FORM 2

THE PATENTS ACT, 1970 (39 of

1970)
&
THE PATENT RULES, 2003
Complete Specification
(See section 10 and rule 13)

1.Title of the Invention: A NOVEL NATURAL FIBER COMPOSITES WITH

ENHANCED THERMAL CONDUCTIVITY

2. Applicants
Name Nationality Address
Mr. Sivasubramanian Palanisamy Indian Associate Professor, Department of Mechanical
Engineering, Dilkap Research Institute of Engineering
and Management Studies, Neral, Karjat- 410101,
Raigarh, Maharashtra, India.
Dr. Sivakumar Karthikeyan Indian Associate Professor, Department of Mechanical
Engineering, SRM Valliammai Engineering College,
SRM Nagar, Chennai, Kanchipuram-603203, Tamil
Nadu, India.
Ms. Shweta Singh Indian Assistant Professor, Department of Mechanical Engineering,
Guru Ghasidas Vishwavidyalaya, Bilaspur, Chhattisgarh,
India.
Dr. P. Ranjith Indian Director of Physical Education, Department of Science
and Humanities, Sri Sairam Institute of Technology,
West Tambaram, Chennai, 600044
Dr. Yagya Dutta Dwivedi  Indian Associate Professor, Department of Aeronautical Engineering,
Institute of Aeronautical Engineering, Hyderabad, 500043

Dr. P. Suresh Kumar  Indian Associate Professor, Mechanical Engineering Department,

RVR&JC College of Engineering, Chowdsvaram, Guntur 

Mr. M. Sudhakar Indian Assistant Professor, Department of Mechanical

Engineering, Sri Sai Ram Engineering College,
West Tambaram, Chennai, Tamil Nadu - 600044
3. Preamble to the Description :
The following specification particularly describes the invention and the manner in which it is to be performed.
4. DESCRIPTION
FIELD OF THE INVENTION

The present invention aims to show a Novel Natural Composites with enhanced thermal

conductivity.

BACKGROUND OF THE INVENTION

Plastic is an important discovery that has improved the quality of human life. In the past few

decades, polymers played a significant role in the world’s economy because of their light

weight, recyclability, and good thermomechanical properties. However, the non-

biodegradability of polymer is a primary environmental concern. It is a hazardous material,

polluting the environment by generating a vast amount of non-biodegradable waste.

Unfortunately, there is no proper way of treating and recycling of polymer. Less than 9% of

the plastic is recycled, and the rest is landfilled or thrown into the environment, polluting

land, and sea. Hence, biodegradable biopolymers are recently considered as replacements for

traditional plastics. Natural fibres are currently used as alternative to synthetic fibres to

reinforce polymer composites for advanced applications. They are extracted from animals,

minerals, and plants, and provide strength and stiffness to the composites. Animal fibres are

mainly obtained from the hairy mammal, sheep wool, chicken feathers, and spiders. The

animal fibres have more tensile strength among the other natural fibres. The main constituent

of animal fibres is protein. The protein group can be subdivided into α-keratin fibres and

fibroin fibres. Hair, wool, and feathers come under α-keratin fibre, whereas silk and spider

web are under fibroin fibres. Mineral fibres are naturally produced and are made from

mineral resources. Ceramic and asbestos are well-known examples of mineral fibre.

However, the applications of asbestos are banned due to the health risk in humans. Among

the natural fibres, plant fibres are the most abundant and cheap. Hemp, jute, flax, sisal, abaca,
agave, pineapple, kenaf, ramie, and banana are the most used fibres for various industries.

The plant fibres are also known as cellulosic fibres since the major constituent is cellulose

and have promising mechanical properties. The high strength of natural fibres is due to the

hydrogen bonds and other linkages in the cellulosic content present in the natural fibres.

However, the performance of the fibre depends on biotic and abiotic factors such as part of

the plant from which the fibre is obtained, the geographical location of plant growth, and

harvest time.

