Electrical Characterization of Graphite Oxideby Ira
JewellAbstractExperimental DesignResultsFuture WorkSince the
discovery in 2004 that single atomic planes of graphite could exist
individually [1], there has been much interest in this
two-dimensional material known as graphene. The original technique
for isolating graphene was simply micro-mechanical cleavage from
bulk HOPG (highly-oriented pyrolitic graphite) with the sticky-tape
method being among the most successful innovations. With this
technique, the experimenter repeatedly divides a piece of HOPG
using regular Scotch tape and presses it against a substrate
(usually Si oxidized to a specific thickness to ensure maximal
visibility of graphenes) and transfers it with gentle rubbing.
While this method does transfer single and few-layer graphenes, it
also transfers many larger graphitic particles (as seen in this
slides background) and finding the desired material is much like
finding the needle in the haystack.
Alternative, chemical, methods for isolating graphene have been
pursued and this work intends to follow one of the most popular. In
this method, graphite oxide (GO) is first synthesized. For this we
used the technique of Hummers as modified by Kovtyukhova [2]. This
graphite oxide is hydrophilic and readily disperses in water with
ultrasonic agitation. Single-layer platelets can then be isolated
by centrifugation. The resulting product is sprayed onto a heated
substrate so that it flash evaporates, leaving a distribution of
platelets. These GO platelets are non-conductive and not of much
use, but under certain conditions they can be made to conduct.
We propose to use direct-write laser lithography to define
four-point resistivity structures atop individual single-layer GO
platelets. The number of atomic layers in the samples will be
characterized using both atomic force microscopy (AFM) and Raman
spectroscopy. Resistivity measurements will be taken in situ as the
GO sample is exposed to a variety of reducing gasses over a range
of temperatures. We have already shown the possibility of
increasing the conductivity of a sample by several orders of
magnitude (using two-point contact measurements on a multi-layered
sample) and hope to refine our technique to produce device-quality
graphenes by this method in the near future.Why is Graphene
Interesting?Single-layer graphene is interesting for a large number
of reasons, both theoretical and practical. Perhaps the most unique
feature of graphene lies in its bandstructure. At certain points in
reciprocal space the conduction band and the valence band actually
touch, making graphene a zero-bandgap semiconductor. Even stranger,
in the region of k-space near these points the dispersion is
linear.References[1] Novoselov. Science. 306, 666 (2004)[2]
Kovtyukhova. Chemistry of Materials. 11, 771 (1999)[3] Geim.
Physics Today. 60 (Issue 8), 35 (2007)[4] Novoselov. Nature. 438,
197 (2005)[5] Zhang. Nature. 438, 201 (2005)[6] Nishioka. Applied
Physics Letters. 90, 252505 (2007)[7] Gilje. Nano Letters. 7, 3394
(2007)[8] Gomez-Navarro. Nano Letters. 7, 3499 (2007)Bandstructure
of single-layer graphene [3]To a physicist, this is interesting
because it forces the (conduction) electrons in graphene to behave
as massless Dirac fermions and not like an ordinary electron at
all. These electrons possess zero rest mass and travel with a
constant velocity 106 m/s [4]. In addition, graphene displays such
exotic effects as the anomalous (half-integer) quantum Hall effect
and a nonzero Berrys phase [5].To an engineer, this is interesting
because the number and type of carriers (electrons or holes) can be
tuned by application of an electric field. Moreover, both carrier
types have quite high mobilities ( 10,000 cm2/V-s) even with
carriers approaching concentrations as high as the theoretical
limit 7*1012 cm-2. Graphenes high mobililty, coupled with the fact
that its conductivity can be smoothly modulated by application of
an electric field through a gate electrode, make it an attractive
material for FET applications.
