Dataset of nanocrystalline cellulose production and the effects of solvent and thermal

performance.

A. Macías-Almazán1, J. A. Lois-Correa1, M. A. Domínguez-Crespo2*, A. B. López-Oyama3,

A. M. Torres-Huerta2, S. B. Brachetti-Sibaja4, A. E. Rodríguez-Salazar5.
1
Instituto Politécnico Nacional, Centro de Investigación en Ciencia Aplicada y Tecnología Avanzada CICATA, Unidad Altamira, Carretera
Tampico-Puerto Industrial, Km 14.5, Altamira, Tamaulipas, CP 89600, MÉXICO.
2
Instituto Politécnico Nacional UPII Hidalgo, Ciudad del Conocimiento y la Cultura, Carretera Pachuca - Actopan Kilómetro 1+500, San
Agustín Tlaxiaca, C.P. 42162, Hgo. México.
3
CONACYT – CICATA- Altamira. Carretera Tampico-Puerto Industrial Altamira. C. P. 89600. Altamira, Tamps. México.
4
TecNM, Instituto Tecnológico de Cd. Madero. Ave. Primero de Mayo s/n Col. Los Mangos Cd. Madero Tamps. C.P. 89440.
5
Instituto Politécnico Nacional, Centro de Investigación en Ciencia Aplicada y Tecnología Avanzada Unidad-Querétaro, Cerro Blanco No. 141
Col. Colinas del Cimatario, C.P. 76090. Querétaro, Querétaro. México.

Corresponding author: adcrespo2000@yahoo.com.mx

Abstract
The data shown in this article are related to the article in Carbohydrate Polymers entitled “Proton
Conductivity of Nanocellulose films Derived from Agroindustrial Wastes Sugarcane Bagasse
and Pinewood Sawdust” [1]. The data includes Fourier transform infrared (FT-IR) graphs, X-ray
diffraction (XRD) patterns, evidences of photographies and SEM and TEM images as well as
their SAED patterns of the CNCs obtained from CC, PSW and SCB after treating with either 5
wt.% or 10 wt.% followed by an acid treatment with 45 wt.% of H 2SO4 at different temperatures.
Also, it is included the data obtained from the computational methods generated in GLYCAM
carbohydrate builder based on the coordinates for alpha and beta cellulose by considering a
microfibril of 5, 10, 20 and 50 glucosyl residues (degree of polymerization (DP). This work also
contains the characterization data of the samples from nanoindentation technique. To date, all
data have not been previously published and are available to enable a better understanding of the
CNCs preparation through different solvent and temperatures of processing.
Keywords: Agroindustrial Wastes; Sugarcane Bagasse; Pinewood Sawdust; Nanocellulose; PEMFCs.

Specifications Table
Subject area
More specific subject area
Type of data
How data was acquired
Data format
Experimental factors
Experimental features
Data source location
Materials science
Nanotechnology
Tables, Figures, Scheme and Micrographs, Images
Samples were prepared as described in [1]. The characterization was realized by
X-ray diffraction (XRD, Brucker D8 Advanced), FTIR (Perkin Elmer Spectrun
One FTIR spectrometer), Scanning Electron Microscopy (JEOL JSM-6701F
microscope), Transmission electron microscopy (JEOL JEM-2000 FX). MD
simulations were produced with Ambertools suite. The mechanical properties
was carried out on an Anton Paar Nanoindentation Tester NHT3.
Raw, filtered, fitted curves and analyzed data.
The data were realized on the isolation of cellulose nanocrystals from two-
agroindustrial wastes sugarcane bagasse and pinewood sawdust powders.
The relationship between the structure of cellulose and the electric performance
depending on the source and synthesis parameters.
SEM and TEM images were taken at ESIQIE of the Instituto Politécnico
Nacional, C.P. 07738 Ciudad de México, CDMX, México.
FT-IR technique, mechanical properties and XRD patterns were collected at
Centro de investigación en Ciencia Aplicada y Tecnología Avanzada del Instituto
Politécnico Nacional, C.P. 89600 Altamira, Tamaulipas, México.
 Data accessibility
Related research article
All data are available with this article
A. Macías-Almazán, J. A. Lois-Correa, M. A. Domínguez-Crespo, A. B. López-
Oyama, A. M. Torres-Huerta, S. B. Brachetti-Sibaja, A. E. Rodríguez-Salazar.
Proton Conductivity of Nanocellulose films Derived from Agroindustrial Wastes
Sugarcane Bagasse and Pinewood Sawdust

