Fabrication of metal thin films prepared by the sputtering technique

Tan Teck Seng (U084494N) Lim Yong Sheng Eric (U084517A) Christina Setiawan (U084326R)

(Group 5)

Department of Materials Science and Engineering, Faculty of Engineering, National University of

Singapore, Singapore 117574.

Introduction

The objective of this experiment is to investigate sputtering technique, the sputtering rate, and to

measure the thickness of the film by measuring its resistivity.

Thin film is defined as a layer of material ranging from fractions of a nanometer (monolayer) to

several micrometers in thickness. It is widely used for semiconductor devices and optical coatings.

There are several ways of fabricating thin film, such as: electroplating, sol gel, and sputtering 1. In

this experiment, we will investigate further on sputtering technique.

Sputtering is a vacuum process during which energized plasma ions strike a target composed of the

desired coating materials and causes the atoms from that target to eject with enough energy to

travel to and bond with a substrate to form a thin film2. There are several types of sputter deposition

techniques, DC, Radio Frequency (RF), and magnetron. In this experiment, A DC sputter coater

(BAL-TEC SCD 005) is used for fabrication of gold thin films. The principle behind sputtering is

to apply a high voltage between the cathode and the anode to induce ionization of the gas (the most

common is argon), which is filled in the chamber. Positive ions are accelerated towards to the

cathode under the electrical field. The ions will then bombard the cathode in high-velocity which

may cause the ejection of the surface atoms. The ejected atoms can condense on a substrate to form

a thin film.

The schematic DC sputter coater is shown in figure 1 below.

1 http://en.wikipedia.org/wiki/Thin_film#Deposition
2 www.angstromsciences.com/reference/dictionary-of-terms/print.html

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 Figure 1.Schematic drawing of DC apparatus

In DC deposition technique, the sputtering rate depends on the argon pressure and voltage. The

optimum argon pressure is around 100mTorr. And sputtering rate is proportional to the voltage.

Sputtering rate is defined as the film thickness / sputtering time.

One of the most important parameter of a thin film is the thickness. In this experiment, we will

investigate the thickness of a film by measuring the resistivity of the film. The four point probe

method will be used in this experiment. Four point methods comprises of four metal tips in a linear

array are pressed on the surface of the specimen, as shown in Fig. 2. To measure a resistivity, a

small current I from a constant-current source is passed through the outer two probe tips, while the

voltage V is measured between the inner two probe tips. Therefore, the resistivity is given as:

V
ρ= t (CF)
I

where ρ is the resistivity, t is thickness of the specimen and CF is the correction factor.

Fig. 2. Schematic setup of four-point probe method to measure sample resistivity.

CF is a geometrical correction factor. It depends on the specimen shape and geometry of the probe

tips. If the probe-tip spacing s is much less than the lateral dimension d of the specimen, CF

becomes (π/ln2) = 4.5324.

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Therefore, by measuring the resistivity of the material, all the variables in the equation is known

and therefore, the thickness of the thin film can be determined.

Experimental

6 Glass substrates were cleaned in an ultra-sonic bath with ethanol for 15 minutes and then dried on

a tissue. The vacuum chamber of the DC sputter coater was evacuated to a pressure of 5×10-2

mbar and argon gas will be then filled. This process was repeated 3 times.

The sputtering current was set to 50mA. The dried glass substrates were put in the DC

sputter coater. The sputtering times was set to 50s with the working distance of 50mm. The last

process was repeated with different sputtering times L 100s, 150s, 200s, 250s, and 300s.

After the glass substrates underwent sputtering and thin layer of different thickness was formed, the

resistivity measurement was carried out. A four-point probe station, a constant current source

(CCS) and a digital voltmeter (DVM) were used for resistivity measurement. The first specimen

was put under the four-point probe tips. Tips were firmly pressed on the specimen surface by

lowering the tips by turning the handle on the probe station. The desired current I in the μA range

was provided by the constant-current source (CCS). The voltage was read by digital voltmeter

(DVM). The true voltage V was obtained through:

V = Von - Voff

where Von is the voltage measured with current and Voff is without current.

7 different currents of 10, 20, 30, 40, 50, 60 and 70mA were applied on the same specimen on one

measurement point and the respective Voff and Von were recorded. The last process was repeated

with another 4 points on the same specimen. The processes were repeated for the remaining

specimens.

Results and discussion

Question 1: Calculation of thickness of various specimens.