SUMMARY OF THE INVENTION

Natural fibre-reinforced composites possess many advantages such as low density,

biodegradability, and recyclability. Thus, natural fibre composites have been considered as an

alternative to synthetic fibre-based composites. Though the natural fibres are hydrophilic, less

resistant to wet environmental conditions, and highly susceptible to moisture, they are widely

used in many applications, including automotive, aerospace, and infrastructure, whereby

these composites are limited to semi-structural and non-structural applications. In this

context, hybrid fibre composites have been developed. Thus, the result of hybridized

composites exhibits a balance of mechanical properties, thermal stability, aggressive

environmental conditions, and cost reduction. In this chapter, the thermal properties of

natural fibre-based hybrid composites were discussed. Many researchers reported that the

thermal stability of hybridized composites provided enhanced properties; also, the hybrid

composites overcome the drawbacks of single fibre-reinforced composites. Besides, the

hybridization helps to improve the physical property and dimensional stability of the

composites. The performance of the hybrid composites could also be influenced by chemical

treatments, type of matrix, bonding strength between the fibre and matrix, and weight

percentages of fibres used.

BRIEF DESCRIPTION OF THE DRAWINGS

Fig.1: depicts natural fiber reinforced polymer composites.

Fig.2: depicts thermal conductivity.

BRIEF DESCRIPTION OF THE INVENTION

Plastic is an important discovery that has improved the quality of human life. In the past few

decades, polymers played a significant role in the world’s economy because of their light

weight, recyclability, and good thermomechanical properties. However, the non-

biodegradability of polymer is a primary environmental concern. It is a hazardous material,

polluting the environment by generating a vast amount of non-biodegradable waste.

Unfortunately, there is no proper way of treating and recycling of polymer. Less than 9% of

the plastic is recycled, and the rest is landfilled or thrown into the environment, polluting

land, and sea. Hence, biodegradable biopolymers are recently considered as replacements for

traditional plastics. Natural fibers are currently used as alternative to synthetic fibers to

reinforce polymer composites for advanced applications. They are extracted from animals,

minerals, and plants, and provide strength and stiffness to the composites. Animal fibers are

mainly obtained from the hairy mammal, sheep wool, chicken feathers, and spiders. The

animal fibers have more tensile strength among the other natural fibers. The main constituent

of animal fibers is protein. The protein group can be subdivided into α-keratin fibers and

fibroin fibers. Hair, wool, and feathers come under α-keratin fiber, whereas silk and spider

web are under fibroin fibers. Mineral fibers are naturally produced and are made from

mineral resources. Ceramic and asbestos are well-known examples of mineral fiber.

However, the applications of asbestos are banned due to the health risk in humans. Among

the natural fibers, plant fibers are the most abundant and cheap. Hemp, jute, flax, sisal, abaca,

agave, pineapple, kenaf, ramie, and banana are the most used fibers for various industries.
The plant fibers are also known as cellulosic fibers since the major constituent is cellulose

and have promising mechanical properties. The high strength of natural fibers is due to the

hydrogen bonds and other linkages in the cellulosic content present in the natural fibers.

However, the performance of the fibers depends on biotic and abiotic factors such as part of

the plant from which the fiber is obtained, the geographical location of plant growth, and

harvest time.

The fibers are extracted from the plants by manual extraction, retting, and mechanical

extraction, where the latter is the most preferred method for the industrial production of plant

fibers. Plant fibers are commonly used as reinforcement for both thermoplastic and thermoset

polymers. Recently, natural fibers are used with biodegradable polymers such as polylactic

acid (PLA), polycaprolactone (PCL), and poly(3-hydroxybutyrate-co-3-hydroxyvalerate)

(PHBV). However, the plant fibers are hydrophilic, while most of the polymers are

hydrophobic. Thus, the plant fibers have poor adhesion with polymer matrices. In improving

the compatibility of natural fibers with polymer matrices, the fibers were surface-treated with

chemical reagents, plasma, laser, ozone, ultraviolet (UV) irradiation, corona treatment, and

polymer coating. The factors that affect the properties of the composites are the size of the

fiber, fiber diameter, aspect ratio, extraction method, and cellulose content. The

disadvantages of natural fiber-reinforced composites are their anisotropic properties, moisture

adsorption, and low thermal resistance. Even though chemical and physical treatments

improve composites’ overall performance, there are drawbacks such as limited mechanical

