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Photovoltaic solar cells industry wastewater treatment

a a a a
Nadjib Drouiche , Fadila Djouadi-Belkada , Tarik Ouslimane , Aissa Kefaifi , Jihane
b c
Fathi & Emina Ahmetovic
a
Centre de Recherche en Technologie des Semi-conducteurs pour l’Energétique, 2,
Bd Frantz Fanon BP140 Alger-7-merveilles, 16027, Algiers, Algeria Phone: Tel. +213 21
279880x192 Fax: Tel. +213 21 279880x192
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Régie Autonome de Distribution d’Eau et d’Electricité de la Chaouia (RADEEC) Settat,
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c
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Tourism and Environment Protection (EKOPOT), Obala Zmajaod Bosne 4, 75000, Tuzla,
Bosnia-Herzegovina
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doi: 10.1080/19443994.2012.763217

Photovoltaic solar cells industry wastewater treatment

Nadjib Drouichea,*, Fadila Djouadi-Belkadaa, Tarik Ouslimanea, Aissa Kefaifia,

Jihane Fathib, Emina Ahmetovicc
a
Centre de Recherche en Technologie des Semi-conducteurs pour l’Energétique, 2, Bd Frantz Fanon BP140 Alger-7-
merveilles, 16027 Algiers, Algeria
Tel. +213 21 279880x192; Fax: +213 21 433511; email: [email protected]
b
Régie Autonome de Distribution d’Eau et d’Electricité de la Chaouia (RADEEC) Settat, Maroc
c
Association for Development, Advancement and Promotion of Ecological Agriculture, Tourism and Environment
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Protection (EKOPOT), Obala Zmajaod Bosne 4, 75000 Tuzla, Bosnia-Herzegovina

Received 28 September 2012; Accepted 31 December 2012

ABSTRACT

Nowadays, in the photovoltaic (PV) industry there still remains a huge potential to be exploited,
where markets are dominated by crystalline silicon PV-based cells. However, in the future it is
expected that thin films PV will have a larger market share. Until recently, the prevailing tech-
nology based on mono-crystalline silicon has been gradually exceeded by poly-silicon technol-
ogy due to its lower production cost. In PV industry, solar-graded silicon is the main material
used in manufacturing process. In this industry, manufacturing and production processes
require large amounts of water that result in important discharged industrial effluents contain-
ing different pollutants such as hydrogen fluorides, suspended solids, mixed acids, SiO2, and
high oxide particles. Among discharged pollutants, the hydrofluoric acid is significantly used in
photovoltaic’s (PV) manufacturing for both quartz cleaning and wafer etching. In fact, wastewa-
ters from PV industries have high concentrations of fluoride, typically in a range of 500–
2,000 mg/L. They are considered highly toxic and need to be strictly monitored and regulated.
Three production phases that generate the highest flow of wastewaters are texturing (multi-
crystalline silicon wafers need a mixture of HF/HNO3 dilution and also a hot caustic solution
with IPA used for the multi-crystalline wafers mixture), etching, and formation of PV cells.
Phosphorus diffusion leads to formation of phosphorus silicate layer that needs to be eliminated
by means of hydrofluoric acid (HF) application. Classification of effluents from a point of
source, concentration, chemical, or composition feature is compared. Wastewater treatment
optimization is often conducted and we discussed major treatment methods in solar cells manu-
facturing: treatment of HF discharges, neutralization, and collection of isopropanol discharges.
The article discusses design of wastewater treatment system that is operational in practice.

Keywords: Solar cell; Silicon wafers; Treatment of hydrofluoric acid; Isopropanol discharges;
Neutralization; Sedimentation; Filtration

1. Introduction been to capture this energy and transform it into

electricity.
The sun represents an almost inexhaustible
The solar photovoltaic branch industry is growing
source of energy. The challenge has always
rapidly and electricity production from solar energy is
becoming more efficient and less costly thanks to
*Corresponding author. innovations in technology. Although, the proportion

1944-3994/1944-3986 Ó 2013 Balaban Desalination Publications. All rights reserved.

