Silicon for the chemical and solar industry XVII

Edited by M.Tangstad, H.Rong, A.Valderhaug, B.Andresen and I.G.Page

Trondheim, 10-13 September 2024

Use of Agglomerates in Silicon Production

Tin Tin Kyaw1, Merete Tangstad2

1Department of Materials Science and Engineering, Norwegian University of Science

and Technology, Trondheim, Norway, [email protected]

2Department of Materials Science and Engineering, Norwegian University of Science

and Technology, Trondheim, Norway, [email protected]

Keywords: charcoal, Sio generation, SiC generation, SiO reactivity

Abstract –The effect of reaction temperatures on carbothermic reactions between quartz-silicon

mixture (SiO2-Si mixture) and four kinds of charcoal materials (charcoals A, B and charcoal
briquettes AA, BB) is studied. Referred to previous work, the comparison of results indicated that
Silo generation is increased with the increasing reaction. With increasing temperature, the SiC
formation increased significantly in charcoals A and charcoal briquettes while a slight increase
was seen in charcoal B. Thus, SiO gas diffusion in charcoal materials except charcoal B is quite
temperature dependent. Charcoal briquettes had comparable silicon monoxide (SiO) reactivity as
charcoals. The tumbling of charcoal materials contributed to their decrepitation. Charcoal
briquettes with the lowest tumbling strength decrepitated more than other charcoal materials at
high temperatures. The decrepitation of charcoal materials increased with the increased reaction
temperature.

1. INTRODUCTION
From the mining of raw materials to the production of metallurgical grade silicon (MG-Si), the
total greenhouse gas emission has been estimated to be around 12 metric tons of CO2-
equivalents per ton of MG-Si produced (Saevarsdottir et al., 2023; Sævarsdottir et al., 2021). As
bio-based carbon mix (charcoal and woodchip) has lower environmental impacts compared to
conventional charge mix (coke and coal), replacing part of the current fossil reductants with
biocarbon is a probable approach to mitigate the fossil CO2 emissions from the
silicon/ferrosilicon industry. Using woody biomass such as charcoal improves the quality of
metal as its sulfur and ash contents are less than those of fossil reducers (Kumar and Gupta,
1998; Wei et al., 2017). In silicon production which requires high Si purity, charcoal makes it
possible to obtain silicon metal with better chemical specifications for polysilicon applications
in the photovoltaic industry (Braga et al., 2008).
Reaction [1] represent an overall reaction in silicon production. It is a combination of sub-
reactions reacting at different locations and temperatures within the furnace. The submerged
arc furnace is divided into three different zones: combustion zone, low-temperature zone
below 1700° C, and high-temperature zone from 1700°C and up to more than 2000°C. In the
combustion zone, CO and SiO ascending from the high temperature zone, through the lower
temperature zone, react with open air, resulting in condensed silica and carbon dioxide. In the
low-temperature zone, the ascending SiO gas from the lower part of the furnace can react with
carbon, as given in reaction [2]. SiO generation occurs in the high-temperature zone,
particularly from the reaction of quartz and silicon (reaction [3]), and from the reaction of
quartz and silicon carbide (reaction [4]). The generated SiO gas reacts with SiC and produces
silicon liquid metal, which is stated in the reaction [5] (Schei et al., 1998; Tangstad, 2013).

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 𝑆𝑆𝑆𝑆𝑆𝑆2 (𝑠𝑠, 𝑙𝑙) + 2𝐶𝐶(𝑠𝑠) = 𝑆𝑆𝑆𝑆(𝑙𝑙) + 2𝐶𝐶𝐶𝐶(𝑔𝑔) [1]

𝑆𝑆𝑆𝑆𝑆𝑆(𝑔𝑔) + 2𝐶𝐶(𝑠𝑠) = 𝑆𝑆𝑆𝑆𝑆𝑆(𝑠𝑠) + 𝐶𝐶𝐶𝐶 (𝑔𝑔) [2]

𝑆𝑆𝑆𝑆𝑆𝑆2 (𝑠𝑠, 𝑙𝑙) + 𝑆𝑆𝑆𝑆(𝑙𝑙) = 2𝑆𝑆𝑆𝑆𝑆𝑆(𝑔𝑔) [3]

2𝑆𝑆𝑆𝑆𝑆𝑆2 (𝑠𝑠, 𝑙𝑙) + 𝑆𝑆𝑆𝑆𝑆𝑆(𝑠𝑠) = 3𝑆𝑆𝑆𝑆𝑆𝑆(𝑔𝑔) + 𝐶𝐶𝐶𝐶(𝑔𝑔) [4]