Value of the Data

______________________________________________________________________________
· The data are useful since show the importance of solvent effects to produce nanocellulose
membranes from agroindustrial waste materials.
· The agroindustrial sector can be benefited to process its by-products into products of high
added value to be applied in the PEMFC production.
· The additional value of these data is that the researchers can understand and exchange the
behavior of the donor-acceptor of CNCs in the different solvent and thermal effects.
_____________________________________________________________________________________

1. Data

In the present article, we report the data related to the nanocellulose production from agroindustrial waste
materials. The dataset includes three FT-IR spectra that were plotted from the 950 to 850 cm -1 in the
transmittance % corresponding to different treatments of CNC, SCB and PWS. In each of these figures,
the spectrum of samples after treating them with 5 wt.% of NaOH followed of the acid hydrolysis with
H2SO4 at 45 wt.% at the temperature of 60 °C (Figure a), 75 °C (Figure b) and 90 °C (Figure 1c) are
included.
Figure 2 depicts the XRD patterns that include the results of the raw SCB (Figure 2a), SCB cellulose
obtained with 5 wt.% (Figure 2b) and 10 wt.% (Figure 2c) of NaOH followed of the acid hydrolysis with
45 wt.% of H2SO4, respectively, and the control cellulose (Figure 2d). The XRD patterns are displayed in
the 10-40 2θ (°) range on the x-axis with arbitrary units on the y-axis. Also, the photographies recording
the isolated CNCs from PWS, SCB and CC at each experimental condition can be observed in Figure 3;
these photographs consist of vials with the different samples treated with either 5 or 10 wt.% of NaOH,
with 45wt.% of H2SO4 at 60, 75 and 90 °C. In there, the appearance of the samples incorporated with
water can be distinguished.
Figure 4 and 5 correspond to the TEM images with their corresponding selected area electron diffraction
(SAED) patterns in a 100 nm in scale for CC (60 °C and 75 °C), SCB (75 °C) and PWS (75 °C) in a 100
nm scale. Similarly, the SEM images are presented in Figure 6 and 7.
, The flowchart of the MD production from initial coordinates and thermal effects to obtain final
trajectories is shown in Fig. 8. H-bonds of donor-acceptor glucosyl residues at 333 K, 348 K and 363 K
are shown in Fig. 9. The root mean square deviation (RMSD) of the probabilistic structure of CNC by
using 5, 10, 20 and 50 glucosyl residues is shown in Fig. 10.
The mechanical properties were carried out on an Anton Paar Nanoindentation Tester NHT 3. A Poisson’s
ratios of 0.38 [2], was used for the evaluation, each sample was measured 5 times on different points with
a loading and unloading rate of 80 mN/min with a max load of 40 mN supported for 10 seconds and then
unloaded. The acquisition rate used was 10 Hz, the mechanical properties were calculated by using the
Oliver & Pharr method, see Fig. 11.
 2. Experimental design, materials, and methods

