Solar Energy Materials & Solar Cells 157 (2016) 48–54

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Solar Energy Materials & Solar Cells

journal homepage: www.elsevier.com/locate/solmat

0.76% absolute efficiency increase for screen-printed multicrystalline

silicon solar cells with nanostructures by reactive ion etching
Wen-Hua Chen b, Franklin Chau-Nan Hong a,c,d,n
a
Department of Chemical Engineering, National Cheng Kung University, Taiwan
b
Department of Materials Science and Engineering, National Cheng Kung University, Taiwan
c
Center for Micro/Nano Science and Technology, National Cheng Kung University, Taiwan
d
Advanced Optoelectronic Technology Center, National Cheng Kung University, Taiwan

art ic l e i nf o a b s t r a c t

Article history: In this study, the reactive ion etching in combination with alkaline etching was employed to texture the
Received 30 December 2015 surface of a 156
156 mm2 multi-crystalline silicon wafers to reduce their solar reflectivity and improve
Received in revised form conversion efficiency. Reactive gases comprising chlorine (Cl2), sulfur hexafluoride (SF6) and oxygen (O2),
13 May 2016
were activated in the radio-frequency (rf) plasma to fabricate pyramids in an reactive ion etching (RIE)
Accepted 19 May 2016
Available online 24 May 2016
system. The multi-crystalline Si substrates were etched in various compositions of gases to form the
nanostructures of various shapes. Besides the nanoscale features, the high density of nanostructures
Keywords: formed on the multi-crystalline Si surface was also required to significantly reduce the reflectivity. A low
Nanostructure reflectivity surface was successfully fabricated with the average reflectivity significantly reduced down to
Anti-reflection
o2% for the wavelength range of 300–850 nm. The short wavelength spectral response (blue response)
Reactive ion etching
improvement is observed in RIE textured solar cells compared to the standard textured cells. The RIE
Solar cell
textured surfaces in combination with optimized emitter resistance result in a remarkable enhancement
of short circuit current density. Compared with the acidic textured solar cells, the absolute conversion
efficiency of the alkaline þRIE textured cells was improved by 0.76% in average.
& 2016 Published by Elsevier B.V.

1. Introduction nanostructures [3,4] are being studied. Some approaches involve

Among all renewable energy resources, solar energy is con-
sidered as one of the most important alternative energy sources
and has been actively pursued as the most promising technology.
At present, crystalline silicon wafers remain the most widely used
materials in the solar cell industry with relatively high efficiencies
and reasonable costs to convert solar energy into electric energy.
The surface texturing in crystalline silicon solar cells can reduce
light reflection at the wafer surface. Reducing reflection on the top
surface of solar cells is often needed for improving energy con-
version efficiency.
In order to improve the cell efficiency, light trapping structures
such as surface texturing [1] and anti-reflection multilayer coat-
ings [2] have been applied to the fabrication of solar cells. Nano-
texturing of substrates has been widely studied, as it will reduce
broad-band anti-reflection effectively and increase light trapping
effects. A variety of techniques for fabricating anti-reflection
n cell industry, the costs of large capacity RIE equipment need to be
Corresponding author at: Department of Chemical Engineering, National Cheng
Kung University, Taiwan.
E-mail address: hong@mail.ncku.edu.tw (F.C.-N. Hong).
conventional wet etching [5]. Wet texturing has been commonly
used in the single crystal silicon (100) solar cell process by the
acidic or alkaline solution [6–8]. The dry etching methods, such as
mechanical diamond saw cutting [9], porous-Si etching [10], laser-
structuring [11], photo-lithographically defined etching [12] and
masked or maskless reactive ion etching (RIE) texturing, [13–20]
etc. have recently been studied to help prepare the ideal surface
textures. Reactive ion etching (RIE) texturing can provide us sin-
gle-side, surface reflection controllable texturing with very little
material loss, avoiding wafer breakage during processing, and
reduction of chemical wastes. In the RIE process, it is relatively
easy to control all parameters, thus a better reliability can be
achieved. Furthermore, RIE process equipment is quite mature in
performing anisotropic etching at high rates with a large pro-
duction capacity, and thus can be easily integrated into an
industrial production line for manufacturing solar cells. Therefore
we only need to add RIE equipment into currently cell production
line to achieve process integration. For the widespread use in solar
reduced. In this paper, to achieve self-masking without the need to
use the nanoscale mask and photolithography, the species and