 2 N. Drouiche et al. / Desalination and Water Treatment

of electricity produced from solar cells is continuously most performed solar panels are manufactured from the
increasing, environmental concerns are unavoidable in larger crystals that also may contain a fewer defects [3].
the choice of industrial products [1]. Using various saws, ingots produced are cut into
Solar cells are manufactured in a complex process bricks and then into wafers. The wafers are attacked
that requires enormous know-how. The objective is to by an acid or base to reduce their reflectivity.
produce panels with high level of efficiency at low In the diffusion furnace, phosphorous atoms are
cost. To achieve this, different production processes added to the surface of the cells creating an electric
are used with a fundamental distinction between field where electrons will be collected. A nitride
solar cells on the basis of silicon wafers and thin-film deposit then allows to the reflectivity to be improved
cells. The latter technology, known as the second-gen- further. Contacts are deposed by screen printing that
eration PV cells relies on special process to apply the allows to the electric charges to be collected. Cells are
photovoltaic layer onto a carrier medium. Photovol- then annealed to eliminate solvents and ensure the
taic cells manufacturers of solar cells are constantly mechanical strength.
developing and improving production processes. Finally, a laser is used to isolate the junction. The
Regardless of technology used, large quantities of finished cells are then assembled into modules that
water are required and this eventually results with are characterized and tested under real sunlight.
polluted wastewaters. Water is becoming increasingly
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valuable as a raw material necessitating efficient 2.2. Types of effluents generated: characteristic and
water management of this resource. The wastewater classification
from the production process must be treated in a
way to recycle as much water as possible. The treated Photovoltaic cells production generates different
wastewater must comply with discharge parameters types of effluents from successive processes steps:
in order to prevent pollutants going into environ-
ment. For this reason, optimization of the production • Crystalline growth (elaboration of multi-crystalline
process and the wastewater treatment are often silicon wafers)
necessary [2]. • Silicon wafers sawing
Environmental and economic impacts associated • Texturing
with the photovoltaic systems are mainly due to • Phosphorous doping
hydrofluoric acid (HF) effluents generated during the • Etching
various steps of fabrication. • Metallization
This article provides an overview for the typical
wastewater techniques for silicon solar cell manufac- Some processes steps generate low volumes of
turing. The main steps of the process are described effluents, while others produce significant volumes of
as well as types of waste generated during produc- rinsing water and concentrated acids that must be
tion. Methods of the treatment of HF streams are treated. The process steps that generate the most
presented. In addition, few options for the water significant flux and concentration of wastewater are
reclamation and reuse are discussed and guidelines the following (Fig. 1):
for the design of wastewater treatment systems are
given. • Texturing
• Phosphorous doping
• Photovoltaic cell formation
2. Production process
Typical characteristics of wastewater resulting
2.1. Description
from photovoltaic solar cells wastewater plant are
Solar cells are produced from solar grade silicon summarized in Table 1.
(SOG). Silicon is manufactured by a silica reduction
process in an arc furnace. Metallurgical quality silicon
2.2.1. Texturing
is obtained in this way, containing around 1% impuri-
ties. The silicon then solidifies ejecting metallic Depending on the type of silicon wafers, several
impurities. After that, it is purified using a plasma methods are used for the sawing defects elimination
torch to remove any boron. (texturing process):
The crystallization of the silicon is performed by
extracting heat through the base of the container that • The multi-crystalline silicon wafers need a mixture
allows to the crystals to grow in a controlled way. The of hydrofluoric and nitric acids diluted (HF/HNO3).
 N. Drouiche et al. / Desalination and Water Treatment 3

