PROPERTIES OF BAMBOO ON FREEZE-THAW TREATMENT

AND OIL HEAT TREATMENT

SEMINAR REPORT

Submitted in partial fulfillment of the requirements for the award of the Degree of Bachelor of
Technology in Civil Engineering by APJ Abdul Kalam Technological University

by
AMMU RAJ
(TRV20CE059)

DEPARTMENT OF CIVIL ENGINEERING

GOVERNMENT ENGINEERING COLLEGE BARTONHILL
THIRUVANANTHAPURAM- 35
NOVEMBER 2023

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 DECLARATION

I, the undersigned declare that the seminar report “Properties of bamboo on freeze-thaw
treatment and oil heat treatment”, submitted for partial fulfillment of the requirement for the
award of the degree Bachelor of Technology of the APJ Abdul Kalam Technological University,
Kerala, is a bonafide work done by me under supervision of Dr. Girija K, Professor, Department
of Civil Engineering, Government Engineering College Barton hill. This submission represents
my ideas in my own words where pictures or words of others have been included. I have
adequately and accurately cited and referenced the original sources. I also declare that I have
adhered to ethics, academic honesty, and integrity and have not misrepresented or fabricated any
data, idea fact, or source in my submission. I understand that any violation of the above will be a
cause for disciplinary action by the institute and/or the University and can also evoke penal
action from the sources that have thus not been adequately cited or from whom proper
permission has not been obtained. This report has not previously formed the basis for the award
of any degree, diploma, or similar title of any other University.

Place: Thiruvananthapuram
Date: 07-11-2023
AMMU RAJ

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 DEPARTMENT OF CIVIL ENGINEERING GOVERNMENT
ENGINEERING COLLEGE, BARTON HILL

CERTIFICATE
This is to certify that the Seminar Report titled “PROPERTIES OF BAMBOO ON
FREEZE-THAW TREATMENT AND OIL HEAT TREATMENT” submitted by
AMMU RAJ to the Department of Civil Engineering, Government Engineering College Barton
Hill, Thiruvananthapuram as partial fulfillment for the award of degree B.Tech in Civil
Engineering is a bonafide work undertaken under my supervision.
This report in any form has not been submitted to any other university or institute for any
purpose

DR. GIRIJA K DR. V THULASEEDHARAN

Professor Head of the Department
Dept. of Civil Engineering Dept. of Civil Engineering.
GEC Barton Hil GEC Barton Hill
(Guide)

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 ACKNOWLEDGEMENT

First of all, I would like to express my gratitude to the Almighty for the invisible guidance. A
special gratitude to my project guide Dr. Girija K (Professor, Dept. of Civil Engineering, Govt
Engineering College Barton Hill, Trivandrum), whose contribution in stimulating suggestions
and encouragement helped me to coordinate my report. I would like to thank
Dr. V Thulaseedharan (Professor and Head of Dept. Civil Engineering, Govt. Engineering
College Barton Hill, Trivandrum) for his guidance and support.
I am very thankful to my staff advisors Dr. Girija K ( Professor, Dept. Civil Engineering, Govt.
Engineering College, Trivandrum) and Prof. Karthika Priyadarshiny (Assistant Professor,
Dept. Civil Engineering, Govt. Engineering College, Barton Hill, Trivandrum) for their
guidance. Last but not least, I would like to express my deepest appreciation to all those who
provided me with the possibility to complete this report.

AMMU RAJ

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 ABSTRACT

With the rapid development of the country, economic growth, and standard of living conditions,
the demand for wood in the construction industry has increased. It is necessary to use renewable
materials instead of existing non-renewable materials in the construction field to reduce the
effects of greenhouse gases and global warming. One of the green bioresources, bamboo with
high mechanical properties has been attracting growing attention nowadays.

According to the references[1,2], researchers studied the various effects of oil heat treatments
and modifications on the properties of bamboo including chemical compositions, physical and
mechanical properties, decay resistance, anti-mildew properties, surface-wettability and; the
mechanical properties of bamboo based on the effect of freeze-thaw treatment with different
initial moisture conditions respectively.

