Lab Report 2

Thin Films: Physical Vapor Deposition by Sputtering

and Reactive Sputtering

By:

Suryanarayana Kalaga

Sxk7317@rit.edu
Introduction and Theory

Physical Vapor Deposition (PVD) involves converting the target material into vapor and then transporting
the gas to the substrate via pressure difference where it condenses on the surface of the substrate to form a
film. In VLSI fabrication, the most widely-used method of accomplishing PVD of thin films is by
sputtering.

Sputtering

Sputtering is a vacuum process where ions in a plasma bombard a target under the influence of an electric
field. The electric field may be generated by a d.c. potential (typically 500 to 5000 V), or a high
frequency a.c. voltage source. The plasma is an electrically neutral glow discharge of electrons and
positive ions. Noble gases work best as a bombarding species because they are least likely to form
reactants on the target surface. Argon is usually the gas of choice because these atoms are comparable in
size to most target atoms and this result in optimum sputter yield. Krypton and Xenon have also been
used, but they are more costly than Argon. When the argon ions collide with the target, target atoms are
ejected by momentum exchange with energies in the range of 10 - 40 eV. These collisions also produce a
small number of secondary electrons. The secondary electrons enter the plasma and ionize neutral Ar
atoms thereby sustaining the plasma. The probability for ion production by energetic electrons (>100 eV)
passing through low pressure argon (<2 mT) is low. The probability of secondary electrons ionizing
enough argon atoms to produce more electrons from the target can only be increased by increasing the
working (Ar) pressure. However, making the pressure too high would decrease the deposition rate
because significant numbers of sputtered atoms would not be able to penetrate the discharge atmosphere.
Some would even be reflected back to the target. There exists stress in the sputtered films, compressively
stressed films would like to expand parallel to the substrate surface and in the extreme, films in
compressive stress will buckle up on the substrate. Films in tensile stress, on the other hand, would like to
contract parallel to the substrate, and may crack if their elastic limits are exceeded.

Figure 1: Sputtering Process

Reactive Sputtering

In Reactive Sputtering a target material (e.g. Tantalum or Aluminum) is sputtered in the presence of a
reactive gas (e.g. oxygen or nitrogen) to produce a compound such as TaN or Al2O3. Both the coating rate
and film stoichiometry are sensitive functions of the reactive gas partial pressure and control of this
pressure is key to producing good quality coatings with reasonable deposition rates.

The rate of film growth and hence its ultimate thickness is dependent on factors such as the sputtering
rate, sputtering pressure, power, substrate temperature, and in the case of reactive sputtering, the fraction
of argon gas in the mixture. It was expected that the sputter rate will be proportional to the Ar gas
composition. With a higher Ar content, more Ar+ ions are generated to bombard the target. The deposition
rate will depend on the amount of sputter material that can reach the substrate through the plasma. As the
Nitrogen composition of the gas increases (Ar composition decreases respectively) the film thickness in
general decreases due to the reduced sputter rate. The reactivity between Ta and N2 atoms is higher at a
high N2 gas composition than at a lower N2 composition because of a higher probability of interaction
between sputtered Ta and N2 molecules. So, as the amount of N2 in the gas mixture increases, the N2
content of the film is expected to increase also.

Analysis and Results

Metal Al Al Al Mo Al Al Al Mo

Power(W) 300 600 900 600 300 600 900 600

Voltage(V) 369 400.4 425 343.5 344 369.2 382.5 343

Current(A) 0.81 1.49 2.11 1.74 0.87 1.62 2.35 1.74

Avg. Thickness(Å) 3533.83 4395.5 6920.5 3925.5 2063.5 4180 6236.5 4142.6

Std. Dev. 546.05 641.19 241.64 552.15 462.23 634.23 412.96 207.34

Sputter rate [Å/min]

706.76 879.1 1384.1 785.1 412.7 836 1247.3 828.52
Figure 2 : Table showing the variation of Al and Mo film thicknesses at different deposition
parameters