properties, excess water adsorption, and poor thermal properties compared with synthetic

fiber-based composites. These deficiencies of natural fiber-reinforced composites can be

overcome using new methods such as compatibilization and hybridization. In the

compatibilization, a coupling agent compatible with both natural fibers and polymers are

preferred to use [20]. Studies have shown that the compatibilizer is required to have adequate
enhancements in the properties of the natural fiber-based polymer composites [21]. In the

hybridization, two or more natural fibers or natural and synthetic fibers/fillers are used to

improve the performance. There is a new method called self-hybridization, in which the same

fibers with different aspect ratios are used for property improvement. The property of the

hybridized composites depends on the fiber loading, fiber length, fiber orientation,

fiber/matrix bonding, and stacking sequence in the composites. Recently, most of the studies

concentrate on hybridizing natural and synthetic fibers rather than hybrid composites made

up of two plant fibers. This is because the properties of the hybrid composites complement

with what is lacking in the other fiber and hence justifiable.

THERMAL PROPERTIES OF NATURAL FIBER COMPOSITES

Thermogravimetric Analysis (TGA) Thermogravimetric analysis (TGA) is used to measure

the change in weight percentage of the sample as a function of temperature. Purge gas was

flown through the balance to create an inert atmosphere. Usually, nitrogen (N2) is used as the

purge gas. Prior to the reinforcement of the fibers with polymer matrices, the thermal stability

of the natural fibers was measured. The thermogram of buriti fiber is shown. It can be noticed

that the natural fiber undergone decomposition at various temperatures. The constituents of

natural fiber such as cellulose, hemicellulose, pectin, lignin, moisture, etc. are volatiles and

decomposes at elevated temperatures. The initial weight loss at 50–100 ∘C is due to the

release of moisture from the fiber. The weight loss between 200 and 350 ∘C is due to the

decomposition of hemicellulose, and the main degradation in the temperature range of 320–

400 ∘C is due to the decomposition of cellulose.

due to the decomposition of hemicellulose in the SPF. In another study, fabricated hybrid

TPU composites reinforced with the treated SPF and GF. The composites reinforced with

treated fiber showed lower water absorption properties and higher thermal stability. The best
thermal properties were observed for 6% alkaline-treated and 2% silane-treated fiber

composites studied the thermal properties of epoxy hybrid composites containing raw jute

and banana fiber. The composites with the varying weight ratio of banana and jute fiber

(100/0, 75/25, 50/50, 25/75, and 0/100) were prepared. Among the composites studied, an

even combination of banana and jute fiber showed the best thermal properties shows the

differences in thermal stability of varying weight ratio of banana and jute fiber-reinforced

epoxy composites studied the thermal stability of flax/carbon fiber-based hybrid epoxy

composites. Two types of flax fibers such as unidirectional (UD) and cross-ply (CP) were

used for the fabrication of composites. On the other hand, unidirectional carbon fiber was

commonly used. The flax fiber-reinforced epoxy composite showed the lowest thermal

stability among the composites prepared. The hybridization of flax fiber with carbon fiber

improved the onset temperature, main decomposition peak temperature, and char residue. The

results suggest that hybridizing natural fiber with synthetic fiber was a good method to

improve the thermal stability of the composites. Kumar and Reddy studied the thermal

behavior of 5% NaOH-treated and NaOH-untreated sisal/glass fiber-reinforced epoxy

composites. The authors observed improved thermal stability and char residue for the epoxy

hybrid composites when treated fibers were used. Srinivasan studied the thermal stability of

glass/flax epoxy composites, glass/banana epoxy composites, and glass/flax/banana epoxy

composites. The authors reported the highest thermal stability and limiting oxygen index for

the hybrid glass/flax/banana fiber-reinforced epoxy composites performed TGA of epoxy-

based natural fiber composites. The fibers such as Cocos nucifera sheath, Kevlar, and

graphene nanoplatelets were used to fabricate the composites. The authors observed three

stages of thermal decomposition for the composite prepared. The initial degradation at 100

∘C was due to the evaporation of moisture. The main degradation at 300 ∘C was due to the

degradation of the epoxy matrix. Also, the final degradation above 500 ∘C was due to the
degradation of Kevlar and graphene nanoplatelets. The authors proposed a schematic

showing the thermal degradation of hemicellulose, cellulose, and lignin along with epoxy,

Kevlar, and graphene nanoplatelets in the composites, the heat deflection temperature (HDT)

and thermal stability of bio-poly (tri-methylene terephthalate) (bio-PTT)-based hybrid

composites containing lignin nanoparticle (LNP) and vapor grown carbon fiber (VGCF).

