Solid State Phenomena Submitted: 2020-05-06

ISSN: 1662-9779, Vol. 314, pp 228-233 Accepted: 2020-08-13

© 2021 Trans Tech Publications Ltd, Switzerland Online: 2021-02-09

The Effect of Thermal Aging on Nano-Particle Removal

Yeoho Kim1, Seung-Wan Jin1, Hyun-Tae Kim2, Tae-Gon Kim3,
Kyu-Hwang Won4, and Jin-Goo Park1, 2, a
1
Department of Materials Science and Chemical Engineering, Hanyang University, Ansan, 15588,
Republic of Korea
Department of Bio-Nano Technology, Hanyang University, Ansan, 15588, Republic of Korea
2

Department of Smart Convergence Engineering, Hanyang University, Ansan, 15588,

3

Republic of Korea
Manufacturing Engineering Team, Samsung electronics co., ltd, Kyunggido, Republic of Korea
4

a
jgpark@hanyang.ac.kr

Keywords: Particle Defect, Wafer backside, Footprint, Thermal aging, Cleaning

Abstract The adhesion behavior of thermally aged particles was studied by characterizing the
footprint, which could be formed between a particle and a substrate. To understand the formation
mechanism of the footprint, the effects of temperature and aging time on the particle removal were
studied. Understanding the particle adhesion and removal aged at high temperatures is important to
maintain the cleanness of the wafer backside where many contaminants could adhere on in various
wafer process chambers.

Introduction
The cleanness of the wafer backside is vital in improving process quality and device yield for
advanced technology nodes, 10 nm, 7 nm, and beyond [1, 2]. Defects such as particles and scratches
on the wafer backside could be sources of local deformation of a wafer [2], causing the
photolithography hotspot generation [3], the local variation of film thickness, wafer breakage, so on.
The micron-size particle defects are easily generated during deposition, etch, CMP processes, and
they can be easily transferred to subsequent processing tools. The particles will be exposed to various
process conditions such as high compressive stress and high temperature, and it can be seen on the
end-effector and wafer chuck in the process chamber. In order to make the wafer backside clean, we
need to understand the behavior of particle adhesion and removal, especially at high temperatures. In
this paper, the adhesion behavior of aged particles at high temperature and the footprint of them were
studied.

Experimental Materials and Procedures

For studying the adhesion and removal of particles, 8-inch Si (100) p-type bare wafers (resistivity:
~8 Ωcm, SK siltron, Korea) were used. The wafer was cut to a size of 2 cm x 2 cm, then cleaned with
SC1 and dried with N2 gas. 100 nm, 500 nm, and 1 μm of silica particles (Corpuscular Inc., USA)
were deposited on Si wafer. Those samples were immediately stored at 300°C and 600°C in a furnace
(Furnace, J vac., South Korea) for 1 to 15 hours to investigate the thermal aging effect. The
atmosphere in the furnace was maintained with Air, N2, and O2. For particle removal, brush scrubbing,
ultrasonic, and CO2 jet cleaning were performed. DIW was used for brush scrubbing and ultrasonic
cleaning. Also, chemical cleaning was evaluated to remove the footprints using SC1 and dHF. The
SC1 solution was composed of ammonia water, H2O2, and H2O in a ratio of 1:1:5 at a temperature of
70℃, and HF was diluted in DIW in a ratio of 1:100. Samples were dipped in each solution for 1 to
5 minutes and then dried with N2 gas. Optical microscopy (Eclipse LV100DA, Nikon, Japan) and
atomic force microscopy (AFM, NX-20, Parks Systems, South Korea) were used to observe the
footprint before and after particle removal.

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 Solid State Phenomena Vol. 314 229

Result and Discussion

In order to evaluate the effect of thermal aging on the particle adhesion behavior, 100 nm silica
particle removal tests were performed with brush scrubbing. Figure 1 shows the particle removal
efficiency (PRE) behavior of the 100 nm silica particle aged at a temperature of 600°C as a function
of heat treatment time. It shows that the PRE dropped as aging time was increased. It means that
thermal aging makes the adhesion of the particles and the substrate stronger.

Figure 1: PRE of 100 nm silica particle aged at a temperature of 600°C as a function of heat treatment
time.

The footprint of the particle after particle removal was investigated to understand the mechanism of
the increase of adhesion force. Wet and dry cleaning processes were performed to check the footprints.
Figure 2 shows several 1 μm silica particles clustered, and the particle residues that remained after
performing particle removal by brush scrubbing, ultrasonic, and CO2 jet cleaning processes. The
footprints remained independent of the clean techniques and the shape of the footprints was various
as shown in Figure 3.

