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Graphene Reinforced Concrete Composition And A Process For Its Preparation

Abstract: ABSTRACT GRAPHENE REINFORCED CONCRETE COMPOSITION AND A PROCESS FOR ITS PREPARATION The present disclosure relates to a graphene reinforced concrete composition and a process for its preparation. The graphene reinforced concrete composition of the present disclosure demonstrates improved compressive strength, flexural strength, split tensile strength and reduced water permeability, chloride ingress, crack propagation compared to the conventional concrete.

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Patent Information

Application #
Filing Date
30 January 2024
Publication Number
31/2025
Publication Type
INA
Invention Field
CHEMICAL
Status
Email
Parent Application

Applicants

RELIANCE INDUSTRIES LIMITED
3RD FLOOR, MAKER CHAMBER-IV, 222, NARIMAN POINT, MUMBAI-400021, MAHARASHTRA, INDIA

Inventors

1. Vivek Prabhakar Raje
Vertica C-102, Casa Bella Gold, Palava city, Nilje, Dombivali East, Thane-421204, Maharashtra, India
2. Amol Shewale
Shree Samarth Krupa, RH-04, Om Sai Residency, Behind metro driving school, Karad, Dist Satara-415110, Maharashtra, India
3. Debarati Roy Chowdhury
Saradapalli, Ramkrishna Asram Road, Panihati, Kolkata-700114, West Bengal, India
4. Joseph Berkmans Amirthasamy
21, Subramaniyaraja Nagar, 3rd street, Sivaganga-630561, Tamil Nadu, India

Specification

DESC:FIELD
The present disclosure relates to the field of construction materials.
DEFINITION
As used in the present disclosure, the following terms are generally intended to have the meaning as set forth below, except to the extent that the context in which they are used, indicate otherwise.
Slump Height: The term “slump height” refers to the height of the slumped column of concrete in a test used to measure its consistency and workability. In this test, fresh concrete is placed in a conical mold, then lifted away, allowing the concrete to slump or settle. The difference in height between the top of the mold and the highest point of the slumped concrete is measured as slump height. It indicates the fluidity of the concrete mix, with higher slumps representing more fluid mixtures.
Retention time: The term “retention time” refers to the time period during which the concrete maintains its desired workability or consistency before it begins to set or harden. This property is crucial for ensuring that the concrete can be transported, placed, and compacted effectively without significant loss of quality.
Compressive strength: The term “compressive strength” refers to a material's ability to withstand forces without breaking or failing. It's a crucial property in engineering and construction, as many materials are subjected to compressive loads. It is generally expressed in N/m2.

Flexural strength: The term “flexural strength” also known as “modulus of rupture, bend strength, or transverse rupture strength”, refers to the ability of a material to resist deformation or failure under bending. It represents the maximum stress, a material can withstand at the point of failure when subjected to a bending load.

wherein F: Maximum applied load (N), L: Span length (distance between supports) (m), b: Width of the specimen (m), and d: Thickness of the specimen (m).
Split tensile strength: The term “split tensile strength” refers to the tensile strength of a material measured indirectly by applying a compressive load along a cylinder's diameter. The load induces tensile stress perpendicular to the loading plane, ultimately causing the specimen to split. This tensile stress is calculated as the split tensile strength.

