Azadeh Goudarzi

Department of Materials Engineering,

University of British Columbia,
6350 Stores Road,
Vancouver, BC V6T 1Z4, Canada
e-mail: goudarzi@mail.ubc.ca
Li-Ting Lin
Department of Materials Engineering,
University of British Columbia,
6350 Stores Road,
Vancouver, BC V6T 1Z4, Canada
Frank K. Ko
Department of Materials Engineering,
University of British Columbia,
6350 Stores Road,
Vancouver, BC V6T 1Z4, Canada
X-Ray Diffraction Analysis of
Kraft Lignins and Lignin-Derived
Carbon Nanofibers
Lignin is a renewable material and it is abundantly available as low priced industrial
residue. Lignin-based carbon bers are economically attractive and sustainable. In addi-
tion, remarkably oxidized molecule of the lignin decreases the required time and temper-
ature of the thermostabilization process compared to other carbon ber precursors such
as polyacrylonitrile (PAN); and thus, decreases the processing cost of carbon ber pro-
duction. The fraction 4 of softwood Kraft lignin (SKL-F
4
) was previously shown to be
spinnable via electrospinning to produce carbon nanobers. In this paper, we character-
ized different Kraft lignin powders through X-ray diffraction (XRD) analysis to measure
the mean size of the ordered domains in different fractionations of softwood and hard-
wood samples. According to our results, SKL-F
4
has largest ordered domains among
SKLs and highest hydroxyl content according to Fourier transform infrared (FTIR) anal-
ysis. In addition, variations in the XRD patterns during carbon nanober formation were
studied and the peak for (101) plane in graphite was observed in the carbon nanober
carbonized at 1000

C. [DOI: 10.1115/1.4028300]
Keywords: lignin, XRD, carbon nanober, electrospinning
Introduction
Lignin is one of the most abundant renewable materials on
earth. Kraft lignin is available as an industrial residue in large
quantities, which is usually burnt as low efciency fuel [1,2]. One
of the promising potential applications for lignin valorization is
production of advanced material, such as lignin-based carbon
bers (CFs). The low cost of lignin, and the fact that it is a renew-
able resource, make it an attractive material to fabricate CFs. The
predominant CF precursor is polyacrylonitrile (PAN, [C
3
H
3
N]
n
)
followed by petroleum pitch, and rayon [3]. The demand for CF is
estimated as 70,000 tons/yr by 2015, if the current 1015%
growth rate is maintained [46]. The price of CF has dropped tem-
porarily in recent years, but is still too high for widespread indus-
trialization. A low cost alternative like lignin would expand the
range of applications. The cost of PAN is over 50% of the total
manufacturing cost of the CF and commercial grade PAN-based
CF is around $20/kg. With lignin-based CF, the manufacturing
cost could be reduced to less than $10/kg, making lignin an attrac-
tive alternate precursor for CF production [2]. In addition to lower
cost of lignin as the precursor, lignin molecule is substantially oxi-
dized compared to PAN, therefore oxidative thermostabilization
process of lignin bers requires shorter stabilization time and
lower stabilization temperature than PAN bers, which translates
to lower processing cost [2,7,8].
Lignin is an amorphous phenyl propylene polymer, which does
not hold most of the CF forming requisites of a polymer (e.g., lin-
ear and exible structure, high degree of symmetry, high molecu-
lar mass >1000 A