Table 1 to create the p/n junction in silicon wafer. The

Operational flow for silicon solar cell plant phosphorus diffusion process leads to the formation
Type of wastewater Flow of a layer of phosphorus silicate over the surface of
the silicon wafer, which must be eliminated through
HF-C 217.4 l/h the application of a dilute solution of hydrofluoric
HF (49%) 63.3 l/h acid (HF). This HF must be treated in the wastewater
HCl (37%) 4.2 l/h treatment installation [1].
HNO3 (65%) 78.3 l/h
HF-D 6.275 l/h 2.2.3. Photovoltaic cell formation
CAW 2.531 l/h
IWW 508 l/h The process of deposition of silicon nitride is car-
PreWaCleaner Si 021 1.5 l/h ried out with the aim of reducing the light reflection
CW-D 2.084 l/h on the wafers surface. The treatment chamber must be
Si 2.90 g/l cleaned regularly (for example with an exhaust
SiC 0.26 g/l system for fluoride). Treatment of this evacuation is
PEG 3.67 g/l usually performed by reduction of local systems. It
CH3COOH 1.79 g/l can generate a small amount of wastewater, but the
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InWaCleaner Si 011 20.0 l/h level is relatively low compared to the first three
CT-BW 480 l/h processes. The other production process steps usually
SiO2 2.9 g/l generate little or no wastewater [6].
HF: hydrofluoric acid; HNO3: nitric acid; HCl: hydrochloric acid;
NaOH: sodium hydroxide; NaOCl: sodium hypochlorite; Si: sili- 2.2.4. Effluent characteristics
con; SiC: silicon carbide; PEG: polyethylene glycol; HF-D: HF Wastewater from photovoltaic wafers production
diluted; HF-C: HF concentrated; AWC: acid wastewater concen-
industry contains HF, mixed acid etchant, suspended
trated; CAW: caustic wastewater; CW-D: caustic wastewater
solid (SS), turbidity, SiO2, and high oxide particle. The
diluted; IWW: industrial wastewater.
pH of wastewater is between 2 and 4.
This so called buffer edge solution is needed to
eliminate defects in the crystal structure caused by 2.2.5. Effluent classification
the manufacturing process of the wafers (on the Different types of wastewaters are generated dur-
surface of each wafer). During the process, chemical ing the production of photovoltaic solar cells which
baths are doped in order to maintain the quality of are made from crystalline silicon. Distinction can be
the etching solution constant [1–5]. Nevertheless, the made according to their source (bathing, cleaning),
bath should be completely changed at regular inter- concentration (diluted, concentrated), the chemical
vals, depending on consumption. This requirement (acids, bases), or according to their compositions (con-
leads to a steady flow of HF/HNO3 solutions at a taining fluoride, not containing fluoride) [7,8].
high concentration, which in turn require further In practice, different types of wastewaters are
treatment. classified according to chemical concentration and
• For mono-crystalline silicon wafers, the process is composition. Wastewaters from the production of
usually performed using a mixture of hot caustic photovoltaic cells are generally classified into two
solution with IPA. groups of wastewater:
• As for poly-crystalline silicon wafers, the baths
used in this process must be completely changed at • Rinsing effluent: the rinsing water, which has much
regular intervals and for the same reasons. lower concentrations of chemicals, is treated in situ
in wastewater treatment system.
Concentrated flows of isopropanol (IPA) are • Concentrated acids effluents: strong acids are
problematic, primarily due to their high temperature, generally collected for external discharge.
so they need to be cooled before they are collected for
the final discharge. From the perspective of the composition, the level
of fluoride content is one of the most important
parameters to be considered because of its relatively
2.2.2. Phosphorous doping
strict discharge concentration limit.
During the doping process, phosphorus is used to Fig. 1 shows the process steps and types of
diffuse into the substrate doped with boron in order wastewater streams generated during the production of
 4 N. Drouiche et al. / Desalination and Water Treatment

EUR 2/kg EUR 40-50 kg 1.0-1.5/piece EUR 1.3-1.5/W

Silicon Poly- Ingot Wafer Cell Module System

metal silicon

Fig. 1. Breaking down production process of solar modules with pricing information for various components.