2.1. Sample characterization

The main information on the extraction and experimental equipment used to obtain the nanocellulose
samples from CN, PWS and SBC is presented in: A. Macías-Almazán, J. A. Lois-Correa, M. A.
Domínguez-Crespo, A. B. López-Oyama, A. M. Torres-Huerta, S. B. Brachetti-Sibaja, A. E. Rodríguez-
Salazar. Nanocellulose films from agroindustrial wastes Sugarcane Bagasse and Pinewood Sawdust as an
alternative in proton electrolyte membranes submitted to the Carbohydrate Polymers.
The FT-IR spectra of CNCs obtained from CC, PSW and CSC were acquired in a spectrum one (Perkin
Elmer) spectrometer in transmittance mode. Samples were scanned 20 times at the maximum resolution
(4.0 cm-1) in the 4000-650 cm−1. The spectra were graphed in the 950-850 cm -1 region.
The structure of the samples was determined by X-ray diffraction (XRD) in film shape with a Bruker D8
Advance diffractometer equipped with a Lynxeye detector and Cu Kα radiation (λ = 1.5405 Å) at 35 kV
and 25 mA. Data were collected at room temperature in the 2θ range of 5–55°, step size of 0.02 and step
time of 0.6 s. Data were plotted and analyzed from 10 to 40° (2θ).
The TEM images and SAED patterns were taken in a JEOL JEM-2000 FX at 200 kV and magnifications
of X25K, X50K, and X120K.
SEM images were taken in a JEOL equipment (JSM-6701F model) equipped with a cold cathode field
emission gun based on Tungsten (W) at high vacuum by using secondary electrons. Samples were coated
with an Au–Pd thin film on a Quorum Q150T ES sputter coater system.
It was employed a simulation protocol for MD simulations and measurements schemes for pertinent order
parameters of cellulose. All primary structures were produced with the GLYCAM carbohydrate builder
prior amber minimization. The system setup and simulation analysis employed the GLYCAM_06j-1 force
field. The Hbond analysis was performed by reading the trajectories and searching for Hbonds
donors/acceptors in specific regions for alpha and beta 1,4-cellulose at 60, 75 and 90 °C for 5, 10, 20 and
50 monomers, respectively. All MD calculations were performed by using the sander module in the
Ambertools program suite.

The samples for the mechanical evaluation were prepared using a solution containing CNC for each one
of the experiments, 1 mL of liquid sample was poured on one edge of a previously cleaned glass substrate
with dimensions of 25.4 x 38.1 mm and then distributing the liquid all over the substrate with an
Elcometer 3580 film applicator for a uniform and reproducible coating, the samples were then oven-dried
at 50 °C for 8 hours before characterization.

The analysis was carried out on an Anton Paar Nanoindentation Tester NHT 3. A Poisson’s ratio of 0.38
[2] was used for the evaluation, each sample was measured 5 times on different points with a loading and
unloading rate of 80 mN/min and a maximum load of 40 mN which was maintained during 10 s and then
unloaded. The acquisition rate used was 10 Hz, the mechanical properties were calculated by using the
Oliver & Pharr method. The data acquired were used to graph the elastic modulus and hardness.
 5 wt. % NaOH
(a) 5 wt. % NaOH (b) (c) 5 wt. % NaOH
45 wt. % H2SO4
PWS
45 wt. % H2SO4
PWS 45 wt. % H2SO4
PWS

3660
3658
O6-H ... O6
3670

3046

3040
3040

3207

3222
3548
3227

3550

3384
3548

3400
3409
C-H
C-H
stretching
stretching
2nd Derivative

2nd Derivative

2nd Derivative
O6-H ... O6
Free OH
SCB SCB SCB
3659

3664
stretching

3667
3176

3050
3051

3219
3537
3526

3422

3262

3533

3412
C-H
3416

stretching
O2-H ... O6
CNC CNC O3-H ... O6
CNC

3664
3670

3678
O3-H ... O6
3066

3065

3066
3371
3497

3518
OH
3342

3508

3347
stretching O3-H ... O5
O3-H ... O5
O3-H ... O6 T = 60°C T = 75°C T = 90°C
3800 3600 3400 3200 3000 3800 3600 3400 3200 3000 3800 3600 3400 3200 3000
-1 -1
Wavenumber (cm ) Wavenumber (cm ) Wavenumber (cm-1)
...

(d) 10 wt. % NaOH (e) 10 wt. % NaOH (f) 10 wt. % NaOH

45 wt. % H2SO4 45 wt. % H2SO4 PWS 45 wt. % H2SO4
PWS
3659

3659
3664

PWS

3050
O3-H ... O5 3213 O3-H ... O5
3066

3042
3219
3197

OH OH

3545
OH
stretching stretching C-H
3540

stretching
3382

C-H stretching

3402
3422

C-H
stretching
O3-H ... O6 stretching
O3-H ... O6 O3-H ... O5

O3-H ... O6

SCB SCB
3662

3654
SCB
3660

3061
O3-H ... O5
3047

3035

O3-H ... O5

3217
OH OH
3210

3541
3411
3535

3263

stretching
3387

OH stretching
3536

C-H stretching C-H C-H

3383
stretching
O3-H ... O5 stretching stretching
O3-H ... O6 O3-H ... O6 T = 90 °C
T = 60 °C O3-H ... O6 T = 75 °C