Compared with wood, bamboo has been widely used in construction as one of the important
resources in the biomass industry for its fast growth, easy propagation, and short renovation.
However, mildew and decay of bamboo restrict its application in specific environments. This
seminar is based on references[1,2], in which the authors have paid attention to the modifications
of bamboo and various treatment methods that have been applied to bamboo to improve
anti-mildew properties and pest-resisting abilities, etc.
Keywords: Freeze-thaw treatment, oil heat treatment, bamboo, mechanical properties, decay
resistance, anti-mildew property.

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 CONTENTS

Sl.No Title Page No:

Abstract 5
1 Introduction 9
1.1_ Scope and Objective 9
2 Literature Review 10
3 Methodology 11
3.1_ Freeze-thaw treatment 11
3.2_ Oil heat treatment 13
4 Results and discussions 14
4.1_ Effect on Microstructure 14
4.2_ Effect on cellulose, hemicellulose, and lignin contents 16
4.3_ Effect on surface wettability 17
4.4_ Effect on physical and mechanical properties 18
4.5_ Effect on decay resistance property 20
4.6_ Effect on anti-mildew property 22
5 Conclusion 23
6 References 24

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 LIST OF TABLES

Table No. Title Page No.

Table 1 The parameters of freeze-thaw treatment 12

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 LIST OF FIGURES

Figure No Title Page No

1 Sample preparation from different parts of bamboo 11

2 SEM image of untreated sample 14
3 SEM image of the treated sample 15
4 Graph showing percentage loss of cellulose, hemicellulose 16
and lignin
5 Graph showing the contact angle of treated and untreated 17
sample
6 Graph showing compressive strength parallel to the grain 18
7 Graph showing bending strength and bending MOE 19
8 Graph showing percentage loss of weight of the sample 20
9 Graph showing percentage loss of starch 21
10 Graph showing the infection ratio treated and untreated sample 22

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 1. INTRODUCTION
The growing demand for wood in various industries due to improved living standards and
economic growth leads to an imbalance in wood supply. Also due to atmospheric conditions like
global warming, carbon emission, greenhouse gases, etc., the necessity of renewable materials in
the construction field instead of existing non-renewable materials increases. Therefore
researchers focus on the increasing interest in biomass materials, specifically bamboo, due to its
high mechanical properties and effectiveness in reducing greenhouse gases. As a result, bamboo
has become a crucial substitute for wood globally.
Bamboo has been used as a building material for a long time. Still, its widespread acceptance has
been limited due to the absence of unified and reliable design standards and the vulnerability of
fungi, pest attacks, and certain environmental factors. To address these issues, various
modification techniques such as γ-irradiation, nanotechnologies, chemical impregnation, and
thermal treatment have been explored. Among them, thermal modification, particularly oil heat
treatment, emerges as an eco-friendly and effective method. The paper focuses on studying the
effects of oil heat treatment on bamboo properties using methyl silicone as the heat medium at
various temperatures for 2 to 6 hours.
The material properties of bamboo mainly consist of vascular bundles and matrix, which are
significantly influenced by moisture and environmental temperature, especially in extremely
colder regions. This research aims to investigate the effects of freeze-thaw treatment on bamboo
with varying initial moisture contents through various testing methods. The study is crucial for
understanding how bamboo behaves under low temperatures and could contribute to its
development and utilization in outdoor applications, especially in extremely cold environments.

1.1 SCOPE AND OBJECTIVE

Research centers on understanding the impact of freeze-thaw treatment and oil heat treatment on
bamboo, specifically exploring how different initial moisture contents influence the materials’
properties and the impact of methyl silicone oil on various properties of bamboo respectively.
The study helps us to enhance the understanding of how the unique structure of bamboo changes
in bamboo’s material properties when exposed to different moisture and temperature conditions.
Overall, the study aims to understand the comprehensive effect of freeze-thaw treatment and oil
heat treatment on bamboo.

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2. LITERATURE REVIEW
The effects of freeze-thaw treatment and oil heat treatment on bamboo, and various changes in
the physical, mechanical, and biological properties with different temperatures and moisture
conditions were studied by the researchers.