𝑆𝑆𝑆𝑆𝑆𝑆(𝑔𝑔) + 𝑆𝑆𝑆𝑆𝑆𝑆(𝑠𝑠) = 2𝑆𝑆𝑆𝑆(𝑙𝑙) + 𝐶𝐶𝐶𝐶(𝑔𝑔) [5]

Silica- and carbon-waste is formed from the raw materials preparation, transportation, and
industrial processing of quartz and carbonaceous materials. The direct use of these fine ore
wastes in the submerged arc furnace will cause bad permeability of the charge layer and
unstable furnace conditions (Jusnes et al., 2020). Therefore, these waste fines can be used to
prepare agglomerates in the industrial silicon production process to improve resource
utilization, stabilize submerged arc furnace operation, and improve the thermal balance of the
furnace.
The most common agglomeration techniques are pelletizing, briquetting and extrusion. The
fundamental processing difference is the use of a piston or screw press for briquetting and
extrusion, whereas biomass pellets are produced in a pellet mill (Stelte et al., 2012). In
agglomerates, binder plays an essential role that determines their strength, thermal stability,
combustion performance and cost of agglomerates (Altun et al., 2001). Binder can be divided
into three categories: organic binder, inorganic binder, and compound binder (Chen et al.,
2009; Kpelou et al., 2019). The organic binder has good bonding performance but may
decompose at medium to high temperatures leading to lower mechanical strength and thermal
stability. The inorganic binder provides thermal stability, strong adhesion, non-pollution, low
cost, and good hydrophilicity. The inorganic binder will however add more trace elements.
The compound binder is composed of two or more organic or inorganic binders, consisting of
the benefits of different types of binder and improving the quality of agglomerates (Zhang et
al., 2018).
In this study, the carbothermic reaction between SiO gas and four different types of charcoal
materials (charcoals A, B and charcoal briquettes AA and BB) at 1800°C is investigated. The
SiO gas is produced from a quartz-silicon mixture (SiO2-Si mixture). Referring to previous
work done at 1700°C [reference], the 1700°C will be compared to the 1800°C results found in
this work.

2. EXPERIMENTAL PROCEDURE
2.1. Materials Preparation
The carbothermic reaction between SiO gas from SiO2-Si mixture and four different charcoal
materials at 1800°C was investigated. Figure 2 illustrates the overview of experimental stages
of SiO generation, SiC formation and characterization methods. Quartz and silicon (800-1000
µm) are used as a source of SiO generation as per reaction [3] and two diverse types of
charcoals (A, B, lab-made briquette AA, and commercial briquette BB) are employed to study
SiC formation as per reaction [2]. Table I shows the chemical composition of quartz and

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silicon, which both have a purity of around 99 wt.%. Charcoal A was previously used in pilot-
scale experiments conducted by Andersen (Andersen et al., 2023). Lab-made charcoal
briquettes AA were made from charcoal A and corn starch as a binder in a ratio of 9:1 (charcoal
A: corn starch) at 5 bar by using a hydraulic press machine. Charcoal B and charcoal briquette
BB with an unknown binder are commercial charcoal products from the Perechin Timber-
Chemical Plant in Ukraine.
Table II states the proximate analysis of charcoal materials, which shows that charcoal
briquette have lower fix C and higher volatiles due to the added binder. The porosity of
charcoal materials in a particular size larger than 10 mm and tumbling strength index (TSI) of
charcoal materials in a particle size of 8-12.5 mm are described in tables III and IV. Charcoal
briquettes have lower porosity than lumpy charcoals. Charcoal briquette AA has a lower
tumbling strength than other charcoal materials.