3800 3600 3400 3200 3000 3800 3600 3400 3200 3000 3800 3600 3400 3200 3000
-1
Wavenumber (cm-1) Wavenumber (cm-1) Wavenumber (cm )
Fig. 1. 2nd derivative of FTIR region 3800-3000 cm-1 of H-bonds that compose the -OH stretching
band of the nanocellulose by varying the solvent medium and temperature.
 Amorphous band
PWS PWS
PWS

Amorphous band

Amorphous
Transmittance (%)

Transmittance (%)
Transmittance (%)

SCB SCB
SCB

band
CNC CNC CNC

5 wt.% NaOH, 45 wt.% H SO 5 wt.% NaOH, 45 wt.% H SO 5 wt.% NaOH, 45 wt.% H SO

2 4 2 4
(a)
2 4
T= 60°C (b) T= 75°C (c) T= 90°C
950 900 850 950 900 850 950 900 850
-1 -1 -1
Wavenumber (cm ) Wavenumber (cm ) Wavenumber (cm )

Fig. 1. FTIR spectra of crystalline nanocellulose from CNC, SCB and PWS produced with 5 wt.% NaOH,
45 wt.% H2SO4 at (a) 60 °C, (b) 75 °C and (c) 90 °C.

(d)
(100) (200) (004)
Intensity (a.u.)

(c)

(b)

(a)
10 15 20 25 30 35 40
2 (Degrees)
Fig. 2. XRD patterns of (a) raw SCB, (b) SCB cellulose produced with 5 wt.% NaOH, 45 wt.% H 2SO4,
(c) SCB cellulose produced with 10 wt.% NaOH, 45 wt.% H 2SO4 and (d) control cellulose.
 40 40

35
(a) CC (45 wt.% H2SO4, 75 °C)
35
(b) SCB(5 wt.% NaOH, 45 wt.% H SO , 75 °C) 0.5
2 4

DLS intensity (%)

DLS intensity (%)
0.5

0.4
30 0.4 30

Absorbance
0.3

Absorbance
0.3 3 4
25 25 2
3 0.2
0.2 1
20 2 20 0.1
0.1
15 1 15 0.0
0.0 3800 3600 3400 3200 3000
-1
3800 3600 3400 3200 3000 Wavenumber (cm )
10 Wavenumber (cm )
-1 10

5 5

0 0
16 20 24 28 32 36 40 30 40 50 60 70
Diameter (nm) Diameter (nm)
40 40
(c) SCB(10 wt.% NaOH, 45 wt.% H SO , 75 °C) 2 4 (d) PWS ( 5 wt.% NaOH, 45 wt.% H2SO4, 75 °C)
DLS intensity (%)

DLS intensity (%)

35 0.5 35
0.40
0.4 0.35
30 30
Absorbance

0.30
3

Absorbance
0.3 3 2
0.25
25 2
25
0.2 4 0.20

20 1 20 0.15
0.1 0.10 4
1
15 0.0 15 0.05
3800 3600 3400 3200 3000 0.00
-1 3800 3600 3400 3200 3000
Wavenumber (cm )
10 10 Wavenumber (cm )
-1

5 5

0 0
200 250 300 350 400 450 500 20 30 40 50 60 70 80

Diameter (nm) Diameter (nm)

40 40
(e) PWS ( 10 wt.% NaOH, 45 wt.% H SO , 60 °C) 2 4 (f) PWS ( 10 wt.% NaOH, 45 wt.% H SO , 75 °C)
DLS intensity (%)

2 4
DLS intensity (%)

35 35 1.0

0.15 0.8
30 30 2

Absorbance
Absorbance

0.6
0.10
25 25
1
0.4
3
20 0.05 2 20
0.2
1 4 3
15 0.00 15 0.0
3800 3600 3400 3200 3000 3800 3600 3400 3200 3000
-1 -1
10 Wavenumber (cm ) 10 Wavenumber (cm )