, high degree of crystallinity, high degree of

orientation, and high carbon content) [9]. However, lignin CFs
have successfully been prepared from different types of lignins
through different methods (electrospinning, melt-spinning, and
wet spinning) [10,11]. Yet, the challenge remains preparing a
consistent and uniform lignin substrate from such complex and
variable compound [7,8]. The reported mechanical properties of
the lignin-based CFs are relatively lower than the PAN-based CFs
(e.g., tensile strength of 0.51 GPa compared to 37 GPa)
[8,1216]. Understanding the process in which the complex mole-
cule of lignin forms ber and the process of carbonization of such
ber is not clearly known. Understanding such process might
assist improving the properties in the future. Therefore, in this
paper we studied XRD analysis of different Kraft lignin powders
to examine the mean size of the ordered domains. We also studied
the carbonized lignin bers produced from electrospinning pro-
cess. XRD analysis previously was reported for lignins [1719],
but to our knowledge the size of the ordered domains and diffrac-
tion angel of the Kraft lignins were not reported.
Materials and Methods
Softwood Kraft lignins (SKL) and hardwood Kraft lignin
(HKL) were from FPInnovation, HP-L lignin was from Lignol.
Lignins are composed of a mixture of different sized molecules.
Lignin fractionation is method to separate different sized mole-
cules, either through dissolving/precipitating the lignin in differ-
ent organic solvents or using membranes [20,21]. Dallmeyer
studied electrospinning of softwood lignins and showed that the
higher molecular weight fraction, fraction 4, is spinnable through
electrospinning [22]. Therefore, we used fractionation 4 SKL
(SKL-F
4
) for electrospinning. SKL-F
4
:PEO with the 99:1 (w/w)
ratio was dissolved in dimethylformamide at 30 wt.% concentra-
tion. The polymer solution was electrospun using a number
25-gauge needle spinneret at a spinning distance of 18 cm, at
20 kV applied voltage, and a 0.03 ml/min ow rate. The ber mat
was hold in a stretched position using Teon coated glass sheets
in a glass petri-dish and thermostabilized for 1 h at 200

C with
heating rate of 3

C/min in air. Then, the ber mat is carbonized

in N
2
environment in a tube furnace at 1000

C for 1 h.
The XRD analysis instrument was a Rigaku model MultiFlex
diffractometer, running on Cu-Ka (k 1.542 A

). The lignin pow-

der data were collected at standard 2 deg/min scan rate. The
highly porous nature of ber mats required longer data collection
times to obtain sufcient amount of diffracted X-rays, therefore
scan rate of 0.05 deg/min was applied. A Perkin Elmer spectrum
100 was used to perform FTIR analysis, using attenuated total
reection sampling technique and a diamond coated Tl-Br-I plate.
Manuscript received April 9, 2014; nal manuscript received July 17, 2014;
published online September 4, 2014. Assoc. Editor: Hsiao-Ying Shadow Huang.
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2014 by ASME
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Microstructure analysis was conducted by a Hitachi S3000N
Tungsten hairpin lament source SEM. To calculate the ber
diameter, the average of 100 measurements in four different SEM
image was used. A Q500 TA instrument was used for thermo
gravimetric analysis (TGA). The tests were performed in N
2
and
air, by heating rate of 10