Figure 2: Schematic diagram of experimental work

Table I: Chemical composition of raw materials

Content (wt.%) SiO2 Si Al2O3 CaO Cr2O3 Fe2O3 K2O Na2O MgO MnO
Quartz 99.73 - 0.19 0.0075 <0.001 0.025 0.029 0.0052 0.0071 0.0035
Silicon - 99.95 0.006 0.0048 0.0018 0.03 0.0022 0.0008 0.0018 0.0019

Table II: Proximate analysis of charcoal materials

Charcoal materials Fix C Volatiles Ash Moisture
A 83.05 14.90 2.05 3.73
AA 75.84 21.95 2.21 2.88
B 82.74 12.92 4.34 3.08
BB 75.28 20.27 4.45 5.22

Table III: Average porosity result of three different samples of each charcoal materials
Charcoal Weight Absolute density Apparent density Porosity Standard deviation
materials (g) (g/cm3) (g/cm3) (%) (%)
A 0.36 1.43 0.48 66.44 10.08
AA 0.33 1.43 0.59 58.43 1.29

B 0.22 1.36 0.48 65.96 5.05

BB 0.56 1.55 0.71 53.89 3.22

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Table IV: Tumbling strength index of charcoal materials
Charcoal materials TSI+3 mm (%) Standard deviation (%)
A 80.73 2.96
AA 26.69 9.02
B 72.84 2.29
BB 80.12 4.65

2.1. SiC Formation Test

The charcoal materials are prepared in a particle size of 2.5-3.15 mm for the SiC formation test
based on the inner diameter of crucible (Ø 30 mm). As the crucible and sieve are graphite
materials, they are coated with boron nitrite paste to slightly prevent from the reaction
between SiO gas generated from SiO2-Si mixture and graphite. Then, SiO2-Si mixture is placed
at the bottom of the crucible in the reaction chamber and is split from charcoals using a
graphite sieve. Then, the SiC formation test is conducted at 1800°C for 2 hours under Argon
(Ar) gas atmosphere using Thermal Technology LLC- 1000-3560-FP20-Resina Furnace and
each test is repeated twice.

2.1. Characterization
The SiO generation rate is investigated by measuring the weight changes of quartz and silicon
before (𝑀𝑀 (𝑆𝑆𝑆𝑆𝑆𝑆2 + 𝑆𝑆𝑆𝑆)𝑓𝑓 )and after the test (𝛥𝛥𝛥𝛥 (𝑆𝑆𝑆𝑆𝑆𝑆2 + 𝑆𝑆𝑆𝑆)𝑖𝑖 , as shown in equation [1]. For SiC
formation, charcoal materials after the test are sent to D-LAB, Degerfors Laboratorium AB to
analyze total C, Free C, and Si, and then the content of SiC is calculated by equations [2] and
[3].
To study the morphology of the after-test charcoal materials, they are firstly mounted with a
ratio of 10:6 of clarocit powder and clarocit liquid, followed by grinding with abrasive SiC
paper and polishing with 3 µm and 1 µm polishing plates with diamond paste using a
combined grinding-polishing machine (Struers TegraPol-31). The microstructure and
mapping analysis are observed using a high-performance thermal field emission electron
probe microanalyzer (EPMA) (JEOL-JXA 8500F-Miroprobe). Charcoal materials after the test
are sieved using 2.5-3.15 mm sieves to determine the decrepitation. The final weight of
charcoal materials after the test (𝑊𝑊𝑓𝑓 ) and the weight of charcoals in a size of 2.5-3.15 mm
(𝑊𝑊𝑓𝑓+2.5 𝑚𝑚𝑚𝑚 ) after sieving are used to calculate weight percent of charcoal materials greater than
2.5 mm by equation [4].

𝛥𝛥𝛥𝛥 (𝑆𝑆𝑆𝑆𝑆𝑆2 +𝑆𝑆𝑆𝑆)𝑓𝑓

% 𝑆𝑆𝑆𝑆𝑆𝑆 𝑐𝑐𝑐𝑐𝑐𝑐𝑐𝑐𝑐𝑐𝑐𝑐𝑐𝑐𝑐𝑐𝑐𝑐𝑐𝑐 𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟 = 𝛥𝛥𝛥𝛥 (𝑆𝑆𝑆𝑆𝑆𝑆2 +𝑆𝑆𝑆𝑆)𝑖𝑖
× 100 [1]
𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚 𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚 𝑜𝑜𝑜𝑜 𝑆𝑆𝑆𝑆𝑆𝑆
% 𝑆𝑆𝑆𝑆𝑆𝑆 = % 𝑆𝑆𝑆𝑆 × [2]
𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚 𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚 𝑜𝑜𝑜𝑜 𝑆𝑆𝑆𝑆
𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚 𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚 𝑜𝑜𝑜𝑜 𝑆𝑆𝑆𝑆𝑆𝑆
% 𝑆𝑆𝑆𝑆𝑆𝑆 = ( 100 − % 𝐶𝐶𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡 − % 𝑎𝑎𝑎𝑎ℎ) × 𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚 𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚 𝑜𝑜𝑜𝑜 𝑆𝑆𝑆𝑆
[3]
𝑊𝑊𝑓𝑓+2.5 𝑚𝑚𝑚𝑚
% 𝐶𝐶𝐶𝐶𝐶𝐶𝐶𝐶𝐶𝐶𝐶𝐶𝐶𝐶𝐶𝐶𝐶𝐶𝐶𝐶 𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝 𝑜𝑜𝑜𝑜 𝑐𝑐ℎ𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎 + 2.5𝑚𝑚𝑚𝑚 = � � × 100) [4]
𝑊𝑊𝑓𝑓