5 5

0 0
20 24 28 32 36 40 44 48 40 50 60 70 80 90 100 110 120

Diameter (nm) Diameter (nm)

40
(g) PWS ( 10 wt.% NaOH, 45 wt.% H SO , 90 °C) 2 4
DLS intensity (%)

0.7
35
0.6 3

30 0.5
Absorbance

0.4 2
25 0.3

0.2 4
1
20 0.1

0.0
15 3800 3600 3400 3200 3000
-1
Wavenumber (cm )
10

0
30 40 50 60 70 80 90
Diameter (nm)
Figure 3. Particle size distribution histograms of crystalline nanocellulose obtained from DLS
measurements. The inset figures shown deconvolution of FT-IR spectra in the 3800-3000 cm -1
region for all the samples to observe inner components of hydrogen-bonded OH stretching.
 Raw materials

5000
C ellu lose I  14000 Cellulose I
C ellu lose I  Cellulose I

(200)
4000 SCB 12000 PWSD

(200)
In te nsity (a.u.)
In te n sity (a .u .)

am orphous 10000
3000 amorphous
cellulose cellulose
8000
(-110)
(110)

(-110)
(110)
2000 6000

(-110)
(-110)

4000
1000
2000

0 0
12 14 16 18 20 22 24 26 12 14 16 18 20 22 24
2 (de grees) 2 (deg re es)

CC (45 wt.% H2SO4)

Cellulo se I Cellu lose I 
(200)

(200)
1200 350

T= 60 °C 300 T= 90 °C
1000

Inten sity (a .u .)
In te n sity (a .u .)

amo rphous
ce llulose 250 am orph ous
(110)

800

(110)
cellulos e
200
(-110)

(-110)
600
150

400 100

200 50

0 0
14 16 18 20 22 24
12 14 16 18 20 22 24 26
2 (d egre es)
2 (degrees)

SCB (5 wt.% NaOH, 45 wt.% H2SO4)

700
1200 C ellulose I Cellulose I 
C ellulose I 600 Cellulose I 
(200)

1000 T= 60 °C T= 90 °C
In te n sity (a .u .)
In te n s ity (a .u .)

500

(200)
800
400 am orphous
(110)

(110)
a morph ou s cellulose
(-110)

600

(-110)
cellulos e
(-110)

(-110)
300
400
200
200
100

0 0
12 14 16 18 20 22 24 26
12 14 16 18 20 22 24 26
2 (deg rees) 2 (d eg ree s)

SCB (10 wt.% NaOH, 45 wt.% H2SO4)

1600 Cellulose I C ellulose I
(200)

800 C ellulose I
Cellulose I
1400
Cellulose II C ellulose II
In te n sity (a .u .)

1200 T= 60 °C T= 90 °C
Inten sity (a .u .)
(200)

600 am o rph ous

1000 am o rpho us cellulos e
(-110)

ce llu lo se
(110)

800 400
(110)
(-110)

(-110)
(-110)

600
(-110)

(-110)

400 200
200

0 0
10 12 14 16 18 20 22 24 26 10 12 14 16 18 20 22 24 26
2 (deg rees) 2 (deg rees)

PWSD (5 wt.% NaOH, 45 wt.% H2SO4)

1200
Cellulos e I  Cellulose I 
(200)
(200)

1200
Cellulos e I  Cellulose I 
Cellulos e II 1000
Cellulose II
In te n sity (a .u .)

1000
In te n sity (a .u .)

T= 60 °C T= 90 °C
800
800
am orphou s
(110)

cellulo se 600 am orphous

600
cellulose
(110)
(-110)
(110)

400
(-110)

400
(-110)
(-110)

(110)

(-110)
(-110)

200 200

0
0
10 12 14 16 18 20 22 24 26
10 12 14 16 18 20 22 24 26
2 (degre es) 2 (degrees)

PWSD (10 wt.% NaOH, 45 wt.% H2SO4)

1000
(2 0 0 )

C ellul ose I
500 C ellu lose I 
(200)

C ellul ose I
C ellu lose I 
In te n s ity (a .u .)