Jieyu et al.(2021) studied the effects of freeze-thaw treatment on bamboo with different initial
moisture conditions. For the study, they used three-year-old bamboo Moso bamboo,
(Phyllostachys pubescens). Bamboo culms at a 2-4m height from the base were used for the
experiment. For the analysis, FE-SEM observation, FT-IR, XRD, and thermal conductivity
analysis, parts close to the outer and inner layers of bamboo were separated due to its gradient
structure. The unique gradient structure is formed due to the distribution of vascular bundles
decreasing from the outer to the inner layer of bamboo. In this investigation, bamboo with
different moisture conditions was subjected to two freeze-thaw treatments to evaluate the
variations in its mechanical properties by certain analyses. The microstructure, chemical
composition, mechanical properties, and thermal conductivity of bamboo were analyzed by field
emission scanning electron microscopy (FE-SEM), Fourier-transform infrared
spectroscopy(FT-IR), X-ray diffraction(XRD), mechanical testing machine and thermal
conductivity tester.

Xiaomeng et al.(2021) studied the effects of oil heat treatment on the properties of bamboo
including chemical composition, physical and mechanical properties, surface wettability, decay
resistances, and anti-mildew properties. For the study, they used methyl silicone oil as a heat
medium. They selected Moso bamboo, five years old, as a testing specimen.
Oil heat treatment: In this treatment samples were oven-dried at 105 degrees Celsius until weight
consistency was achieved. After this, samples were transferred and immersed in a heated oil bath
at 140, 160, 180, and 200 degrees Celsius for 2, 4, and 6 hours respectively. After the treatment,
samples were cooled and wiped out. For the analysis, oil-heated samples were subjected to
various property tests and evaluated the changes in the various properties in comparison with
untreated samples.

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3. METHODOLOGY

3.1 Freeze-thaw treatment

Moso bamboo of a three-year-old was cut into 20 mm in width, length, and 30mm thickness
respectively. Bamboo was cut into 160mm×10mm in length and width respectively and the
thickness of the sample was the same as that of the bamboo wall. Figure 1 shows the details of
sample preparation from different parts of the bamboo culm.

Fig. 1. Sample preparation from different parts of the bamboo culm.

(SOURCE: The mechanical properties and thermal conductivity of bamboo with freeze-thaw
treatment, (2021))

They divided samples into six groups based on three moisture contents and were treated with two
types of freeze-thaw treatment. Freeze-thaw treatment parameters are given in Table 1.
C0 was the control sample, which means an untreated sample. T and F are referred to as -20◦ 𝐶
and -40◦ 𝐶 respectively. Numbers 1, 2, and 3 were referred to as three different moisture
contents, respectively

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Table 1 The parameters of freeze-thaw treatment

Treatment condition Sample initial Freezing Place at room Heat treatment

state treatment temperature

C0 Air-dried - - -

T-1 Water- saturated

T-2 Air-dried –20◦ 𝐶/24h About 28◦ 𝐶/24h 60◦ 𝐶/24h
T-3 Oven-dried

F-1 Water-saturated
F-2 Air-dried –40◦ 𝐶/24h About 28◦ 𝐶/24h 60◦ 𝐶/24h
F-3 Oven-dried
(SOURCE: The mechanical properties and thermal conductivity of bamboo with freeze-thaw
treatment, (2021))