Hall coefficient (which is inversely proportional to carrier
concentration) as function of applied field [1]A solution of
graphite oxide was first prepared according to the method of
Hummers as modified by Kovtyukhova [2]. The solution was filtered
and allowed to dry, forming GO paper. The graphite oxide was then
resuspended in solution and exfoliated by stirring for several
days.A Heidelberg DWL66fs laser lithography system was used to
pattern photoresist atop a Si wafer substrate (with 300nm thermally
grown SiO2 to enhance visibility of graphenes). The pattern is a
repeating grid of four-point measurement structures consisting of
1m wide lines connecting to larger (90m x 90m) pads for probing or
wirebonding. Gold (~100nm) and a thin chrome adhesion layer (~5nm)
was then deposited using thermal evaporation. Liftoff was performed
using acetone and ultrasonic agitation to remove the undeveloped
photoresist, thus defining the metal contact structures. The
substrate was then heated on a hotplate and the solution of GO
spray deposited as a fine mist so that the droplets
flash-evaporate. This is necessary because the GO is hydrophilic
and would agglomerate if larger drops were used [7]. The substrates
were then analyzed by optical microscope to find samples that have
by chance landed in the correct place (spanning all four probes of
a measurement structure)Unfortunately, results from this current
design have not yet been obtained (see Future Work below). We have,
however, shown with two-point measurements of rather thick samples
of graphite oxide that the resistance of the sample can be
significantly reduced by simple exposure to a forming gas ambient
at an elevated temperature (300C)The resistance (inverse slope of
plots shown) is seen to decrease dramatically after
reduction.AcknowledgementsI would like to thank Dr. Albrecht
Jander, Chris Tasker, Sean Smith, and Chien-Chih Huang. This
project is funded by the Army Research Labs contract #/280710A/
Once characterized by AFM, the next step is to connect each of the
90m pads (of the structure with the correctly situated GO sample)
to larger contact pads via wirebonding. We will use a Mech-El 827
manual bonder.Finally, the appropriate electrical connections will
be made, and the entire substrate placed in a ProboStat measurement
cell so that resistivity can be monitored in situ as reducing
gasses are flowed and temperature is varied.The next step in the
project is to characterize each of the potential samples of GO,
keeping only those with one or two layers. We will use atomic force
microscopy, as step height profiles can reveal the number of layers
in the sample. AFM image of single folded sheet of GO [8]To a
magnetician, graphene is interesting because spins can remain
coherent over long distances because of the long times between
scattering events. This makes graphene a good candidate material
for spintronics applications. One group of researchers have
demonstrated the spin valve effect with a sample of several-layer
graphene forming the spacer layer between a pair of Cobalt
contacts. The magnetic electrodes were separated by 500nm and the