http://dx.doi.org/10.1016/j.solmat.2016.05.046
0927-0248/& 2016 Published by Elsevier B.V.
 W.-H. Chen, F.C.-N. Hong / Solar Energy Materials & Solar Cells 157 (2016) 48–54
compositions of the gas mixtures as well as the process conditions
were varied in the reactive ion etching process to fabricate the
high aspect-ratio nanoscale pyramids over a large area within a
short process time.
2. Experimental
In this study, P-type multi-crystalline (mc) silicon wafers, with
a size of 156
156 mm2 and a thickness of 200 mm, were used as
the substrates. For acidic textured reference cell, the substrate was
etched using acidic solution (5 wt% HFþ25 wt% HNO3) at room
Fig. 1. Fabrication process for screen-printed multi-crystalline Si solar cells with
RIE texturing.
Fig. 2. The optical images of (a) is the original substrate with acidic pre-etching, (b) is the original substrate with alkaline pre-etching and (c) is the substrate with alkaline
pre-etching under optimized RIE process conditions.
49
temperature for an etching depth of 5 mm. Before RIE texturing, the
substrates were immersed in HF solution (HF:H2O ¼1:1) to remove
the SiO2 layer, 20 wt% KOH solution to remove the saw damage
layer and then cleaned by DI water. Anti-reflection nanostructures
were fabricated on these substrates by reactive ion etching (RIE)
process, in which the plasma was generated by a radio frequency
(RF) power supply with a frequency of 13.56 MHz. RF power was
applied to the substrate electrode inducing a negative dc self-bias
on the substrate. The gas reactants of RIE process comprised
chlorine (Cl2), sulfur hexafluoride (SF6), and oxygen (O2). The
fabrication of nano-textures on the surface of multi-crystalline
silicon substrate was studied by adjusting the compositions of SF6,
Cl2, and O2 gas mixtures. We have studied the effects of etching
gas compositions on the texturing and reflection of the surface.
First, we varied the flow rate ratios of Cl2/O2 at the SF6 flow rate of
6 sccm, the RF power of 100 W, a chamber pressure of 17.5 pa and
an etching time of 10 min Second, we varied the flow rate ratios of
SF6/O2 at the Cl2 flow rate of 10 sccm, the RF power of 100 W, a
chamber pressure of 17.5 pa and an etching time of 10 min Finally,
we varied the gas compositions of Cl2:O2:SF6 at an RF power of
100 W, a chamber pressure of 17.5 pa and an etching time of
10 min After the RIE texturing process, the substrate was
immersed in 5 wt% KOH for 1–3 min to etch away the damage
layer. Phosphorous diffusion using POCl3 was performed at 830–
850 °C for 15–25 min to form the n-type emitter with sheet
resistance from 70 to 100 Ω. Emitter resistance also played a key
role in order to optimize and achieve high efficiency gain in this
textured surface. The phosphorus silicate glass (PSG) was removed
by a diluted solution (5 wt% HFþ 25 wt% HNO3 þ20 wt% H2SO4).
Silicon nitride (SiNx) thin film of thickness 80 73 nm and the
refractive index of 2.2 70.05 was deposited by plasma enhanced
50 W.-H. Chen, F.C.-N. Hong / Solar Energy Materials & Solar Cells 157 (2016) 48–54

Fig. 3. SEM images inclined angle of 45° of textured surface etched with the gas flow ratios of Cl2 to O2 are (a) 0.5, (b) 1, (c) 2 and (d) 3 under the RF power of 100 W and an
etching time of 10 min