TGA and differential thermogravimetric (DTG) curves of bio-PTT and hybrid

nanocomposites are shown. Bio-PTT reported an HDT of ∼55 ∘C, and this value increased to

∼120 ∘C with the addition of 1.5% of LNP into bio-PTT. The HDT of bio-PTT further

increases to ∼180 ∘C by incorporating 1.5% of LNP and 7% VGCF. TGA results indicates a

good improvement in the initial degradation temperature, the temperature at 50%

degradation, and final degradation temperature with the incorporation of 1.5% of LNP and

7% VGCF in bio-PTT. The improvement in HDT and thermal stability of the hybrid

composites was due to the better dispersion and interaction of the fillers with the polymer

matrix, the thermal behavior of the sisal fiber-reinforced PLA composites. The thermal

stability of the PLA composites was reduced with the incorporation of sisal fibers. It was

ascribed to the lower thermal stability of the sisal fiber than the pure PLA matrix. The effect

of recycling on the thermal stability of the composites was also studied. The use of recycled

thermoplastics reduced the thermal stability of the composites, especially with fiber content

above 20% observed a reduction in thermal stability of PHBV matrix with the addition of

Ceiba pentandra fiber. The hydrolysis of PHBV caused the drop in thermal stability due to

the presence of the OH groups in the natural fiber, observed that the decomposition of the

PLA composites occurred at a lower temperature with the incorporation of chicken feather

fiber (CFF). This is due to the lower thermal stability of the CFF than that of PLA. The aging

effect on the thermal decomposition of the PLA composites was also studied. The results
showed that the thermal stability of pure PLA and its composites was marginally reduced

after the aging studies.

Differential scanning calorimetry (DSC) was used to study the thermal transitions in natural

fibers or natural fiber-reinforced polymer composites. It works on a simple principle by

measuring the difference in the heat flow rate between the sample and the reference that

permits the determination of various endothermic and exothermic processes taking place in

the sample during thermal heating. The thermal parameters such as glass transition

temperature (Tg), cold crystallization temperature (Tcc), melting temperature (Tm), enthalpy

of melting (ΔHm), crystallization temperature (Tc), enthalpy of crystallization (ΔHc), and

percent crystallinity are measurable from the DSC thermogram, performed the DSC

thermograms of vascular bundles and fiber strands of date palm tree. A series of exothermic

and endothermic peaks were observed for both vascular bundles and fiber strands. The

endothermic peak at ∼93 ∘C of vascular bundles and ∼89 ∘C of fiber strands showed the

evaporation of moisture absorbed in the fibers. The exothermic peak at ∼297 ∘C of vascular

bundles and ∼284 ∘C of fiber strands exhibited the degradation of hemicellulose of the fibers,

while the peak at ∼367 ∘C of vascular bundles and ∼356 ∘C for fiber strands corresponds to

cellulose degradation. On the other hand, the exothermic peak at ∼432 ∘C of vascular

bundles and ∼419 ∘C of fiber strands corresponds to the degradation of lignin, fabricated

PLA-based hybrid composites containing sisal fiber and cuprous oxide (Cu2O) particles and

studied the thermal transitions of the composites using the DSC. It was observed that the

incorporation of sisal fiber and Cu2O filler improves the percent crystallinity of the PLA

because both the filler and fiber provide new sites for the crystallization of the polymer, the

DSC of curcumin-modified PLA composites. The incorporation of curcumin improved the

crystallinity of the PLA due to the heterogeneous nucleation caused by the presence of

curcumin carried out the DSC analysis of before and after aged CFF-reinforced PLA
composites. The concentration of the CFF used for the fabrication of the composites was 2%,