Analysis of Microstructure and Chemical Composition

The field emission scanning electron microscope (FE-SEM) was used to analyze the outer and
inner layer cross-section of bamboo after freeze-thaw treatment. They tested the two specimens
for each sample. They cut all the samples into a length of 19mm and a width of 19mm for XRD
testing, three replicates were tested for each sample. The crystalline cellulose structure of
untreated and treated samples was measured by XRD.
Analysis of Mechanical Properties and Thermal Conductivity
Five specimens were tested for each sample for the analysis. For this analysis, a bending test was
conducted based on GB/T 15780-1995 and performed by a universal testing machine. The strain
rate was 10 mm/min. The thermal conductivity of bamboo was measured with a thermal
conductivity tester at a test temperature of 25◦ 𝐶. For the thermal conductivity analysis, three
specimens were tested for each sample. The thermal conductivity of the sample was measured
by:
κ = (µ × µ) ÷ ρ𝐶𝑝 – – – – – – – – – – – – – – – – – – – – – – (1)
where κ is thermal conductivity,
µ 𝑖𝑠 𝑡ℎ𝑒𝑟𝑚𝑎𝑙 𝑒𝑓𝑓𝑢𝑠𝑖𝑣𝑖𝑡𝑦,
ρ 𝑖𝑠 𝑑𝑒𝑛𝑠𝑖𝑡𝑦,
𝐶𝑝 𝑖𝑠 𝑡ℎ𝑒 𝑠𝑝𝑒𝑐𝑖𝑓𝑖𝑐 ℎ𝑒𝑎𝑡 𝑐𝑎𝑝𝑎𝑐𝑖𝑡y.

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3.2 Oil heat treatment

Oil heat treatment - Bamboo samples were oven-dried at 105◦C till weight consistency was
achieved. After that, samples were transferred and immersed in a heated oil bath at
140,160,180,200◦C for 2,4, and 6 hours at each defined temperature respectively.
Moso bamboo five years old was used for this treatment. Defect-free samples of 300mm×30mm
×8mm were cut 2m away from the root. Thermally oil-treated samples were divided into 12
treated groups and one group was set as a C0, control ( untreated) sample. All tests were repeated
8 times and the average results were collected and tested.
Scanning Electron Microscopy (SEM), X-ray diffraction (XRD), Major chemical compaction
test, Surface wettability, Physical and chemical property test, Decay resistance test, and
Anti-mildew property tests were used for the analysis of bamboo samples in oil heat treatment.

Scanning Electron Microscopy is used for the analysis of the microstructure of the bamboo
sample and is done by TM3030 (Opton, UK) scanning electron microscopy. The bamboo was cut
off from the middle part, surface was smoothened and dried in an oven at 105◦ C.

X-ray diffraction (XRD) was used for the analysis of crystallinity and lattice spacing of
cellulose of bamboo samples before and after the oil heat treatment. It is a scanning method done
with powder X-ray diffractometer T-6000 (Malvern Panalytical, UK). The scanning angle was 5
to 50 degrees Celsius and the speed was 2 degrees per min.

Major chemical composition test, the contents of three major elements ( cellulose,
hemicellulose, and lignin) were determined by the National Renewable Energy Laboratory.
High-performance liquid chromatography(HPLC) was used for the analysis of sugar content in
the supernatant.

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The surface wettability test is used for analyzing the hydrophobic properties of treated bamboo
samples by liquid droplet method.

Physical and mechanical property test is used for analyzing the compressive parallel to grain
size, bending strength, and modulus of elasticity of the treated sample by DNS50 electronic
universal testing machine.

Decay resistance and anti-mildew test, used for analyzing the decay resistance and anti-mildew
properties of the treated bamboo sample.

4. RESULTS AND DISCUSSIONS

4.1 EFFECT ON MICROSTRUCTURE

Figures 2 and 3 show the SEM images of untreated and treated bamboo samples in cross-section
and longitudinal sections respectively.

Fig. 2. SEM image of untreated sample.

(SOURCE: The effect of oil heat treatment on biological, mechanical, and physical properties of
bamboo, (2021))

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Fig. 3. SEM image of treated sample.
(SOURCE: The effect of oil heat treatment on biological, mechanical, and physical properties of
bamboo, (2021))

In Figure 2, it can be seen that the parenchyma cell wall is smoothened and pits inside the cell
lumen are distributed evenly throughout the cell wall and are circled by a short yellow dashed
line as in Figure 2 f. Pits are the channel through which the exchange of nutrients and moisture
among cells takes place. Starch granules are pointed by yellow arrows in Figure.2.c and f which
are supposed to be nutrients for the growth of molds.
Figure 3, shows the treated bamboo sample with methyl silicone oil at 200◦ C for 2 hours. Cells
are distorted and deformed by yellow dotted lines. Gaps between adjacent cell walls increase and
are pointed by green arrows. The dense structure is destroyed. Moreover, there are no starch
granules inside the parenchyma cells of the treated bamboo sample at 200◦ C for 6 hours. Small

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molecules of oil enter the crystallization area of starch granules, resulting in swelling and
collapse of starch molecules. From the Figure itself, it can be observed that pits are blocked by
the mixture of oils and galvanized starch.