chemical vapor deposition using SiH4 and NH3 reactants as anti- Table 1.
reflection coating layer. Finally, the front and back metal contacts Optical and electrical performance under the different flow ratio of Cl2 to O2 (each
were formed by screen printing and co-firing in an in-line furnace condition over 10 wafers average).
system at 910–940 °C. The solar cell fabrication process is outlined
Process Avg. reflectance at λ300– Jsc gain Efficiency gain
in Fig. 1. Reflectance and surface textures were performed using (mA/cm2)
900 nm (%) (%)
ultraviolet-visible spectroscopy and scanning electron microscopy
(SEM), respectively. For studying the optical properties, reflection FCl2/FO2 ¼0.5  5.5 0.74 0.30
measurements with anti-reflection coating were conducted by FCl2/FO2 ¼1 7 0.49 0.25
FCl2/FO2 ¼2  8.5 0.31 0.18
JASCO V-660 UV/VIS Spectrophotometer, which use halogen lamp FCl2/FO2 ¼3  10 0.12 0.03
and photomultiplier tube as light source and detector, respectively. Reference cell with  12 – –
The scanning electron microscopy (SEM) instruments (JEOL JSM- SiNx
6700F and Hitachi SU8000) were operated at an accelerating
voltage of 15 kV with an emission current of 10 μA. The cell effi-
(c) shows the alkaline pre-etched substrate in Fig. 2(b) followed by
ciency was measured by a solar simulator under the illumination
the etching of plasma using the flow rates of 8.5, 2 and 12.5 sccm
of AM1.5. All of these measurements were performed at 25 °C.
for the SF6, Cl2 and O2 reactants, respectively, at an RF power of
100 W and an etching time of 10 min Fig. 2(b) shows that the
alkaline etching process is anisotropic resulting in various orien-
3. Results and discussion tations of grains. Then, as shown in Fig. 2(c), we have minimized
the appearance of oriented grains and achieved nearly black sur-
The surface textures were found to be dependent on many face by forming nanostructures using the maskless RIE subsequent
process conditions including the pre-etching solutions to form to alkaline etching (alkaline þRIE). Mc-Si wafers with black sur-
microstructures, the compositions of gas mixture, RF power, the faces can be easily produced under the proper RIE conditions.
gas pressure and the etching time in RIE process to form nanos- The surface texture could be varied by controlling several
tructures. For comparison, the optical images of mc-Si wafers with process parameters including the composition of gas mixture, RF
pre-etched and pre-etched þ RIE texturing are both prepared. Fig. 2 power, gas pressure and etching time of RIE system. Since the
(a) shows the substrate etched using acidic solution at room etching of silicon is more rapid than that of silicon oxide in the Cl2
temperature for an etching depth of 5 mm (traditional cell process). and SF6 gas plasma, the effect of flow ratio Cl2/O2 and SF6/O2 on
Fig. 2(b) shows the substrate etched using alkaline solution at the etching of multi-crystalline silicon surface were studied. The
70 °C for an etching depth of 5 mm with no RIE texturing, and Fig. 2 O2 gas was added in SF6 or Cl2 gas to partially oxidize silicon for
 W.-H. Chen, F.C.-N. Hong / Solar Energy Materials & Solar Cells 157 (2016) 48–54 51

Fig. 4. SEM images inclined angle of 45° of textured surface etched with the gas mixture flow ratios of SF6 to O2 are (a) 0.5, (b) 1, (c) 2 and (d) 3 under the RF power of 100 W
and an etching time of 10 min