wherein, T: Split tensile strength (Pa or MPa), P: Maximum applied load before failure (N), L: Length of the cylindrical specimen (m), and D: Diameter of the cylindrical specimen (m).
Chloride ingress: The term “chloride ingress” refers to the penetration of chloride ions into concrete, especially in structures exposed to marine environments, deicing salts, or industrial pollutants. Chloride ingress is a critical concern of durability issues because it leads to the corrosion of steel reinforcement, which compromises the structural integrity and lifespan of concrete structures.
BACKGROUND
The background information herein below relates to the present disclosure but is not necessarily prior art.
Concrete is a widely used construction material known for its strength, durability, and versatility. Cement is the key ingredient in concrete, which is responsible for generation of massive environmental pollution and carbon footprint. Production of Portland cement involves quarrying that cause airborne pollution in the form of dust. During the production of clinker, limestone (CaCO3) gets converted to lime (CaO) and CO2. Huge amount of CO2 is also emitted during cement production by fossil fuel combustion. Due to economic and environmental concerns, there is always a room for the development of the concrete compositions without compromising the mechanical properties of the concrete.
Furthermore, conventional concrete compositions are typically brittle when cured. Various approaches were adopted for the production of concrete with improved mechanical properties and enhanced durability to reduce the overall maintenance cost. Usually, additives are added to improve the strength of the concrete such as silica fume, rice husk ash, carbon fiber, steel fiber, natural pumice, resins, enzyme, isocyanate compounds, epoxy compounds and the like. However, uses of these additives are restricted with limited applications.
Generally, steel bars are used as reinforcement in concrete structures to enhance its mechanical properties. However, steel may undergo corrosion due to chloride ion migration, carbonation of concrete and lack of oxygen surrounding the steel bar. The corrosion of steel leads to generation of rust which causes a loss of bond between the steel and the concrete and subsequent delamination and spalling. Various measures have been taken to reduce the chloride ion migration and water permeability into the concrete structure in order to protect steel rebar corrosion. Permeability-reducing admixtures (PRAs) can be considered as an option to reduce water ingress and improve lifespan of the concrete structures. Permeability reducing admixtures includes silicates, alkyl siliconates, slaked lime, oxides, fatty acid salts and the like. However, few of these additives underperform in harsh environmental conditions and may cause difficulty in mixing.
Furthermore, the hydration of cement in the concrete generates enormous amount of heat. Due to low thermal diffusivity in the concrete, a temperature gradient is generated between the inner core and the outer surface of the structure, resulting in thermal cracking. Various additives such as carbon nanotubes, titanium oxide, nanosilica, nano alumina, hydrated salts, and the like, are added to reduce the thermal cracking. Still further, the additives are added in concrete to reduce the overall carbon dioxide emission and cost. Addition of so many additives in the concrete for the above-mentioned reasons can add extra processing steps, cost, and labour and time as well.
Therefore, there is felt a need to provide a concrete that can mitigate the drawbacks mentioned hereinabove or at least provides an alternative solution.
OBJECTS
Some of the objects of the present disclosure, which at least one embodiment herein satisfies, are as follows:
It is an object of the present disclosure is to ameliorate one or more problems of the background or to at least provide a useful alternative.
Still another object of the present disclosure is to provide a graphene reinforced concrete material.
Yet another object of the present disclosure is to provide a graphene reinforced concrete material that is strong, crack resistant, low permeable, thermally stable, durable, and lightweight.
Still another object of the present disclosure is to provide a graphene reinforced concrete material that provides enhanced service life.
Yet another object of the present disclosure is to provide a graphene reinforced concrete material that provides reduced carbon footprint.
Still another object of the present disclosure is to provide a graphene reinforced concrete material that provides enhanced processability.
Yet another object of the present disclosure is to provide a process for the preparation of a graphene reinforced concrete material that is simple and efficient.
Other objects and advantages of the present disclosure will be more apparent from the following description, which is not intended to limit the scope of the present disclosure.
SUMMARY
In an aspect the present disclosure relates to a graphene reinforced composition comprising:
a. a concrete composition; and
b. a non-aqueous graphene dispersion,
The non-aqueous graphene dispersion is uniformly distributed in the concrete composition, and the amount of graphene is in the range of 0.0002 mass% to 0.02 mass% with respect to the total mass of the concrete composition.