Looking at the results from Figure 2, the uniformity of Aluminum film thickness across wafer varied with
deposition parameter (power). At 300W, taking the average of the standard deviation for the two different
current and voltage combinations, the film thickness varied by about 504.14 Ao. At 600W, the thickness
of the Aluminum film across the wafer varied by about 637.71 Ao and the thickness variation decreased to
224.49 A0 for sputtering at 900W. On the other hand, the thickness of Molybdenum at 600W varied by
about 379.745Å across the wafer, which is a better uniformity than Al with similar deposition parameters.

The sputtering was done for 5 minutes for all metals at different current and voltage combinations. The
sputter rate in A0 per minute can be determined by dividing the resulting thickness by 5. The fastest film
growth was 1384.1 A0/min for Aluminum at 900W, which also has the best uniformity which is unlikely
as it is expected to have the worst uniformity across the wafer due to the fast sputter rate. The slowest
sputter rate was 412.7 A0/min, which ironically did not have a better uniformity. Therefore the expected
outcome which was supposed to be better uniformity for slow sputter rates did not happen in the case of
900W power supply. . Aluminum and Molybdenum can be compared by looking at their sputter yield:
the number of atoms released from target compared to the number of ions that make it to the substrate. To
calculate deposition rates, we need to know how many sputtered atoms we create per incoming ion,
sputtering yield.

# 𝑜𝑓 𝑎𝑡𝑜𝑚𝑠 𝑟𝑒𝑙𝑒𝑎𝑠𝑒𝑑 𝑓𝑟𝑜𝑚 𝑡𝑎𝑟𝑔𝑒𝑡

𝑆𝑝𝑢𝑡𝑡𝑒𝑟 𝑌𝑖𝑒𝑙𝑑 (𝑆) = (1)
# 𝑜𝑓 𝑖𝑛𝑐𝑖𝑑𝑒𝑛𝑡 𝑖𝑜𝑛𝑠

3𝛼4𝑚₁𝑚₂𝐸
𝑆= (2)
4𝜋2 (𝑚1 +𝑚2 )2 𝑈𝑠

Where E = ion energy (< 1keV in this case since all voltages are 200 – 400 volts), m₁ = mass of ion being
sputtered, m₂ = mass of target and Us = energy to break bonds.

Using published sputtering yield data for metals and semiconductors [Ref. 1], the sputter yield for Argon
incident on Al at 500eV is 1.05 atoms/ ion and 0.80 atoms/ion for Mo at the same sputter gas energy,
however, when the sputter energy is increased to 1keV, the sputter yield for Al is 1.0 and 1.13 for Mo.
Therefore, at higher sputter energies, Mo has a better sputter rate than Al. The ion energy for the results in
Figure 1 was between 257 – 300eV for Al and 244 – 354eV for Mo, hence the published sputter yield
results at 500eV are reasonably close to be used for comparing S for Al and Mo.

Al sputter rate (Å/min)at different

powers
Sputter Pressure 300W 600W 900W
(mT)
5 (Monday lab)
706.76 879.1 1384.1
5 ( Thursday lab)
412.7 836 1247.3

Figure 3: Sputter rates at different power values

 1600

1400

1200
Sputter rate [A0/min]

1000
300W
800
600W
600
900W
400

200

0
Monday Lab Thursday Lab

Figure 4: A bar chart showing the effect of power on the Sputter rate

The chart in Figure 4 shows that the sputter rate remained relatively constant for three different powers at
the same sputter pressure of 5mTorr. However, a significant difference in sputter rate can be observed
between depositions with the same power if the sputter pressures were to be changed. Higher Sputter
pressure would result in a faster sputter rate.