Figure 2: AFM measurement of the samples contaminated with 1um silica particles (a) before
cleaning, after (b) brush scrubbing, (c) ultrasonic cleaning, and (d) CO2 jet cleaning.
230 Ultra Clean Processing of Semiconductor Surfaces XV

Figure 3: (a) AFM 2D measurement of the footprints, 3D measurement of (b) crowned and (c)
towering footprint.

To understand the formation mechanism of the footprint, the shape and size of the footprints were
investigated after removing the thermally aged particles under various conditions. Figure 4 shows the
AFM images of the footprints of 500 nm and 1 μm silica particles aged at different aging time and
temperature.
The dimensions of the footprints were analyzed as shown in Figure 5. The outer contact diameter and
height of the footprints aged at 300°C and 600°C for 4.5 hours were characterized. According to the
results, bigger footprints were observed at a higher temperature. Figure 6 shows the outer contact
diameter and the height of the footprints aged at a temperature of 600°C for 4.5 and 9 hours,
respectively. No significant difference in the dimension of the footprints was observed at an aging
time of over 4.5 hours. It seems that the footprint was saturated around the aging time of 4.5 hours.
Figure 7 and 8 show the influence of the aging atmosphere and the hydrophilicity of the substrate on
the size of the footprints, respectively. According to the results, the footprint size aged in air
atmosphere was bigger than that in the N2 atmosphere. It shows that the size of the footprint aged on
the hydrophilic surface is bigger than that on the hydrophobic surface. As a result, the formation of
the footprints strongly depends on the aging temperature, atmosphere and hydrophilicity of the
substrate. It could be explained that the formation mechanism of the footprint is mainly the oxidation
process [4, 5]. Water vapor and O2 molecules in the air condenses around the contact surface between
the particle and the substrate, and it forms a water ring around the neck, and the molecules become a
source of oxidation to grow the footprint, and the growth of footprint depends on temperature and
time.

Figure 4: AFM images of the footprint of the 500 nm and 1 μm silica particles aged at 300 and 600°C
for 4.5 and 9 hours.
 Solid State Phenomena Vol. 314 231

Figure 5: (a) The outer contact diameter and (b) the height of the footprints by the aging temperature
of 300°C and 600°C for 4.6 hours.

Figure 6: (a) The outer contact diameter and (b) the height of footprint at the aging time of 4.5 and 9
hours

Figure 7: The outer contact diameter of the footprints in air and N2 atmosphere
232 Ultra Clean Processing of Semiconductor Surfaces XV

Figure 8: The outer contact diameter of the footprints on different hydrophilicity of the substrate
surface.

Chemical cleaning was performed to remove the footprints. Figures 9 and 10 show the results of the
chemical cleaning of the footprint. The footprint could not be removed by dipping for 5 minutes with
the SC1 solution, but the footprint was completely removed in the dHF solution. Since dHF easily
removed the footprint, it was verified that the footprints are mainly formed with chemical oxides.

Figure 9: AFM images of the footprint samples cleaned with SC1 cleaning for (a) 1 min and (b) 5
mins.

Figure 10: AFM images of the footprint samples cleaned with dHF for (a) 1 min and (b) 5 mins.

Conclusion
In this paper, we studied the adhesion behavior of thermally aged particles at high temperatures by
characterizing their footprints. At high temperatures, the thermally aged particles strongly adhere to
the substrate, cleaning them more difficult. To investigate these footprints' formation mechanism, the
 Solid State Phenomena Vol. 314 233

thermally aged particles were removed under various conditions and their footprints were
characterized. According to the study, the formation mechanism of the footprint is strongly related to
the oxidation process. The O2 molecules and water vapor in the air condense between a particle and
a substrate and it forms a water bridge. The water bridge becomes a source of oxidation and it starts
growing a chemical oxide depending on temperature and aging time. The chemical oxide is formed
around the neck, contributing to the increase of particle adhesion strength. Higher temperature
accelerates the thermal oxidation process further, and hydrophilic substrates condense water widely,
resulting in a larger footprint formation. Because these footprints could play a role of particle defects
in the following processes, it is important to prevent or remove footprints. The removal of the
thermally aged footprint was demonstrated and dHF showed a good cleaning performance.

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