Figure 6a shows SEM images of another CNN device before and after HfB2 deposition. Therefore. We believe that the difference in the work function of the electrode metal. HfB2-deposited. Data regarding the presence of boron are provided in the Supporting Information. In order to test the stability of the improved junctions with time.1021/nl4026083 | Nano Lett. we also performed time-dependence measurements in which current was passed through one of our nanosoldered devices for more than 20 h (see Figure S3 in Supporting Information). The drain and source electrodes are false-colored in red and the deposited HfB2 is false-colored in yellow. However. The bright islands in the figure indicate that HfB2 has been deposited primarily at crossed NJs. HfB2. The yellow circles indicate regions where HfB2 was deposited on the NJs.5 eV). while p-type behavior is induced at CNT contacts to the source and drain electrodes because Pd has a high work function. plays a role here.53 Figure 5a shows SEM images of a CNN device before and after HfB2 nanosoldering. n-type behavior is induced in the middle of the CNT percolation paths between the source and drain electrodes. and Pddeposited devices. We also note that a few Letter Figure 5. This mismatch of work functions will create back-to-back pnp junctions within the CNN for HfB2 nanosoldered junctions.23 V). as well as CNT crossbar devices. vividly highlighting the most conductive current pathways that heat up during device operation. when the NJs are nanosoldered with HfB2. whereas the blue curve shows the EDS spectrum obtained from CNTs in the same device away from the bright island under the same acquisition conditions. and the deposited metal. unlike the Pd case. The nanosoldering technique may be generally applicable to improve the performance of other materials and devices. This process results in self-aligned and self-limiting nanosoldering that reduces the junction resistance and improves the device transport properties. which can degrade the current transport of the device. 5848 CNTs are coated with HfB2 along almost their entire lengths.

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