900
880
860
Sputter rate [A0/min]

840
820
Al
800
Mo
780
760
740
720
Monday Lab Thursday Lab

Figure 5: Comparison of sputter rate of Aluminum and Molybdenum at the same Power of 600W
but difference in Current and Volatge ratings

The sputter rate of Aluminum and Molybdenum at the same power but different voltage and current
ratings is shown in figure 5. It is seen that for the same current and voltage rating ( Thursday lab) the
sputter rate is almost similar but aluminum has a better sputter rate. When there is a significance change
in the current rating it is seen that the sputter rate is varied by a large margin.
 700

600
Standard Deviation in Thickness

500

400
Al
300
Mo
200

100

0
Monday Lab Thursday Lab

Figure 6: Comparison of uniformity of the film thickness in Aluminum and Molybdenum at the
same power

Figure 6 shows the comparison in the uniformity of the film thickness when Aluminum and Molybdenum
are used . It is seen that the uniformity is less for Aluminum than Molybdenum in both th labs as the
sputter rate of Aluminum is more than Molybdenum and faster the rate of deposition of the film the less is
the uniformity.

Total Power Run Ar N2 Voltage Current Rs Appearence

Pressure Pressure
Pressure (W) [V] [A] [Ω/sq.]
[mT] [mT]

6mT 225W 1 6.0mT 0.0mT 288V 0.78A 2.42 Metallic

225W 2 5.0mT 1.0mT 358V 0.62A 25.95k Semi-transparent

225W 3 4.0mT 2.0mT 369V 0.6A 3.25M Semi-transparent

500W 4 6.0mT 0.0mT 301V 1.66A Delaminated Metallic

6mT 350W 1 6.0mT 0.0mT 298V 1.17A 2.77 Metallic

350W 2 5.0mT 1.0mT 353V 0.99A 19 Semi-transparent

350W 3 4.0mT 2.0mT 380V 0.92A 7.5k Semi-transparent

450W 4 6.0mT 2.0mT 298V 1.50A 1.62 Metallic

Figure 7: Reactive Sputter Data

Reactive sputter was used to form a film of TaN on 4-inch wafers at different gas flow pressures.. It is
seen that the sputter rate will be proportional to the Ar gas composition. With a higher Ar content, more
Ar+ ions are generated to bombard the target. The deposition rate will depend on the amount of sputter
material that can reach the substrate through the plasma. As the Nitrogen composition of the gas increases
(Ar composition decreases respectively) the film thickness in general decreases due to the reduced sputter
rate. Thus as the Ar composition is higher a thicker film is formed which is more opaque and has less
sheet resistance.

Conclusion

The deposition parameter that produced the best film thickness uniformity across wafer was 600W (343V
and 1.74A) for Molybdenum. Al film thickness uniformity deteriorated with an increase in power with
different current and voltage combinations except in the case of 900W which may be because of the non
uniformities in the vapor distribution from the source. Also, at 600W, the uniformity of molybdenum
across wafer was much better than Al at 600W. Hence, if the sputtering has to be done at 600W,
molybdenum is a better choice than Al unless other properties of Al are desired for the specific device
being fabricated. The sputter rate results in Figure 2 ,in general showed that there is an inverse
relationship between sputter rate and film uniformity across wafer; slower sputter rates produce a more
uniform film thickness and vice versa. It is also noted that no arcs were observed. In reactive sputter it is
seen that the sputter rate will be proportional to the Ar gas composition, with higher Ar composition a
thicker film is seen .At low partial pressures film compositions (and therefore properties) are not ideal. At
higher partial pressures the target may be poisoned by reaction with the reactive gas. The ideal operating
point is between these two extremes and it is required to control the flow of the reactive gas in order to
maintain the partial pressure within this region. The solution is to control the reactive gas partial pressure
directly, avoiding target poisoning and improving film composition and deposition rates.

References:

1. Ohring, Milton. Materials of Thin Films: Deposition & Structure. Second edition (Table 4-2)
2. Boenig, Herman V. Plasma Science and Technology.