C/min.
Results and Discussion
Lignins have three precursors: p-coumaryl alcohol, coiferyl
alcohol, and sinapyl alcohol [1,23]. The polymerization of these
three primary monomers results in formation of structural units in
lignin: p-hydroxyphenyl (H), guaiacyl (G), and syringyl, respec-
tively [24]. Approximately, 90% of SKL units are G units [1,23].
HKL units contain both G and S units. FTIR spectroscopy,
according to Popescu et al. is an important tool for structural char-
acterization between hardwood and softwood samples [25]. Figure
1 shows FTIR spectra of the lignin powders. The hydroxyl region
of the spectra (3000 cm
1
3700 cm
1
) shows that SKL-F
4
had the
highest amount of hydroxyl groups available. A distinctive differ-
ence between HKLs and SKLs is the ratio of the peaks at
1130 cm
1
and 1030 cm
1
: in softwoods 1130 cm
1
<1030 cm
1
and in hardwoods 1130 cm
1
>1030 cm
1
. The peak at
10301035 cm
1
is allocated to Aromatic CH in plane deforma-
tion, where amount of G units are higher than S units, this region
is also allocated to CO deformation in primary alcohols, and
CO stretch (unconjugated) [26,27]. Peaks at the wavenumber
range of 12661270 cm
1
are associated with G ring vibrations
and as shown in Fig. 2, they are not present in HKL samples.
Twin peak at 855 cm
1
and 815 cm
1
is assigned to softwoods
and single peak at 835 cm
1
to hardwoods [26]. The presence of
more methoxyl groups attached to the aromatic rings in HKLs (S
unit) inhibits formation of 55 or dibenzodioxocin linkages [1],
where for SKLs b-O-4 linkages are more predominant. Differen-
ces in the available functional groups might affect stacking of the
molecules and affect size of the ordered domains in the samples.
To calculate the size of the ordered domains, XRD analysis was
acquired. Figure 2 shows XRD patterns of the three fractions of
HKLs, three fractions of SKLs and HP-L powder samples. For
each sample, peak tting was performed for four different rene-
ments: PearsonVII, Pseudo-Vigot, Lorentzian, and Gaussian.
Gaussian character was predominant in overall peak shape for
softwood samples and Lorentzian character was predominant in
hardwood samples and HP-L. After tting the curves, the maxi-
mum diffraction angel was determined for each sample. The aver-
age peak for hardwoods is located at 2h 21.2 60.15 deg and for
softwood it is located at 2h 19.35 60.18 deg (Table 1 shows the
values for each sample). Kubo et al. reported the diffraction angel
of 22.7 deg for hardwood acetic acid lignin [18] and Ansari and
Gaikar reported 2h 22.37 deg for lignin from sugar mill [19].
Such differences could be caused by the difference in the lignin
type. The Scherrers equation is usually used for calculating
the mean size of the ordered domains (crystallite):
d Bk=bcosh, where d is the mean size of the ordered domains,
Bdimensionless shape factor (value of 0.9 is used [28,29]),
k X-ray wavelength (0.154 nm for Cu K-a), and b full width
at half maximum (FWHM) [30]. To measure the FWHM, instru-
mental broadening effect should be subtracted from the data.
Table 1 shows the results of calculated mean size of the ordered
domains (d in Scherrers equation) for lignins. Among SKLs,
the fraction 4 had the highest size of the ordered domains.
According to literature, SKL-F
4
has ber forming ability by
Fig. 1 FTIR spectra of lignin powders
Fig. 2 XRD patterns of the lignin powders
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electrospinning method [22]. Among HKLs, the unfractionated
sample (HKL) had the highest size of the ordered domains. How-
ever, because unfractionated sample is composed of different
sized molecules in its structure (higher polydispersity index),
when spinning parameters were adjusted for one portion of the
molecular weight (e.g., viscosity of the solution), the other por-
tions were not spinnable. In other words, although some ber for-
mation was observed in electrospinning, spraying also occurred.
Therefore, SKL-F
4
was selected for nanober production via
electrospinning and further analysis of the nanobers.
Carbon content is an important factor in a CF precursor. Figure
3 shows the results of elemental analysis of the lignin powders by
energy-dispersive X-ray spectroscopy (EDS) method to measure
carbon and sulfur content. EDS is considered a qualitative method
for elemental analysis, specially, when the energy region in below
3 keV. A procedure in which corrections for atomic number
effects (Z), absorption (A), and uorescence (F) are calculated,
are called ZAF correction and usually available in instrument
settings [31]. The ZAF correction was selected for better
accuracy of the results. However, we are aware that the results
presented in Fig. 3 are relative rather than absolute values. The
presented EDS results are the average of at least six analyses.
Relatively, HP-L sample was a sulfur-free lignin and the sulfur
content of the SKL-F
4
was the highest among SKLs. SKL-F
4
was
previously shown to be spinnable via electrospinning [22]. As a
summary from the lignin powder characterization, SKL-F
4
had
the highest hydroxyl and sulfur content, and the highest size of the
ordered domain among SKLs. We produced and electrospun
SKL-F
4
bers and characterized the produced carbon nanobers.
Figure 4 shows (a) as-spun ber, (b) thermostabilized ber, and
(c) the carbonized ber with their EDS analysis results for carbon
and sulfur content. The sulfur content was decreased by thermal
treatment, which probably could be due to the release of SO
2
gas
during the heat treatment. Further investigation such as analyzing
the gas content of the sample is required to conrm release of SO
2
gas. The decomposition temperature in air was higher than decom-
position temperature in N
2
environment for the SKL-F
4
lignin
powder (Fig. 5, Td in air: 475