C ellul ose II
400 T= 60 °C 800 C ellu lose II
In te n s ity (a .u .)

T= 90 °C
300 a m orp hou s
600 am orphou s
c ellu lo se
(110)

cellulo se
( -1 1 0 )

(-1 1 0 )

200
(1 1 0 )

(-1 1 0 )

400
(110)
(-110)

100
(110)
(-110)

(-110)

200
0
12 14 16 18 20 22 24
0
10 12 14 16 18 20 22 24 26
2 (deg rees )
Figure 4. Separation of amorphous and crystalline phases in dependence of synthesis parameters
using the Shirley background substation with a Gaussian- Lorentzian profile.

5000
Cellulose Ia 14000 Cellulose I

(200)
Cellulose Ib Cellulose I

(200)
12000

Intensity (a.u.)
4000
SCB PWSD
Intensity (a.u.)

amorphous 10000 amorphous

3000 cellulose cellulose
8000
(-110)

(-110)
(110)
(110)

2000 6000

(-110)
(-110)
4000
1000
2000

0 0
12 14 16 18 20 22 24 26 12 14 16 18 20 22 24
2(degrees) 2(degrees)
Cellulose I
1200 350 Cellulose I
T= 60 °C
T= 90 °C
(200)

amorphous

(200)
1000 300
Intensity (a.u.)
cellulose
Intensity (a.u.)

(110)

800 250 amorphous

(-110)

(110)
cellulose
200

(-110)
600
150
400
100
200
50
0
12 14 16 18 20 22 24 26 0
14 16 18 20 22 24
2(degrees) 2(degrees)
700
Cellulose I
1200 Cellulose I
Cellulose I
(200)

T= 60 °C
600 Cellulose I
1000 T= 90 °C
(200)
500
Intensity (a.u.)
Intensity (a.u.)

amorphous
800
cellulose amorphous
(-110)
(-110)

(110)

400
(110)

600
cellulose
(-110)
(-110)

300

400 200

200 100

0 0
12 14 16 18 20 22 24 26 12 14 16 18 20 22 24 26
2(degrees) 2(degrees)

1600 Cellulose I Cellulose I

800
1400
Cellulose I Cellulose I
Cellulose II Cellulose II
(200)
Intensity (a.u.)

(200)

1200 T= 60 °C amorphous
amorphous 600 T= 90 °C
Intensity (a.u.)

1000 cellulose
cellulose
(110)
(-110)

(-110)

(110)

800
(-110)

400
(-110)
(-110)

(-110)

600

400
200
200

0 0
10 12 14 16 18 20 22 24 26
10 12 14 16 18 20 22 24 26
2(degrees) 2(degrees)
 1200
Cellulose I
1200 Cellulose I
Cellulose I 1000 Cellulose I

(200)
(200)

Intensity (a.u.)
1000 Cellulose II
T= 60 °C amorphous Cellulose II
Intensity (a.u.)

800
800 cellulose T= 90 °C amorphous

(110)
600 cellulose
600

(110)
(-110)
(110)
(-110)

(-110)

(-110)
(110)
400 400

(-110)
(-110)
200 200

0 0
10 12 14 16 18 20 22 24 26 10 12 14 16 18 20 22 24 26
2(degrees) 2(degrees)
1000
500
Cellulose I Cellulose I
Cellulose I Cellulose I

(200)
(200) 800
Intensity (a.u.)

400 Cellulose II Cellulose II

amorphous T= 90 °C amorphous

Intensity (a.u.)
T= 60 °C 600
300 cellulose cellulose
(110)

(110)
(-110)

(-110)
(110)

400

(-110)
(-110)

(110)
(-110)
200

(-110)
100 200

0 0
12 14 16 18 20 22 24 10 12 14 16 18 20 22 24 26
2(degrees) 2(degrees)
Fig. 3. Photographic recording of the nanocrystalline cellulose produced from agroindustrial
wastes with 5 and 10 wt.%. NaOH, 45 wt.%. H2SO4 under different temperatures.
 (a) (b)

100 nm

(c) (d)

100 nm

(e) (f)