a) BHF/HNO3 conc.
HF-containing
wastewater

HF/HNO3 rinse

HF conc.
Caustic and acid
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wastewater

HF rinse

c)PSG etching

Other : industrial Concentrated acids

d) Si3N4 deposition wastewater
(HF, HNO3)

Fig. 2. Types of effluent during photovoltaic cells manufacturing [1].

typical poly-crystalline silicon. The only difference 3.1.1. Precipitation

between this figure and that of solar cell-based
This method eliminates substances dissolved in
mono-crystalline silicon production resides in the steps of
wastewater. This is achieved by adding chemicals that
the development process, as explained above [1,8] (Fig. 2).
react with the targeted substance to form an insoluble
compound. These reactions generally have an optimum
pH that must be adjusted if necessary. Lime (Ca(OH)2)
3. Treatment methods or calcium chloride (CaCl2), are commonly used for
The usual approach for wastewater treatment in precipitation of fluorides, sulfates, and phosphates. The
solar photovoltaic cells manufacturing is: basic chemical reactions are presented below.
Case of calcium hydroxide:
• Treatment of HF discharges
• Neutralization 2HF þ CaðOHÞ2 ! CaF2 þ 2H2 O ð1Þ
• Collection of discharges containing isopropanol (for
the production of cells based on mono-crystalline
silicon.) Case of calcium chloride:

3.1. Fluoride wastewater treatment 2HF þ CaCl2 ! CaF2 þ 2HCl ð2Þ

Discharges containing fluoride are collected and

3.1.2. Sedimentation
sent for treatment in a physicochemical treatment plant.
In the treatment plants, three steps are performed: Sedimentation is also called settling. It is the physi-
neutralization, sedimentation, and filtration. Insoluble cal separation of suspended solids in a liquid flow
solids generated during the treatment are dried and using gravity. Equipment used in this process involves
sent to a landfill for disposal, as shown in Fig. 3. settling tanks, clarifiers and inclined plate clarifiers,
 N. Drouiche et al. / Desalination and Water Treatment 5

Buffer Treatment Treatment

tank tank II Flocculation
tank I
tank

Filter cake to
external diposal
Pre clarification /
Sludge collection
inclined plate clarifer
Filter press tank

Clear water to neutralisation

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Fig. 3. Diagram of HF wastewater treatment [2].

and thickeners. Some variations in sedimentation units 3.1.4. Neutralization

are inclined plate clarifiers and clarifiers. Retention
Fig. 4 shows a simplified diagram of a typical
time, the rate of surface load, sedimentation rate, and
system of neutralization, which treats wastewater
maintenance requirements of the reactor are the
contaminated by acids or bases. This treatment con-
parameters that must be considered when choosing a
sists on the wastewater pH adjustment to a neutral
sedimentation unit [9,10].
range between 6 and 9 or as required by regulation
emission standards. To meet these requirements, the
3.1.3. Filtration addition of acids or bases might be necessary. Sulfuric
acid (H2SO4) and hydrochloric acid (HCl) are the most
Filtration is a separation process where a mixture commonly used acids in this process. However, HCl
of liquid and solids passes under a pressure gradient generates corrosive vapors and it is not recommended
through a filter medium. The liquid passes through for this process. H2SO4 is the cheapest, easiest, and
the filter medium as a filtrate while the impermeable safest to use. Sodium hydroxide (NaOH) is the
substances are retained as a residue. alkaline chemical most commonly used because it is
Various degrees of filtration can be achieved by both easy to handle and inexpensive. The choice of
changing characteristics of the filter; such as pore size chemicals depends on the cost and operation of the
and filter thickness. By decreasing the pore size, filter plant [10–14].
medium can vary from sand bed filter, paper, and In the neutralization process, design parameters
textiles to membranes. Filtration can also be classified are important, for example: stirring time and dosage
as frontal or as cross flow. In dead-end filtration, fluid of reagents. These factors determine the size of the
which needs to be filtered passes perpendicular to the reactor and that of the metering valve. Particular
surface of the filter. The liquid passes through the attention should be paid to process control and the
medium as a filtrate while substances impermeable to assay reagents [10].
the medium are retained as residues [10].
In the PV industry, frontal filtration (such as the
filter press) is the most common approach for separat- From HF treatment
ing liquids and solids. Solids (as filter cake) are
collected in a shipping container for land application
Drains
or sent to a landfill for disposal. In most cases, the
filter cake (CaF2) is non-hazardous, but due to local PH
Treatment tank I Treatment tank II
requirements it may need special treatment. After HF To sewer
treatment, filtrate is sent to a neutralization system for
pH adjustment [10]. Fig. 4. Neutralization system diagram.
 6 N. Drouiche et al. / Desalination and Water Treatment