C and in N
2
was 376

C, SD<1

C
for three tests). The reason for oxidative stabilization (thermosta-
bilization) process is to increase stability of the molecule prior the
carbonization process and avoid fusion of the bers. Figure 6
shows XRD patterns of empty sample holder, SKL-F
4
powder,
carbonized ber mat, and grinded carbonized ber mat. The top
right hand side of Fig. 6 shows the SEM image of carbonized ber
mat, a schematic of carbonized ber structure, and a schematic of
sample preparation method. For ber mat sample, we used a simi-
lar method to XRD method for thin lm characterization. For ana-
lyzing thin lms with XRD, smaller slits in the receiving detector
should be applied. However, our results showed using smaller slit
to increase the resolution of the recording peak was not effective
for the CF mat sample, possibly due to the nano-sized/amorphous
nature of the CF structure and broadness of the peak(s). Therefore,
the only effective parameter was decreasing the scanning rate
Table 1 Location of the maximum peak for different Kraft lignin
samples in XRD patterns, peak tting method, and mean size of
the ordered domain
Sample
name
Peak fitting
method 2h
Mean size of the
ordered domain (nm)
HKL Lorentzian 21.25 0.75
HKL-F
2
Lorentzian 21.22 0.73
HKL-F
4
Lorentzian 20.99 0.63
HPL Lorentzian 21.35 0.69
SKL Gaussian 19.42 0.67
SKL-F
2
Gaussian 19.48 0.68
SKL-F
4
Gaussian 19.14 0.71
Fig. 3 Carbon and sulfur content of the lignin powder based
on EDS analysis (error bars: standard deviation, n>6)
Fig. 4 SEM images of the SKL-F
4
nanobers: (a) as-spun, (b) thermostabilized, and (c) car-
bonized sample. Scale bar is 10lm, d is the average diameter of the bers.
Fig. 5 TGA analysis of the SKL-F
4
(lled line: in air, dashed
line: in nitrogen)
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(increasing the data collection time). The graphite peak for (101)
plane (marked with * in Fig. 6(d) pattern) was not detected for
ber mat sample. However, the peak for (101) plane is a distinc-
tive characteristic of graphite formation and was available in the
grinded CF mat XRD pattern. The EDS analysis showed that
although the sulfur content of the as spun ber mat was reduced
signicantly during carbonization process, but still some sulfur is
available in the CF structure after carbonizing at 1000

C. EDS
analysis of the PAN based CFs do not show the presence of any
sulfur in their structure [32,33]. However, Hwang et al. manually
added elemental sulfur to the PAN based nanobers and suggested
dehydrogenation process during reaction of PAN with sulfur
facilitates intermolecular cross-linkage and therefore resulted in
higher degree of graphitization [34]. In addition, they concluded
that the sulfurization reaction affects conguration of the turbos-
tratic carbon and increases efciency of pp stacking [34]. Kraft
lignin precursors have remarkably higher oxidized molecules than
PAN [2] and they contain sulfate groups in their structure.
Conclusion
In summary, analyzing different Kraft lignin samples, HKL
(unfractionated hardwood Kraft lignin) and SKL-F
4
(fraction 4 of
SKL) had the highest size of ordered domain according to XRD
analysis. SKL-F
4
also showed highest hydroxyl content according
to FTIR analysis. Due to the challenges in electrospinning of
unfractionated HKL sample, we chose SKL-F
4
for electrospin-
ning. As-spun bers from SKL-F
4
precursor were thermostabi-
lized and carbonized to produce CFs. XRD analysis of the carbon
nanobers indicated that the graphite peak for (101) plane was
available in the grinded sample. According to literature, for PAN
bers sulfur facilitates graphite formation. SKL-F
4
showed high-
est sulfur content among SKL samples. Our proposed hypothesis
based on the presented results is that the available sulfate groups
in Kraft lignins might facilitate graphite formation in carbon
nanober production process. Further investigations are required
to conrm such hypothesis.
Acknowledgment
The authors acknowledge the nancial support from Genome
British Columbia (Genome BC) and Genome Canada.
Nomenclature
CF carbon ber
DMF dimethylformamide
FTIR Fourier transform infrared
HKL hardwood Kraft lignin
PAN polyacrylonitrile
PEO poly ethylene oxide
SKL softwood Kraft lignin
SKL-F
4
fraction 4 of SKL
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