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3. RESULTS AND DISCUSSION

3.1. SiO Generation

Referring to the previous work of SiO generation rate at 1700°C, figure 3 illustrates a
comparison of SiO generation rate at 1700°C and 1800°C. This is done with different carbon
materials (charcoal A, B and charcoal briquettes AA, BB) ; however, this should not affect the
SiO generation. At 1700°C, the difference in SiO generation rate is around 0.36 wt.% in average
for charcoal materials. The SiO generation rate at 1800°C is around 0.29 wt.% in average higher
than that at 1700°C due to increased reaction rate between quartz and silicon when the
temperature changed from 1700°C to 1800°C.
Although the amount of quartz and silicon is equally used to generate the SiO gas, a slight
difference in the SiO generation rate was observed between experiments at the same
temperature. One fact is that although boron nitrite coated crucibles and sieves were used, the
bottom of the crucible and sieve were close to the SiO2-Si mixture and may have reacted with
the SiO gas. This consumes SiO gas before it reached the charcoals, resulting in more SiO2-Si
mixture consumption. Another fact is that melted silica and silicon were sometimes left
stickily to the bottom and wall of the crucible, then the weight of the leftover SiO2-Si mixture
is not precise to measure.

Figure 3: SiO generation comparison in charcoal materials with SiO2-Si mixture at 1700°C and 1800°C. It must be
noted that the type of charcoal should not affect the SiO rate.

3.2. SiC Formation

The generated SiO gas from SiO2-Si mixture passes through pores in the charcoal materials
and reacts with carbon, producing SiC as given in reaction [2]. Figures 4 and 5 demonstrate
backscattered electron (BSE) images and EPMA mapping analysis of each charcoal material at
1800°C. Both bright and dark areas are observed in each charcoal materials. In figures 4(a-b),
charcoal A has a porous structure, where rings of the pores of charcoal A (bright areas) were
reacted with SiO gas and converted to SiC, whereas the inside of pores was filled with epoxy
and might or might not react with the SiO gas. Distribution of Si and C is also high in the rings
and some areas according to the EPMA map of charcoal A in figures 5(a). Charcoal briquette
AA in figures 4(c-d) has a different microstructure with no pores. Some bright areas in charcoal

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briquette AA are SiC with high concentration of Si and C while some areas have low
concentration of Si and C, remained unreacted with the SiO gas, as shown in figure 5(b). In
figures 4(e-f) and 5(c), the microstructure of charcoal B is similar to charcoal briquette AA. The
bright areas of charcoal B with high amount of Si and C are SiC while some areas (dark) are
left unreacted. Similarly, in figures 4(g-h), and 5(d), charcoal briquette BB has a similar
structure with charcoal B and has bright areas (SiC) with high distribution of Si and C and
dark areas where some areas didn’t convert to SiC. It has been observed that SiC started
nucleation on the surface and pores of charcoal materials which fits with this work
(Jayakumari and Ringdalen, 2022). One can also see a topochemical reaction in Figure 4(g).

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Figure 4: Overview and 200x magnification back scattered electron (BSE) morphology of SiC in (a-b) charcoal A,
(c-d) charcoal briquette AA, (e-f) charcoal B, and (g-h) charcoal briquette BB at 1800°C

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(a)

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 Figure 5: EPMA Mapping of SiC in (a) charcoal A, (b) charcoal briquette AA, (c) charcoal B, and (d) charcoal
briquette BB

Figures 6 (a-d) compares SiC formation in charcoal materials as a function of SiO generation
from SiO2-Si mixture at both reaction temperatures. Linear trendlines are added in the graphs
to understand the data clearly. In figure 6(a), charcoal briquette AA converted to SiC faster
than charcoal A at both 1700°C and 1800°C. The SiC formation in charcoal briquette BB at
1700°C in figure 6(b) was almost as equal as that in charcoal B but charcoal briquette BB

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converted to SiC much quicker than charcoal B at 1800°C. Thus, charcoal briquettes converted
to SiC faster or at least as equal as charcoals, however, the difference in 3 of 4 is quite small.
This is hence not related to the porosity, as the porosity of the briquettes were a bit lower than
the lumpy material.