Table 2. The SEM images of multi-crystalline Si wafers with RIE texturing

Optical and electrical performance under the different flow ratio of SF6 to O2 (each under the different flow ratios of SF6 to O2 were taken. The effect of
condition over 10 wafers average).
FSF6/FO2 ratio during etching on the substrate is shown in Fig. 4 with
Process Avg. reflectance at λ300– Jsc gain Efficiency gain the RF power of 100 W and an etching time of 10 min As shown in
900 nm (%) (mA/cm2) (%) Fig. 4(a)–4(d), when the FSF6/FO2 ratio was increased from 0.5 to 3,
the height and width of nanostructure on the surface increased and
FSF6/FO2 ¼ 0.5  6 0.45 0.22
reached the largest at the FSF6/FO2 ratio of 2 in the Fig. 4(c). At the
FSF6/FO2 ¼ 1  5 0.89 0.35
FSF6/FO2 ¼ 2  4.5 0.69 0.29 higher flow ratio of SF6 to O2, the surface oxidization was not enough
FSF6/FO2 ¼ 3  8 0.39 0.14 inducing nano-pyramids of poor form. When the FSF6/FO2 ratio was
Reference cell with  12 – – lower, the surface was oxidized to a higher ratio. Therefore, the shape
SiNx
of nanostructures became smaller and the uniformity became better.
The nanostructures of the silicon wafers were formed by competition
creating a self-masking effect. For comparison, the SEM images of between F þ and SFx þ (xo6) ions etching and SixOyFz mask effect
multi-crystalline Si wafers with RIE texturing under the various [21]. This competition between mask effect and etching effect could
flow ratios of Cl2 to O2 were prepared. As shown in Fig. 3, the be controlled by varying the texturing conditions from FSF6/FO2
substrates were etched under various FCl2/FO2 ratios with the RF ratio¼0.5 to FSF6/FO2 ratio¼3, resulting in different nanostructure. As
power of 100 W and an etching time of 10 min Fig. 3(a)–(d) shows shown in Table 2, average surface reflectance of the substrates after
that FCl2/FO2 ratio increased from 0.5 to 3, the nanostructure gra- RIE etching and KOH cleaning was measured by the ultraviolet-
dually turned small and the average heights changed from 200 nm visible spectrometer. The average reflectance of the silicon etched
to 20 nm. When Cl2 concentration was high, the high concentra- under the FSF6/FO2 ratio of 1 was obviously lower than that under the
tion of chlorine radicals in the gas phase induced fast etching of Si FSF6/FO2 ratio of 3. When the FSF6/FO2 ratio was increased from 0.5 to
and SiO2. Therefore, the nanostructures became smaller. The solar 2, the largest heights and widths (150 nm and 50 nm, respectively)
cell efficiency and average reflectance of the multi-crystalline nanostructures were formed under the present plasma conditions
silicon wafers under various RIE conditions are shown in Table 1. (100 W of RF power and 10 min of etching time).
When the FCl2/FO2 ratio was decreased, the etching depth became The solar cell devices were also fabricated under these condi-
deeper and the larger nanostructures were formed. Therefore, tions to characterize their performances. The optical reflectance
the average surface reflectance for the wavelength range of and the solar cell efficiencies of the multi-crystalline silicon wafers
300–900 nm was reduced from 12% to 5.5%. A higher efficiency under various ratios of SF6 to O2 are shown in Table 2. The solar
gain of 0.3% was achieved under a FCl2/FO2 ratio of 0.5. cell with lower surface reflectance after KOH etching may achieve
52 W.-H. Chen, F.C.-N. Hong / Solar Energy Materials & Solar Cells 157 (2016) 48–54
Fig. 5. SEM images inclined angle of 45° of textured surface etched with different ratios of Cl2:O2:SF6 are (a) 5:3:1, (b) 4:4:1, (c) 3:3::3, (d) 1:4:4, (e) 1:3:5, at an RF power of
100 W and an etching time of 10 min
Fig. 6. Front surface reflectance as a function of wavelength for the substrates
etched under various conditions by RIE, all samples with anti-reflection coating of
thickness 807 3 nm and the refractive index of 2.2 7 0.05.
higher solar cell efficiency. On the other hand, the FSF6/FO2 ratio ¼ 2
had the lowest reflectance after RIE etching, but the highest solar
conversion efficiency was achieved at the FSF6/FO2 ratio¼1. The
nano-pyramid structures were formed on a multi-crystalline sili-
con wafer surface to reduce the solar reflection and effectively
enhance the solar cell efficiency gain to a value of 0.35%.
In order to optimize the RIE conditions for minimizing the sur-
face reflectivity and maximizing the conversion efficiency, several
conditions such as the etching gas compositions, the etching times
and the RF powers were adjusted. The substrate with the lowest
reflectivity might not achieve the best efficiency gain. The shapes of
nanostructures after RIE process should be also a factor to affect
conversion efficiency.
Fig. 7. The external quantum efficiency performance of solar cell devices fabricated
by (a) wet texturing, (b) RIE process with Cl2:O2:SF6 ratio at 5:3:1 and (c) RIE
process with Cl2:O2:SF6 ratio at 1:3:5. (For interpretation of the references to color
in this figure, the reader is referred to the web version of this article.)
The random surface nanostructure formation in multi-crystalline
wafer is an advantage of RIE etching. The shapes of nanostructures
on the surface of multi-crystalline wafers could be controlled by
chemical etching and physical bombardments using plasma. The
surface texturing played an important role to reduce the reflectance
for maximizing the absorption of incident light. The adjustment of
three gas compositions was attempted to compare the nanos-
tructures formed. The gas composition ratios of Cl2:O2:SF6 during the
substrate etching are shown in Fig. 5 at the RF power of 100 W and
an etching time of 10 min As shown in Fig. 5(a)–5(e), the uniformity
of nanostructures became better and the top of the nanostructure
became flatter when the gas composition ratio of Cl2:O2:SF6 was
 W.-H. Chen, F.C.-N. Hong / Solar Energy Materials & Solar Cells 157 (2016) 48–54 53