experiment can be taken as evidence that the spinformation
contained in the injected electron survives at least that distance.
Spin valve effect showing lower resistance state when the direction
of magnetization of the two electrodes are aligned. [6]
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Volts
Amps
sample #2 (reduced)
y = 5E-06x + 3E-09
JIS12B
DiodeVf-If
VF=-2to2in0.01step
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2430.422.08E-06
2440.432.13E-06
2450.442.18E-06
2460.452.23E-06
2470.462.28E-06
2480.472.33E-06
2490.482.38E-06
2500.492.43E-06
2510.52.48E-06
2520.512.53E-06
2530.522.58E-06
2540.532.63E-06
2550.542.68E-06
2560.552.73E-06
2570.562.78E-06
2580.572.83E-06
2590.582.88E-06
2600.592.93E-06
2610.62.97E-06
2620.613.03E-06
2630.623.08E-06
2640.633.12E-06
2650.643.17E-06
2660.653.23E-06
2670.663.27E-06
2680.673.32E-06
2690.683.37E-06
2700.693.42E-06
2710.73.47E-06
2720.713.52E-06
2730.723.57E-06
2740.733.62E-06
2750.743.67E-06
2760.753.72E-06
2770.763.77E-06
2780.773.82E-06
2790.783.87E-06
2800.793.92E-06
2810.83.97E-06
2820.814.02E-06
2830.824.07E-06
2840.834.11E-06
2850.844.17E-06
2860.854.22E-06
2870.864.26E-06
2880.874.32E-06
2890.884.37E-06
2900.894.41E-06
2910.94.46E-06
2920.914.52E-06
2930.924.56E-06
2940.934.61E-06
2950.944.67E-06
2960.954.71E-06
2970.964.76E-06
2980.974.81E-06
2990.984.86E-06
3000.994.91E-06
30114.96E-06
3021.015.01E-06
3031.025.06E-06
3041.035.11E-06
3051.045.16E-06
3061.055.21E-06
3071.065.26E-06
3081.075.31E-06
3091.085.36E-06
3101.095.40E-06
3111.15.46E-06
3121.115.51E-06
3131.125.55E-06
3141.135.61E-06
3151.145.66E-06
3161.155.70E-06
3171.165.75E-06
3181.175.81E-06
3191.185.85E-06
3201.195.90E-06
3211.25.96E-06
3221.216.00E-06
3231.226.05E-06
3241.236.11E-06
3251.246.15E-06
3261.256.20E-06
3271.266.25E-06
3281.276.30E-06
3291.286.35E-06
3301.296.40E-06
3311.36.45E-06
3321.316.50E-06
3331.326.55E-06
3341.336.60E-06
3351.346.65E-06
3361.356.69E-06
3371.366.75E-06
3381.376.80E-06
3391.386.84E-06
3401.396.90E-06
3411.46.95E-06
3421.416.99E-06
3431.427.04E-06
3441.437.10E-06
3451.447.14E-06
3461.457.19E-06
3471.467.25E-06
3481.477.29E-06
3491.487.34E-06
3501.497.40E-06
3511.57.45E-06
3521.517.49E-06
3531.527.54E-06
3541.537.60E-06
3551.547.64E-06
3561.557.69E-06
3571.567.75E-06
3581.577.79E-06
3591.587.84E-06
3601.597.89E-06
3611.67.94E-06
3621.617.98E-06
3631.628.04E-06
3641.638.09E-06
3651.648.13E-06
3661.658.19E-06
3671.668.24E-06
3681.678.28E-06
3691.688.33E-06
3701.698.39E-06
3711.78.44E-06
3721.718.48E-06
3731.728.54E-06
3741.738.59E-06
3751.748.63E-06
3761.758.69E-06
3771.768.74E-06
3781.778.78E-06
3791.788.84E-06
3801.798.89E-06
3811.88.93E-06
3821.818.98E-06
3831.829.04E-06
3841.839.08E-06
3851.849.13E-06
3861.859.19E-06
3871.869.24E-06
3881.879.28E-06
3891.889.33E-06
3901.899.39E-06
3911.99.42E-06
3921.919.48E-06
3931.929.54E-06
3941.939.58E-06
3951.949.63E-06
3961.959.69E-06
3971.969.73E-06
3981.979.77E-06
3991.989.84E-06
4001.999.88E-06
40129.92E-06
JIS12B
Volts
Amps
sample #2 (reduced)
y = 5E-06x + 3E-09
Chart1
0
0
0
0
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0
Volts
Amps
sample #2
y = 4E-13x - 1E-13
JIS12A
DiodeVf-If
VF=0to4in0.01step