100 nm

Fig. 4. TEM images with its corresponding SAED patterns and of isolated nanocrystalline
cellulose from CC and SCB at different temperatures where it is seen the nanocrystalline and
microcrystalline regions. TEM micrographs are shown for CC at (a-d) 75 °C and SCB at (e-f) 75
°C. All the samples were prepared with 5 wt.% NaOH followed of an acid hydrolysis with 45 wt.
% H2SO4.
 (a) (b)

50 nm

(c) (d)

100 nm

(e) (f)

100 nm

Fig. 5. TEM images with its corresponding SAED patterns of isolated nanocrystalline cellulose
from PWS and CC at different temperatures where it is seen the nanocrystalline and
microcrystalline regions. TEM micrographs are shown for PWS at (a-b) 75 °C and CC at (c-f) 60
°C. All the samples were prepared with 5 wt.% NaOH followed of an acid hydrolysis with 45 wt.
% H2SO4.
(a) (b) (c)

100 nm 100 nm 100 nm

(d) (e) (f)

1 µm 1 µm 100 nm

(g) (h) (i)

1 µm 1 µm 1 µm

Fig. 6. SEM micrographs of isolated nanocrystalline cellulose from CC at different temperatures

where it is seen the nanocrystalline and microcrystalline regions. SEM images corresponds to CC
at (a-d) 60 °C, (e-f) 75 °C, (g-i) 90 °C. All the samples were prepared with 5 wt.%
 1 µm 100 nm 100 nm

100 nm 100 nm 1 µm

1 µm 1 µm 1 µm

Fig. 7. SEM micrographs of isolated nanocrystalline cellulose from PWS and SCB at different
temperatures where it is seen the nanocrystalline and microcrystalline regions. SEM images
corresponds to PWS at (a-c) 75 °C and SCB at (d-f) 60 °C, (g-i) 75 °C. All the samples were
prepared with 5 wt.% NaOH followed of an acid hydrolysis with 45 wt.% H2SO4.
Fig. 8. Data analysis flowchart for the initial coordinates to analyze the data for DM by using
Ambertools.
Fig. 9. Donor/acceptor H-bonds for the glucosyl residues analyzed.
Fig. 10. RMSD of the probabilistic structure of CNC using 5, 10, 20 and 50 glucosyl residues of
alpha and beta 1,4 at 333, 348 and 363 K.
 60000
CC SCB PWS (a)
Elastic Modulus (MPa) 50000

40000

30000

20000

Nafion
10000

0
60 75 90 60 75 90 60 75 90 60 75 90 60 75 90
5 wt.% 10 wt.% 5 wt.% 10 wt.%
NaOH NaOH

1600
CC SCB PWS (b)
1400

1200
Hardness (MPa)

1000

800

600

400
Nafion

200

0
60 75 90 60 75 90 60 75 90 60 75 90 60 75 90
5 wt% 10 wt.% 5 wt% 10 wt.%
NaOH NaOH

Fig. 11. Result of mechanical properties to different parameter such as temperature of synthesis
at 60, 75 and 90 °C, acid hydrolysis at 45 wt.% H 2SO4 and 5, 10 wt.% of NaOH (a) elastic
modulus and (b) hardness at different synthesis conditions.
Acknowledgments
A. Macías-Almazán is grateful for his postgraduate fellowship to CONACYT, COFAA and SIP-

IPN. The authors are also grateful for the financial support provided by Instituto Politécnico

Nacional through the SIP 20196650, 20196718 and 20196670, and COFAA; CONACYT

through the CB-2015-252181, PC 1905 and SNI-CONACYT. The authors thank to Zucarmex

S.A. of C.V. and the Sugar Mill in El Higo, Veracruz, for the raw sugarcane bagasse.

Competing Interests
The authors declare that they have no known competing financial interests or personal
relationships that could have appeared to influence the work reported in this paper.
References
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Huerta, S. B. Brachetti-Sibaja, A. E. Rodríguez-Salazar. Proton Conductivity of Nanocellulose films
Derived from Agroindustrial Wastes Sugarcane Bagasse and Pinewood Sawdust.

[2] Nakamura, K., Wada, M., Kuga, S., Okano, T. (2004). Poisson’s Ratio of Cellulose Iα and cellulose
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https://doi.org/10.1002/polb.10771