changed from 5:3:1 to 1:3:5. The effects of dry etching on the 300–850 nm. Compared to the acidic textured reference cell, the
nanostructures were dependent on the compositions of Cl2, O2 and reflectance of the RIE textured solar cells is lower especially at
SF6 gas mixtures on a multi-crystalline silicon wafer. During the short wavelength. The lower reflectance implies that the absorp-
silicon etching, the SiOx formed by reaction with oxygen-containing tion of the sunlight will be improved and the short circuit current
species plays a masking role on the silicon wafer. As Cl2 gas chemistry will be enhanced. Since the surface is almost full of high aspect
is dissociated into the plasma, it also can etch Si and SiOx selectively ratio nanostructures, the RIE-textured surface using the gas mix-
ture of Cl2:O2:SF6 ¼1:3:5 had the lowest reflection in the full
in physical etching with ion energetic species and chemical etching
wavelength range. Therefore, the reflectance of the surface using
with active radicals. The higher concentration of Cl2 gas mixture is
gas mixture ratio of Cl2:O2:SF6 ¼1:3:5 was lower than that using
based on physical etching resulting in the sharp shape of texturing.
the gas mixture ratio of Cl2:O2:SF6 ¼ 5:3:1 due to the higher den-
The fluorine-containing species in the plasma etches Si and SiOx at sities of deep uniform nanostructures.
different rates leading to the formation of various shapes of surface Fig. 7 presents the measured external quantum efficiency (EQE)
textures due to chemical etching with active radicals. of solar cells after the acid texturing and the RIE texturing for gas
As shown in Fig. 6, the RIE-textured surface with the nanos- mixture compositions of Cl2:O2:SF6 ¼ 5:3:1 and Cl2:O2:SF6 ¼ 1:3:5.
tructure surface had lower reflection in the wavelength of range The EQE spectra show improved blue response (in the wavelength
range of 350–450 nm) of the RIE-textured surface compared to the
Table 3. wet-textured surface, and the gas mixture compositions of Cl2:O2:
Comparison of solar cell efficiencies with the surface etched under different Cl2/O2/
SF6 ¼1:3:5 has higher blue response than the gas mixture ratio of
SF6 flow ratios (each condition over 10 wafers average).
Cl2:O2:SF6 ¼5:3:1. The blue response improvement would enhance
Condition Voc (V) Jsc (mA/cm2) FF (%) Efficiency (%) short-circuit current (Jsc). Besides, RIE texturing at the gas mixture
compositions of Cl2:O2:SF6 ¼5:3:1 is shown to have slightly worse
Wet texturing 0.624 34.95 78.91 17.21
response in the wavelength range of 450–850 nm than the RIE
FCl2:FO2:FSF6 ¼5:3:1 0.623 35.77 78.01 17.38
FCl2:FO2:FSF6 ¼3:3:3 0.623 35.99 78.22 17.53 texturing at the gas mixture compositions of Cl2:O2:SF6 ¼1:3:5 and
FCl2:FO2: FSF6 ¼ 1:3:5 0.624 36.62 78.62 17.97 the wet texturing. The variation of nanostructures seemed to
induce the difference in efficiency performances.