4. Collection of isopropanol alcohol (IPA) Cutting fluids are viscous slurry consisting of solid
In the case of solar silicon single crystal production, silicon carbide and fluid glycol. Silicon carbide is used
waste stream containing IPA is separated and collected as a sawing agent in the sawing process of wafers; it is
in containers to be transported to landfill. As described applied to the wire saw in order to provide the
above, other waste streams can be processed in a necessary specific hardness to saw wafers. The glycol
common processing system. acts as substrate as well as a coolant for the silicon
carbide [18].
The effluent of cutting fluids called silicon kerf is
formed as slurry along with the cutting fluid (usually
5. Discharges generated by silicon wafers cutting
polyethylene glycol) and other impurities, mainly
Silicon wafers are cut with the wire saw in order from the broken particles of the SiC abrasive and iron
to obtain wafers of 200 microns thickness. The cutting from the wire. It has a non-negligible environmental
fluids are called “slurry.” This is a mixture of organic and economic impact associated with the manufactur-
solvent and abrasive form of micro beads of silicon ing process of PV systems. During the cutting process,
carbide (SiC). When sawing, it takes care of the silicon they carry silicon and iron particles respectively from
particles and iron (from steel cable) [15–17]. the base material and sawing wire. Disposal of such
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Chemicals water

Acid & HF containing Acid scrubber

exhaust Atmosphere

F-containing
wastewater

Chemicals

HF-containing HF Treatment Filter cake for external

disposal
wastewater

Chemicals

Caustic and acid

wastewater Neutralization PH final Sewer
check

Concentrated acids
Collection External treatment
(e.g.HF, HNO3)

Fig. 5. Standard conception of a photovoltaic cell industry wastewater treatment plant.

 N. Drouiche et al. / Desalination and Water Treatment 7

waste is subject to specific regulations regarding dis- 7. Opportunities for reuse of rinsing water
posal of hazardous waste, which depends on special The rinsing water of the etching process which was
industrial waste plans [19]. These types of wastes not contaminated with nitric acid (HNO3) is collected
must not be leaved or burned in open air. Because of separately in a receiving tank. Therefore a separate line
their highly polluting nature, it is recommended to is required to manage and to recycle only the rinsing
collect, concentrate, and regenerate them [20]. water. In a first step, this rinsing water is filtered to
Separation of the solvent and particles is possible prevent damage to the reverse osmosis membrane by
at about 80% and the rate of reuse can exceed 80% broken particles of silicon wafers or others. The pH
[20]. Regeneration of cutting fluids via simple and value of the filtered water is adjusted before the
cheap processes should allow the reuse of used fluid changeover to the reverse osmosis unit, where fluoride
through recovery of its lubricating characteristics. It salts dissolved in the concentrate are retained [22].
allows reduction of the virgin fluid consumption This concentrate will need additional treatment to
while preserving the environment [18]. precipitate fluorides to meet specific requirements. The
permeate from reverse osmosis could be recovered
and used for many purposes, such as water supply for
6. Wastewater treatment plant design scrubbers and cooling towers [1,22].
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Fig. 5 shows a standard installation of the waste-