5%, and 10%. The Tg of PLA was marginally reduced with the incorporation of CFF, which

may be due to the plasticizing action of CFF. The Tcc was not observed in the neat PLA

sample. However, Tcc was observed in the composite samples, suggesting that the

crystallization rate was decreased in the presence of CFF. The Tm of PLA showed no change

with the incorporation of the CFF. On the other hand, the Tg of the aged samples (neat PLA

and composites) increased by ∼10 ∘C, possibly due to the restriction in the mobility of the

PLA chains caused by the embrittlement of polymer during the aging process The Tcc and

Tm showed only marginal variations but within the experimental limits, aging of wood flour-

reinforced PLA composites. Before starting the experiment, the composite samples were fully

desiccated or fully submerged for 3 days at various temperatures. The DSC analysis reported

that the Tg, Tcc, and Tm values of the submerged samples are lower than that of the fully

desiccated samples. It may be attributed to the degradation of the samples in fully submerged

conditions, fabricated the acetylated micro fibrillated cellulose with high cellulose modified

PLA composites. DSC thermograms of PLA/acetylated micro fibrillated cellulose composites

and their photograph. The Tg, Tcc, and Tm of PLA exhibit marginal variations with the

incorporation of the acetylated micro fibrillated cellulose. On the other hand, the authors

reported a good improvement in crystallinity with the incorporation of acetylated micro

fibrillated cellulose, because the filler acts as the nucleating agent for the crystallization of

the PLA matrix. The photographs of the composites shown in Figure 3.8b shows good

transparency irrespective of the filler content, showing uniform distribution of the filler in the

polymer matrix.
We Claim:

1. Samples of natural fibers with varying density from 39,6 kg/m 3 to 102,5 kg/m3,

thermal conductivity, respectively, varies from 0.0599 W/(m·K) to 0.0341 W/(m·K).

2. Despite their low intrinsic thermal conductivity (Table I) and the high Kapitza

resistance, Pyrograf fibers yield the highest thermal conductivity among our

composites with untreated carbon fillers.

3. These fibers can be further elaborated into six types include bast fibers (flax, jute,

etc.), leaf fibers (sisal, pineapple leaf fiber), seed fibers (cotton, coir), core fibers

(hemp, kenaf) grass and reed fibers (wheat, corn, and rice) and all other types (wood

and roots).

4. The thermal conductivity of a fabric is the ratio of the heat energy transferred per

second per unit surface area of the fabric to the temperature difference.

5. Diamond is the leading thermally conductive material and has conductivity values

measured 5x's higher than copper, the most manufactured metal in the United States.

6.  Diamond atoms are composed of a simple carbon backbone that is an ideal molecular

structure for effective heat transfer.

7. The experimental results show that the epoxy composite with the T-Zn network

structure has higher thermal conductivity (4.38 W/ (m K)), which is about 2.7 times

that of the composite with the ZnO network structure.

Dated this the 12th February 2023.

Senthil Kumar B
Agent for the applicant
IN/PA-1549
 ABSTRACT

A NOVEL NATURAL FIBER COMPOSITES WITH

ENHANCED THERMAL CONDUCTIVITY

The use of plant fibers for potential applications such as building, automobile, marine, and

aerospace have received huge attention due to the high cost, complicated manufacturing

process, non‐recyclability, and non‐biodegradability of the synthetic fibers. In this chapter,

the thermal properties of the natural fiber‐based polymer composites were reviewed. The

thermal analysis (TA) techniques are used to measure materials' responses during heating or

cooling and to study the interrelationship between physical property of the materials and

temperature. The popular TA techniques are thermogravimetric analysis (TGA), differential

scanning calorimetry (DSC), dynamic mechanical analysis (DMA), and thermomechanical

analysis (TMA). This chapter discusses TGA, DSC, and DMA of various natural‐fiber based

hybrid composites as they provide information on the thermal stability, thermal transitions,

and viscoelastic properties of the composites, respectively. The thermal properties of the

composites depend on various parameters such as type of natural fiber, fiber treatment,

hybridization with synthetic fibers and nanofillers, distribution of fibers, and interfacial

interaction between the fiber and the polymer.