NO.VFIF
VA
102.10E-13
20.011.20E-13
30.021.70E-13
40.031.30E-13
50.041.20E-13
60.051.50E-13
70.061.00E-13
80.076.00E-14
90.089.00E-14
100.091.60E-13
110.11.40E-13
120.112.70E-13
130.122.80E-13
140.132.40E-13
150.142.30E-13
160.152.00E-13
170.162.60E-13
180.174.00E-14
190.181.20E-13
200.196.00E-14
210.26.00E-14
220.211.70E-13
230.221.40E-13
240.238.00E-14
250.241.20E-13
260.251.60E-13
270.261.80E-13
280.273.20E-13
290.281.30E-13
300.29-1.00E-14
310.31.60E-13
320.311.40E-13
330.321.10E-13
340.331.70E-13
350.341.20E-13
360.352.40E-13
370.368.00E-14
380.371.50E-13
390.381.80E-13
400.391.60E-13
410.41.20E-13
420.411.30E-13
430.421.40E-13
440.431.80E-13
450.447.00E-14
460.451.50E-13
470.461.00E-13
480.471.90E-13
490.481.50E-13
500.491.60E-13
510.52.00E-14
520.512.00E-14
530.521.90E-13
540.532.10E-13
550.541.90E-13
560.551.60E-13
570.561.80E-13
580.571.00E-13
590.581.80E-13
600.591.70E-13
610.61.70E-13
620.611.10E-13
630.621.80E-13
640.632.10E-13
650.641.30E-13
660.651.50E-13
670.661.30E-13
680.671.20E-13
690.681.50E-13
700.691.50E-13
710.77.00E-14
720.712.40E-13
730.721.60E-13
740.733.00E-13
750.741.00E-13
760.753.10E-13
770.761.60E-13
780.772.30E-13
790.789.00E-14
800.791.90E-13
810.81.30E-13
820.811.80E-13
830.821.30E-13
840.831.90E-13
850.841.20E-13
860.852.30E-13
870.861.80E-13
880.871.10E-13
890.881.90E-13
900.892.90E-13
910.92.20E-13
920.912.20E-13
930.921.20E-13
940.932.00E-13
950.942.00E-13
960.951.40E-13
970.962.40E-13
980.971.40E-13
990.982.90E-13
1000.992.40E-13
10111.70E-13
1021.012.90E-13
1031.021.70E-13
1041.031.80E-13
1051.042.60E-13
1061.053.10E-13
1071.062.40E-13
1081.071.80E-13
1091.081.90E-13
1101.091.80E-13
1111.13.40E-13
1121.112.50E-13
1131.121.80E-13
1141.132.20E-13
1151.142.20E-13
1161.152.40E-13
1171.161.50E-13
1181.172.80E-13
1191.181.90E-13
1201.192.50E-13
1211.22.70E-13
1221.212.00E-13
1231.222.40E-13
1241.231.30E-13
1251.242.50E-13
1261.252.60E-13
1271.262.50E-13
1281.272.40E-13
1291.283.60E-13
1301.292.60E-13
1311.31.60E-13
1321.313.00E-13
1331.322.00E-13
1341.332.50E-13
1351.342.70E-13
1361.353.00E-13
1371.362.30E-13
1381.372.30E-13
1391.383.20E-13
1401.392.00E-13
1411.42.00E-13
1421.413.10E-13
1431.422.30E-13
1441.432.10E-13
1451.443.90E-13
1461.452.80E-13
1471.462.70E-13
1481.473.20E-13
1491.483.30E-13
1501.493.50E-13
1511.52.10E-13
1521.512.30E-13
1531.523.20E-13
1541.533.70E-13
1551.542.70E-13
1561.553.00E-13
1571.561.00E-13
1581.572.70E-13
1591.583.00E-13
1601.593.60E-13
1611.63.80E-13
1621.612.90E-13
1631.623.30E-13
1641.632.80E-13
1651.643.60E-13
1661.652.70E-13
1671.663.70E-13
1681.673.30E-13
1691.683.90E-13
1701.694.30E-13
1711.73.40E-13
1721.713.80E-13
1731.723.70E-13
1741.733.60E-13
1751.743.00E-13
1761.754.50E-13
1771.764.50E-13
1781.774.00E-13
1791.784.00E-13
1801.794.70E-13
1811.83.50E-13
1821.814.30E-13
1831.824.20E-13
1841.834.90E-13
1851.843.30E-13
1861.854.90E-13
1871.864.40E-13
1881.875.30E-13
1891.884.30E-13
1901.894.80E-13
1911.93.80E-13
1921.914.00E-13
1931.925.40E-13
1941.935.00E-13
1951.945.10E-13
1961.954.80E-13
1971.964.80E-13
1981.973.50E-13
1991.985.00E-13
2001.995.60E-13
20125.40E-13
2022.016.20E-13
2032.025.60E-13
2042.034.90E-13
2052.045.40E-13