In figure 6(c), charcoal A converted to SiC slightly slower than charcoal B at 1700°C but when
the temperature increased to 1800°C, the transformation of charcoal A to SiC is faster than that
of charcoal B. Among briquettes in figure 6(d), the SiC conversion in charcoal briquettes BB is
faster than charcoal briquettes AA at both reaction temperatures. Therefore, charcoal A and
charcoal briquette BB has more SiO reactivity than charcoal B and charcoal briquette AA.

To summarize, the SiC conversion in charcoal materials apart from charcoal B increased
significantly when the reaction temperature increased to 1800°C. Thus, the diffusion of SiO
gas in charcoal A, charcoal briquettes AA and BB is temperature dependent while that in
charcoal B is more reaction rate determining.

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 11

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 Figure 6: SiO generation versus SiC formation comparison in charcoal materials with SiO2-Si mixture at 1700°C
and 1800°C (a) A vs AA (b) B vs BB (c) A vs B, and (d) AA vs BB

3.3. Decrepitation of Charcoal Materials During Heating and Reaction

Figure 7 shows a comparison of the cumulative weight percent of each charcoal materials
larger than 2.5 mm after the SiC formation test at 1700°C and 1800°C. In figure 7(a), charcoal
A was left a higher weight of charcoal particles > 2.5 mm than charcoal briquettes AA,
indicating that charcoal briquettes AA decrepitated more than charcoal A at both 1700°C and
1800°C. This shows that charcoal briquette AA is thermally and mechanically weaker than
charcoal A due to its higher decrepitation and lower tumbling strength. This is quite expected
as the agglomeration process and binder used was not optimized.
In figure 7(b), charcoal B and charcoal briquettes BB decrepitated almost equally at 1700°C
but charcoal B decrepitated more than charcoal briquettes BB at 1800°C. As charcoal briquette
BB has lower decrepitation and slightly higher tumbling strength than charcoal B, it is
thermally and mechanically stronger than charcoal B. In figure 7(c), the differences in
decrepitation in charcoal A and B are not significant at both reaction temperatures, however,
charcoal briquette AA decrepitated more than charcoal briquette BB.
To summarize, charcoal briquette AA decrepitated the most compared to others, probably due
to its inherent lower tumbling strength. The other charcoal materials was mainly in the same
area between 55 and 70% (+2.5mm), and was probably within the variation in the material.

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.

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Figure 7: Cumulative percent of charcoal materials above 2.5 mm at 1700°C versus at 1800°C a) A vs AA (b) B vs
BB (c) A vs B, and (d) AA vs BB

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4. CONCLUSION
In the study of SiO2-Si mixture and four different charcoals at 1800°C, SiO generation and SiC
formation increased with increasing the reaction temperature. Charcoal briquettes have
comparable SiO reactivity as charcoals. The decrepitation of charcoal materials could relate to
their tumbling strength. Charcoal briquette AA with the lowest tumbling strength
decrepitated more than to others. This is expected as this was the lab-made briquette, and as
such the binder and briquetting procedures was not optimized.

To conclude, using biocarbon such as charcoal is not only an approach to reduce greenhouse
gas emissions and could therefore be a sustainable carbonaceous reductant in silicon
production. In this work, the SiO reactivity and the thermal strength of agglomerates showed
similar properties as the lumpy material and could replace the lumpy material.

5. ACKNOWLEDGEMENT
The authors acknowledge the Norwegian Research Council for the financial support through
the KSP project “Biomet” (336175) and Perechin Timber-Chemical Plant in Ukraine for the
charcoal materials.

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Tin Tin Kyaw

PhD candidate, Norwegian University of Science and Technology, Norway

The author is currently studying in silicon production with biocarbon. She

graduated in Master of Engineering (Industrial Engineering) at King
Mongut’s Institute of Technology Ladkrabang in Thailand and in Bachelor of
engineering (Materials and Metallurgical Engineering at University of
Technology (Yatanarpon Cyber City) in Myanmar. She also studied as a special research
student for one year at Tohoku University in Japan.

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