4.2. EFFECT ON CELLULOSE, HEMICELLULOSE, AND LIGNIN

CONTENTS

Figure 4 shows the variation of cellulose, hemicellulose, and lignin of treated and untreated
samples at varied temperatures before and after the treatment.

Fig. 4. The percentage of cellulose, hemicellulose, and lignin of untreated and treated samples at
varied temperatures (140,160,180, and 200◦ C for varied times (2,4, and 6 hrs).
a) Cellulose b) hemicellulose c) lignin.
(SOURCE: The effect of oil heat treatment on biological, mechanical, and physical properties of
bamboo, (2021))

Compared with untreated samples, the contents of cellulose and hemicellulose rate decrease
gradually. However, the content of lignin increases gradually with time. Cellulose and
Hemicellulose content decreased by 36.6% and 37.2% respectively at 180◦ C for 6 hours
compared with the control group. The decline rate increases when compared with the untreated
sample at 200 ◦C for 6 hours. Because cellulose and hemicellulose are polysaccharides and
which has poor thermal stability.
With the decrease of cellulose and hemicellulose, the relative content of lignin increases with
treated temperature and time because of its high thermal stability.

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4.3. EFFECTS ON SURFACE WETTABILITY
The contact angle of untreated and treated samples at varied temperatures for varied times is
shown in Figure 5.

Fig. 5. The contact angle of untreated and treated samples at varied temperatures for varied
times.
(SOURCE: The effect of oil heat treatment on biological, mechanical, and physical properties of
bamboo, (2021))

The contact angle of the untreated outer layer bamboo sample is 58.03 ◦ C and that of the treated
sample is 84.7◦ 𝐶 to 89.3◦C. The contact angle of the treated sample is much higher than that of
the untreated bamboo sample. Because heat medium on the outermost layer improves the
hydrophobicity of the treated sample.
Moreover, the blockage of pits also reduces the entry of the entry of water into the treated sample
to a great extent. Waxes presented in the oil-heated samples behave like a waterproofing
membrane; thus, the hydrophobic character increases and negatively impacts surface wettability.
Surface wettability reduces with an increase in treated temperature.

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4.4 EFFECT ON PHYSICAL AND MECHANICAL PROPERTIES
Compressive strength parallel to the grain size of treated and untreated bamboo samples at
different temperatures and times is shown in Figure 6.

Fig. 6. The compressive strength parallel to the grain of untreated and the treated sample at
varied temperatures for varied times.
(SOURCE: The effect of oil heat treatment on biological, mechanical, and physical properties
of bamboo, (2021))

Compressive strength parallel to the grain of untreated samples is 89.07MPa. With the increase
of temperature, compressive strength parallel to grain first increases then reaches a maximum of
109.52MPa at 160◦ C for 2 hours and then decreases. The maximum value of compressive
parallel to the grain is 18.63% higher than that of the untreated sample. At 200 ◦C, compressive
strength parallel to the grain is less than that of the untreated sample.
Because, cellulose and lignin content in bamboo is responsible for the elasticity and strength,
hardness and rigidity, respectively. The increase of cellulose and lignin has a positive effect on
strength. Increase in compressive strength parallel to grain due to the cross-linking of lignin
polymer during the heat treatment. Lignin is the main component of the interlayer of bamboo,
cross-linkings enhance the strength of the intermediate layer and are affected by the strength of
the nature of the cell wall.

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The bending strength and bending modulus of elasticity of treated and untreated bamboo samples
are shown in Figure 7.