The resistivity of the specimen is related to its thickness by the following equation:

ρ=Vt(CF)I,

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where ρ is the resistivity of pure gold at room temperature, V is the measured true voltage, I is the

applied current, t is the thickness of the specimen, CF is the correction factor. Therefore, the

thickness can be calculated by rearranging the equation to this:

t=ρIV(CF)

Resistivity of pure gold at 30°C is equal to 2.3x10-8 Ωm.

Correction factor (CF) is equivalent to 4.5324. This is based on the assumptions that the glass

substrate is a perfect square, resulting in ad equal to 1 and the distance between the probes of the 4

probe station is relatively small, compared to the length of the glass substrate (s≪d). Coupled these

with the true voltage and applied voltage obtained from the table in appendix, the average thickness

of glass substrate undergoing different sputtering time can be obtained, as shown in the subsequent

pages. Generally, as the sputtering time increases, the average thickness of the specimen increases

Sputtering time = 50s

Positions Average
Applied current Thickness
1 2 3 4 5 V
V V V V V
(mA)
(mV) (mV) (mV) (mV) (mV) (mV) (nm)
13.87
10 7.466 8.205 6 7.464 6.404 8.683 5.844
14.91 16.39 27.71 14.92 12.79
20 3 0 3 4 2 17.346 5.851
22.37 24.59 41.57 22.40 19.19
30 2 3 6 7 4 26.028 5.849
29.83 32.80 55.43 29.88 25.59
40 4 0 2 5 6 34.709 5.848
37.29 41.00 69.26 37.37 31.99
50 6 8 6 2 6 43.388 5.848
44.76 49.23 83.16 44.87 38.40
60 4 1 6 2 4 52.087 5.845
52.23 57.42 97.06 52.37 44.81
70 9 1 6 4 0 60.782 5.844
Table 1: Thickness of specimen undergoing 50s sputtering.
Average thickness of specimen that undergoes 50s sputtering = 5.847nm

Sputtering time = 100s

Positions Average
Applied current Thickness
1 2 3 4 5 V
V V V V V
(mA)
(mV) (mV) (mV) (mV) (mV) (mV) (nm)
10 3.362 3.076 2.663 3.062 3.573 3.147 16.124

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 20 6.694 6.143 5.318 6.117 7.138 6.282 16.156
10.03 10.71
30 7 9.215 7.980 9.176 0 9.424 16.155
13.37 12.28 10.64 12.23 14.28
40 9 5 0 6 0 12.564 16.156
16.71 15.35 13.29 15.29 17.85
50 7 3 8 3 0 15.702 16.159
20.03 18.42 15.96 18.35 21.42
60 6 3 2 3 1 18.839 16.162
23.37 21.49 18.61 21.41 25.00
70 3 2 6 0 3 21.979 16.162
Table 2: Thickness of specimen undergoing 100s sputtering.
Average thickness of specimen that undergoes 100s sputtering = 16.153nm

Sputtering time = 150s

Positions Average
Applied current Thickness
1 2 3 4 5 V
V V V V V
(mA)
(mV) (mV) (mV) (mV) (mV) (mV) (nm)
10 1.692 2.039 1.659 2.002 1.973 1.873 27.093
20 3.380 4.072 3.315 3.997 3.941 3.741 27.130
30 5.071 6.110 4.975 5.997 5.913 5.613 27.121
40 6.672 8.148 6.635 7.997 7.885 7.467 27.183
10.81
50 8.451 3 8.292 9.995 9.855 9.481 26.761
10.14 12.22 11.99 11.82
60 0 0 9.949 5 6 11.226 27.122
11.82 14.25 11.60 13.98 13.78
70 9 7 5 3 7 13.092 27.132
Table 3: Thickness of specimen undergoing 150s sputtering.
Average thickness of specimen that undergoes 150s sputtering = 27.077nm

Sputtering time = 200s

Applied Positions Average Thicknes
current 1 2 3 4 5 V s
V V V V V
(mA)
(mV) (mV) (mV) (mV) (mV) (mV) (nm)
10 1.163 1.516 1.474 1.252 1.260 1.333 38.069
20 2.322 3.027 2.944 2.499 2.517 2.662 38.129
30 3.484 4.540 4.418 3.748 3.780 3.994 38.116
40 4.645 6.054 5.891 4.998 5.040 5.326 38.115
50 5.805 7.567 7.368 6.246 6.299 6.657 38.115
60 6.967 9.082 8.837 7.496 7.559 7.988 38.116
10.59 10.31
70 8.127 4 1 8.736 8.819 9.317 38.124
Table 4: Thickness of specimen undergoing 200s sputtering.
Average thickness of specimen that undergoes 200s sputtering = 38.112nm