Fig. 8. The optical images of multi-crystalline solar cell devices fabricated by (a) wet texturing, (b) RIE process with Cl2:O2:SF6 ratio at 5:3:1 and (c) RIE process with Cl2:O2:
SF6 ratio at 1:3:5. (For interpretation of the references to color in this figure, the reader is referred to the web version of this article.)
54 W.-H. Chen, F.C.-N. Hong / Solar Energy Materials & Solar Cells 157 (2016) 48–54
The average electrical performances are listed in Table 3 show-
ing the change of Voc and Jsc depending on the gas composition. The
gas composition ratio of Cl2:O2:SF6 ¼5:3:1 and Cl2:O2:SF6 ¼1:3:5 of
RIE cells with optimized emitter resistance is 70 Ω and 90 Ω,
respectively. For the gas composition ratio of Cl2:O2:SF6 at about
1:3:5, the Voc and Jsc were the highest. First, optimized nanos-
tructures cause lower reflectance and then Jsc was improved. Sec-
ond, the open circuit voltage (VOC) of cells with sheet resistance of
90 Ω is higher than that with sheet resistance of 70 Ω which ori-
ginating from the decrease in front surface recombination velocity
and induced by the lower doping concentration.
As shown in Table 3, surface textures could influence the fill
factors (FF) depending on the gas compositions during etching. The
plasma etching at the Cl2:O2:SF6 ratio of 1:3:5 had a highest FF with
the shapes of nanostructures not too sharp due to the higher
spontaneous chemical etching and less anisotropic physical ion
bombardments by fluorine in the SF6 rich plasma [21]. This kind of
shape can be good for emitter doping, anti-reflection surface pas-
sivation coating and electrical contacts. The serial resistance of a
solar cell dropped and the fill factor and the conversion efficiency
increased. However, plasma etching of a gas mixture ratio of Cl2:O2:
SF6 about 5:3:1 showed a somewhat different performance. The
etching of Cl2 plasma is due to more anisotropic physical ion
bombardments and less chemical etching resulting in the vertical
anisotropic etching forming the textures with sharp edges or cor-
ners [21]. And, with nanostructures fabricated by high Cl2 con-
centration etching, the solar cells had poor fill factor and conversion
efficiency resulted from the high serial resistance of the device.
Therefore, the maximum conversion efficiency with specific
nanostructures can be obtained for the etching gas ratios of Cl2:O2:
SF6 at 1:3:5. In general the measured efficiency of wet texturing in
multi-crystalline silicon solar cells is about 17.21%. Optimizing the
etching gas compositions (Cl2:O2:SF6 ¼1:3:5) by fixing the process
parameters (an RF power of 100 W, a chamber pressure of 17.5 pa
and an etching time of 10 min), we had obtained a maximum
conversion efficiency of 17.97% for the nanostructured surface with
nearly 2% average reflectance.
Large-area solar cell devices with a completely-black surface can
be fabricated reproducibly and uniformly across the whole wafer
surface for a size of 156
156 mm2. The solar cell devices using the
wet etching method to texture the surface had a dark blue surface,
as shown in Fig. 8(a). On the other hand, large-area solar cell
devices with completely-black surface can be fabricated uniformly
across the whole wafer surface for a size of 156
156 mm2, as
shown in Fig. 8(b) and (c), for the etching gas ratios of Cl2:O2:SF6 at
5:3:1 and 1:3:5, respectively, at an RF power of 100 W and an
etching time of 10 min The self-masking RIE process was found to
be reproducible in fabricating nano-structures for reducing the light
reflection to increase the solar cell efficiency up to 17.97%, compared
with 17.21% using the conventional wet etching.
4. Conclusions
In this study, a self-masking RIE process for fabricating the
large-area (156
156 mm2) anti-reflective multi-crystalline silicon
surface by creating a high density of nanostructures on the surface
has been developed. The control of the reflectance in the range of
2%–10% was achieved under different RIE conditions. Large-area
multi-crystalline silicon surfaces with low reflectance (o2%) and
high uniformity could be reproducibly achieved. RIE conditions
were optimized to obtain the best textured surface, exhibiting
extremely low reflectance. Based on the external quantum effi-
ciency results, RIE texturing improved the blue response over
conventional cells and thus enhanced the short circuit currents.
Compared with the wet-textured solar cells, the multi-crystalline
Si solar cells with alkaline pre-etching and then RIE texturing have
improved in Jsc 1.67 mA/cm2 in absolute gains, resulting in a gain
of conversion efficiency around 0.76% using the industrial screen
printing process.
Acknowledgments
The authors gratefully acknowledge the financial support from
the National Science Council of Taiwan under Grant NSC-102-
2221-E-006-240-MY3 and the Ministry of Economic Affairs (Tai-
wan, ROC) through project 103-EC-17-A-08-S1-216.
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