Fig. 7. The bending strength and MOE of treated and untreated samples at varied temperatures
for varied times.
(SOURCE: The effect of oil heat treatment on biological, mechanical, and physical properties of
bamboo, (2021))

Bending strength first increases and then decreases. The bending strength of the sample increases
by 8.46%, 19.26%, and 17.25% respectively at 160, 180, and 200 ◦C for 2 hours. At first
moisture content at the fiber saturation point decreases, dimensional stability improves, and
strength increases. At the same temperature, strength decreases due to the degradation of
chemical components, cellulose, and hemicellulose.
The modulus of elasticity of oil heated sample is higher than that of the C0 group, showing that
the treated sample has higher strength and better dimensional stability. It reaches a maximum
value of 12373MPa at 180 degrees Celsius for 2 hours and increases by 59% compared with the
untreated bamboo samples.

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4.5 EFFECT ON DECAY RESISTANCE

Figure. 8 shows the weight loss of the sample before and after the treatment after incubation with
brown-rot fungi for 45 days. From the graph itself, it is clear that maximum weight loss, and
worse decay resistance. Weight loss of treated bamboo sample decreases even after the
incubation for 45 days, indicating better decay resistance.

Fig. 8. The weight loss of the sample after incubation with brown-rot fungi for 45 days.
(SOURCE: The effect of oil heat treatment on biological, mechanical, and physical properties
of bamboo, (2021))

Also, another reason for better decay resistance is due to the blockage of pits and degradation of
cellulose and hemicellulose.

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Figure. 9 shows the percentage of starch content present in the bamboo samples before and after
oil heat treatment.

Fig. 9. The starch content of treated and untreated samples at varied temperatures for varied
times.
(SOURCE: The effect of oil heat treatment on biological, mechanical, and physical properties
of bamboo, (2021))

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4.6 EFFECT OF ANTI-MILDEW PROPERTY TEST

Figure. 10. Shows the infection ratio of the treated and untreated samples under three mixed
fungi at varied times and temperatures. Three different molds are Aspergillus niger, Penicillium
citrinum, and Trichoderma viride. The infection ratio of samples after heat treatment is lower
than that of the control group. Mold growth requires appropriate temperature, moisture, and
humidity.

Fig. 10. The infection ratio of treated and untreated samples with three mixed fungi a) 140◦ 𝐶 b)
160◦ 𝐶 c)180◦ 𝐶 d) 200◦C
(SOURCE: The effect of oil heat treatment on biological, mechanical, and physical properties of
bamboo, (2021))

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Also, according to Figure 9. the starch content decreases with an increase in heated temperature
and time. The decrease in content of cellulose, hemicellulose, and starch inside the treated
bamboo sample restricts mold growth. Also, the blockage of pits results in the formation of oil
film on the surface of the treated sample, and molds are effectively restricted from entering into
the cell wall. Thus anti-mildew property bamboo improve.

5. CONCLUSION

From the analysis done by the researchers, I understood that the properties of treated bamboo can
be improved after thermal modification in comparison with the untreated bamboo samples.
After the treatment, there were no starch granules inside the cell lumen of the parenchyma cell
wall.
Decay resistance and anti-mildew property of the treated samples increases.
Maximum resulting bending strength and bending modulus of elasticity are 142.42MPa and
12373 MPa, respectively at 180 ◦C for 2 hours.
Cellulose and hemicellulose contents decrease on treatment, whereas relative lignin content
increases. Surface wettability decreases due to the change in the functional groups and the
micromorphology of the treated bamboo sample. Thereby increasing the hydrophobic character
of bamboo.

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6. REFERENCES

Reference 1:Hao, X., Wang, Q., Wang, Y., Han, X., Yuan, C., Lou, Z., Li, Y., (2021)
“The effect of oil heat treatment on biological, mechanical, and physical properties of bamboo.”
http://creativecommons.org/licenses/by/4.0/
Journal of Wood Science (2021) https://doi.org/10.1186/s10086-021-01959-7

Reference 2: Wu, J., Wang, X., Fei, B., Xu, W., Lian, C., Chen, H., (2021)
“ The mechanical properties and thermal conductivity of bamboo with freeze-thaw treatment.”
http://creativecommons.org/licenses/by/4.0/
Wu et al. Journal of Wood Science (2021) https://doi.org/10.1186/s10086-021-01998-0

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