2062.055.40E-13
2072.064.90E-13
2082.075.80E-13
2092.084.70E-13
2102.095.10E-13
2112.15.60E-13
2122.115.60E-13
2132.125.10E-13
2142.135.40E-13
2152.145.60E-13
2162.156.30E-13
2172.166.10E-13
2182.175.20E-13
2192.186.40E-13
2202.195.50E-13
2212.26.50E-13
2222.215.10E-13
2232.226.30E-13
2242.236.10E-13
2252.245.10E-13
2262.256.60E-13
2272.264.00E-13
2282.275.00E-13
2292.285.60E-13
2302.296.40E-13
2312.38.30E-13
2322.316.40E-13
2332.325.80E-13
2342.335.80E-13
2352.346.80E-13
2362.357.60E-13
2372.366.80E-13
2382.378.70E-13
2392.387.10E-13
2402.397.20E-13
2412.48.00E-13
2422.416.40E-13
2432.426.80E-13
2442.436.20E-13
2452.448.30E-13
2462.456.50E-13
2472.466.90E-13
2482.478.30E-13
2492.487.70E-13
2502.496.90E-13
2512.58.20E-13
2522.517.00E-13
2532.526.70E-13
2542.537.60E-13
2552.548.80E-13
2562.557.90E-13
2572.568.70E-13
2582.577.70E-13
2592.589.30E-13
2602.599.70E-13
2612.67.90E-13
2622.618.10E-13
2632.628.40E-13
2642.637.10E-13
2652.647.50E-13
2662.658.30E-13
2672.668.30E-13
2682.678.10E-13
2692.687.40E-13
2702.691.08E-12
2712.79.30E-13
2722.718.20E-13
2732.728.60E-13
2742.738.40E-13
2752.748.90E-13
2762.758.80E-13
2772.768.30E-13
2782.779.40E-13
2792.781.09E-12
2802.791.02E-12
2812.88.40E-13
2822.818.40E-13
2832.828.50E-13
2842.839.80E-13
2852.849.70E-13
2862.851.07E-12
2872.869.60E-13
2882.871.03E-12
2892.889.40E-13
2902.891.03E-12
2912.98.60E-13
2922.919.70E-13
2932.929.20E-13
2942.939.70E-13
2952.949.60E-13
2962.958.80E-13
2972.969.40E-13
2982.979.20E-13
2992.981.14E-12
3002.991.02E-12
30131.11E-12
3023.011.06E-12
3033.021.00E-12
3043.039.40E-13
3053.049.20E-13
3063.051.08E-12
3073.061.04E-12
3083.079.70E-13
3093.081.06E-12
3103.099.80E-13
3113.11.03E-12
3123.111.20E-12
3133.121.06E-12
3143.131.27E-12
3153.141.13E-12
3163.151.04E-12
3173.161.00E-12
3183.171.13E-12
3193.181.21E-12
3203.191.16E-12
3213.21.13E-12
3223.211.21E-12
3233.221.06E-12
3243.231.18E-12
3253.241.16E-12
3263.251.16E-12
3273.261.17E-12
3283.271.20E-12
3293.281.04E-12
3303.291.28E-12
3313.31.19E-12
3323.311.24E-12
3333.321.18E-12
3343.331.32E-12
3353.341.20E-12
3363.351.27E-12
3373.361.27E-12
3383.371.32E-12
3393.381.28E-12
3403.391.28E-12
3413.41.28E-12
3423.411.28E-12
3433.421.38E-12
3443.431.30E-12
3453.441.18E-12
3463.451.31E-12
3473.461.32E-12
3483.471.32E-12
3493.481.38E-12
3503.491.37E-12
3513.51.32E-12
3523.511.24E-12
3533.521.41E-12
3543.531.38E-12
3553.541.43E-12
3563.551.29E-12
3573.561.27E-12
3583.571.40E-12
3593.581.36E-12
3603.591.30E-12
3613.61.41E-12
3623.611.35E-12
3633.621.37E-12
3643.631.44E-12
3653.641.32E-12
3663.651.33E-12
3673.661.40E-12
3683.671.44E-12
3693.681.44E-12
3703.691.35E-12
3713.71.39E-12
3723.711.47E-12
3733.721.42E-12
3743.731.36E-12
3753.741.48E-12
3763.751.43E-12
3773.761.41E-12
3783.771.45E-12
3793.781.50E-12
3803.791.52E-12
3813.81.54E-12
3823.811.48E-12
3833.821.42E-12
3843.831.53E-12
3853.841.55E-12
3863.851.56E-12
3873.861.46E-12
3883.871.49E-12
3893.881.60E-12
3903.891.43E-12
3913.91.55E-12
3923.911.52E-12
3933.921.51E-12
3943.931.50E-12
3953.941.50E-12
3963.951.58E-12
3973.961.67E-12
3983.971.52E-12
3993.981.49E-12
4003.991.63E-12
40141.55E-12
JIS12A
Volts
Amps
sample #2
y = 4E-13x - 1E-13