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 Sputtering time = 250s
Positions Average
Applied current Thickness
1 2 3 4 5 V
V V V V V
(mA)
(mV) (mV) (mV) (mV) (mV) (mV) (nm)
10 0.865 0.994 0.960 0.962 0.896 0.935 54.250
20 1.727 1.986 1.921 1.921 1.854 1.882 53.933
30 2.590 2.980 2.885 2.884 2.781 2.824 53.908
40 3.454 3.974 3.847 3.845 3.707 3.765 53.907
50 4.317 4.967 4.810 4.806 4.630 4.706 53.916
60 5.181 5.961 5.773 5.769 5.555 5.648 53.910
70 6.044 6.954 6.735 6.731 6.481 6.589 53.911
Table 5: Thickness of specimen undergoing 250s sputtering.

Sputtering time = 250s

Positions
Applied current Average V Thickness
1 2 3 4 5
V V V V V
(mA)
(mV) (mV) (mV) (mV) (mV) (mV) (nm)
10 0.592 0.798 0.759 0.657 0.670 0.695 72.994
20 1.182 1.570 1.517 1.312 1.338 1.384 73.343
30 1.773 2.350 2.277 1.969 2.008 2.075 73.353
40 2.365 3.134 3.037 2.626 2.678 2.768 73.332
50 2.955 3.917 3.795 3.283 3.347 3.459 73.345
60 3.546 4.700 4.556 3.939 4.017 4.152 73.339
70 4.137 5.483 5.315 4.595 4.666 4.839 73.405
Average thickness of specimen that undergoes 250s sputtering = 53.962nm

Table 6: Thickness of specimen undergoing 300s sputtering.

Average thickness of specimen that undergoes 300s sputtering = 73.302nm

Question 2: Plot a graph of thickness against sputtering time.

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Sputtering 50 100 150 200 250 300
time(s)
Thickness 5.847 16.153 27.077 38.112 53.962 73.302
(nm)

Table 7: Thickness of specimen with respect to sputtering time

Fig 3: Thickness of specimen versus Sputtering time graph

The experiment results gave a best-fit straight line after a plot is done. Hence, the gradient of the

graph will give the sputtering rate of the sputter coater. The voltage is measured at five different

positions, using seven different current values, and the averages of these voltages are used to

calculate the thickness of the specimen. This ensures a higher degree of accuracy of the thickness

measured for each specimen.

The sputtering rate is defined as:

Sputtering rate = film thickness / sputtering time

From the graph, the sputtering rate is found to be 0.264nm/second.

Error Analysis

To ensure a high accuracy in measuring voltage across the specimen, the four point probe method

was used to avoid measuring the voltage drop due to resistance of electrical wires. In consideration

that the thickness is in nanometres and the values are consistent up to one decimal place, the results

obtained can be considered to be highly accurate. As the voltage is measured at various positions of

the sputter, and their values do not significantly from the average thickness, it can be concluded

that the sputtering thickness across the surface is even.

From figure 3, the experimental results gave a best-fit straight line graph, with no points

significantly deviating from the graph. This shows that the results obtained is of high accuracy.

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It is noted that the vertical intercept has a value of -10.4, which is illogical as there should be zero

thickness before sputtering. This implies that the actual thickness of the sputter is actually higher

than the calculated thickness, due to systematic errors in the experiment.

Conclusion

Sputtering of surfaces allows even coating of surfaces. This makes sputtering an effective method

for coating material that require a highly even coating. The thickness of the sputter coating is found

to be linearly proportional to the sputtering time. This implies that the thickness can be easily

calculated through the time taken during sputtering, and that the thickness of the coating can be

controlled by controlling the sputtering time.

References

1. Wikipedia: The Free Encyclopedia. Thin Film. Retrieved on 20 October, 2010 from
http://en.wikipedia.org/wiki/Thin_film
2. Wikipedia: The Free Encyclopedia. Sputter Deposition. Retrieved on 20 October, 2010
from http://en.wikipedia.org/wiki/Sputter_deposition
3. Wikipedia. Sputtering. Retrieved on 23 October, 2010 from
http://en.wikipedia.org/wiki/Sputtering
4. Angstrom Science, Inc. Retrieved on 22 October, 2010 from
www.angstromsciences.com/reference/dictionary-of-terms/print.html

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