water treatment. In this case, the priority in terms of
performance is closely related to the HF discharges 8. Zero discharge concepts
neutralization treatment system. The production of solar cells is increasingly
Concentrated acids are generally collected on site in transferred to countries in which the cells produced
containers and then transported for external treatment. can be effectively used on account of intensive solar
A variation of design standard for wastewater radiation. In these countries (in southern Europe or
treatment does not include the HF or a concentrated northern Africa, for example), there is often a severe
acids treatment step. In this case, neutralization is the shortage of water. For this reason, concepts for water
only operation used. This type of treatment system was recycling, going as far as “zero discharge” are sensible
designed and installed in practice [1]. and cost-effective there.
The wastewater from scrubbers must not be Such a concept has been devised for a customer.
neglected when designing the wastewater treatment From river water treatment to recirculation, a complete
system in terms of HF mass flow. Although the process for water management with “zero discharge”
amount of water is relatively low compared to that criteria was developed. The important thing is to
from various production processes, it represents a master the production process in order to be able to
significant amount in the total HF effluent flow from close the circuit. The production in question is a wafer
the manufacturing plant. This is because the wastewa- and cell production system (Fig. 6). The wastewater is
ter generated by the scrubber depends on the type of classified according to the following criteria:
etching process used.
In terms of discharge limits, the design of wastewa- • Sanitary wastewater from the administration
ter treatment plant strictly depends on its location. For department.
example, the release limit for fluoride differs depend- • Organically contaminated rinsing water from wafer
ing on the different countries or regions. Germany has production.
no general validity. Discharge standards of fluoride • Inorganically contaminated concentrates from cell
depend on requirements of local authorities, ranging production.
from less than 20 mg/L to 50 mg/L [21]. In India • Inorganically contaminated rinsing water.
where natural waters are naturally concentrated in
Fluor, the standard for discharge is <2 mg/L [2]. The weakly contaminated rinsing water is treated
Local infrastructure is another important parame- by reverse osmosis process after an appropriate
ter when designing the installation of releases. conditioning. Permeate is fed back before the water
Discharges of concentrated acids are usually collected treatment plant for high-purity production water. This
and sent to a landfill or for treatment in a specialized makes it possible to save considerable quantities of
treatment center, and if this is possible they might be water.
treated on site. This factor must be considered when The concentrates from the reverse osmosis as
building the plant and waste treatment installation well as for all other wastewater are treated in the
must be constructed. chemical–physical treatment plant. Uniform inflow
 8 N. Drouiche et al. / Desalination and Water Treatment
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Fig. 6. Complete process for water management [22].

conditions are important for stable functioning. For major concern. It is used extensively in PV manufac-
this reason, concentrates (discontinuously discharged turing for wafer etching and quartz cleaning opera-
or rejected treatment baths) are collected separately tions. Fluoride concentrations of 500–2,000 mg/L are
and then dosed. The pretreated inorganic wastewater found in typical wastewater of local PV industry.
is then evaporated. All organically contaminated Fluoride contamination in certain aquatic systems
wastewater is subjected to anaerobic biological worldwide has caused health concern. Due to its high
treatment. The cleaned wastewater is treated by toxicity, industrial wastewater containing fluoride is
membrane technology in order to be used in the strictly regulated.
cooling tower [2]. Contamination can be safely and efficiently
removed from wastewater using conventional
precipitation/neutralization processes or by especially
9. Conclusion
engineered polymers and membrane technologies to
Photovoltaic (PV) energy conversion is increasingly comply with the strictest standards. Using the new
regarded as a technology which may contribute to the treatment technology, photovoltaic cell industries can
world energy supply in a way that is compatible with reduce operating costs, reprocess the water to allow
the concept of sustainable development. However, to either recycling within the same processes or reuse it
ensure that PV energy can indeed fulfill this in another process in the facility, comply with expand-
expectation, a careful consideration of potential ing environmental regulation and improve relations
environmental risks of PV energy conversion is neces- within the local community.
sary. PV manufacturing process, which requires
extremely high precision, generates both conventional
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