In an embodiment of the present disclosure, the non-aqueous graphene dispersion is a homogeneous mixture of a graphene material dispersed in a non-aqueous fluid medium optionally with a surfactant.
In an embodiment of the present disclosure, the non-aqueous fluid medium is selected from the group consisting of monoethylene glycol (MEG), diethylene glycol, polyvinyl alcohol, ethanol and propanol.
In an embodiment of the present disclosure, the concrete composition comprises cement, coarse aggregates, fine aggregates, fly ash and optionally ground granulated blast-furnace slag (GGBS).
In an embodiment of the present disclosure, the surfactant is at least one selected from the group consisting of cellulose, polyvinyl pyrrolidone (PVP), polycarboxylate ether, polyethylene oxide, dodecyl sulfate, lauryl sulfate, cetyltrimethylammonium bromide, polyethylene oxide and alkyl phenol ethoxylate.
In an embodiment of the present disclosure, the graphene material is at least one selected from the group consisting of graphene, graphene oxide, reduced graphene oxide, graphene nanoribbons, graphene quantum dots and doped graphene.
In an embodiment of the present disclosure, the graphene comprises 70% to 85% of a single layer graphene and about 15% to 30% of a multilayer graphene.
In an embodiment of the present disclosure, the multilayer graphene comprises two-layer graphene, three-layer graphene, four-layer graphene, five-layer graphene and any combination thereof.
In an embodiment of the present disclosure, the reinforced exhibits at least one of the following properties:
• compressive strength in the range of 10% to 45% greater than the compressive strength of conventional concrete which is in the range of 20 N/mm2 to 115 N/mm2;
• flexural strength in the range of 10% to 40% greater than the flexural strength of conventional concrete which is in the range of 2 N/mm2 to 10 N/mm2;
• split tensile strength in the range of 5% to 45% greater than the split tensile strength of conventional concrete which is in the range of 1.5 N/mm2 to 8 N/mm2;
• chloride ingress in the range of 40% to 90% less than the chloride ingress of conventional concrete which is in the range of 3 x 10-12 m2 s-1 to 18 x 10-12 m2 s-1 ;
• water permeability in the range of 40% to 90% less than the water permeability of conventional concrete which is in the range of 2 mm to 30 mm;
• acid resistance (strength loss) in the range of 40% to 50% more than the acid resistance of conventional concrete in which strength loss is in the range of 8% to 35%; and
• sulphate resistance (length change) in the range of 80% to 85% more than the sulphate resistance of conventional concrete in which the length change is in the range of 0.012% to 0.07%.
In another aspect, the present disclosure relates to a process for the preparation of a graphene reinforced composition. The process comprises the following steps:
a) mixing predetermined amounts of a graphene material, a non-aqueous fluid medium, and optionally a surfactant, at a speed in the range of 100 rpm to 10000 rpm, and for a first predetermined time period to obtain a non-aqueous graphene dispersion; and
b) mixing the non-aqueous graphene dispersion to a concrete composition for a second predetermined time period to obtain the graphene reinforced composition.
In an embodiment of the present disclosure, the concrete composition comprises cement, coarse aggregates, fine aggregates, fly ash, and optionally ground granulated blast-furnace slag (GGBS), and admixture.
In an embodiment of the present disclosure, the surfactant is at least one selected from the group consisting of cellulose, polyvinyl pyrrolidone (PVP), polycarboxylate ether, polyethylene oxide, dodecyl sulfate, lauryl sulfate, cetyltrimethylammonium bromide, polyethylene oxide and alkyl phenol ethoxylate.
In an embodiment of the present disclosure, the non-aqueous fluid medium is at least one selected from the group consisting of monoethylene glycol (MEG), diethylene glycol (DEG), polyvinyl alcohol (PVA), ethanol and propanol.
In an embodiment of the present disclosure, the graphene material is at least one selected from the group consisting of graphene, graphene oxide, reduced graphene oxide, graphene nanoribbons, graphene quantum dots and doped graphene.
In an embodiment of the present disclosure, the graphene comprises 70% to 85% single layer graphene and about 15% to 30% multilayer graphene.
In an embodiment of the present disclosure, the first predetermined time period is in the range of 2 hours to 5 hours.
In an embodiment of the present disclosure, the predetermined temperature is in the range of 20 °C to 40 °C.
In an embodiment of the present disclosure, the second predetermined time period is in the range of 20 hours to 30 hours.
In an embodiment of the present disclosure, the predetermined amount of the graphene material is in the range of 0.001 mass% to 2 mass% with respect to the total mass of the non-aqueous graphene dispersion.
In an embodiment of the present disclosure, the predetermined amount of non-aqueous fluid medium is in the range of 55 mass% to 99.5 mass% with respect to the total mass of the non-aqueous graphene dispersion.
In an embodiment of the present disclosure, the predetermined amount of surfactant is in the range of 0 mass% to 45 mass% with respect to the total mass of the non-aqueous graphene dispersion.
In an embodiment of the present disclosure, the graphene reinforced composition is retained for a predetermined retention period followed by casting and curing at a predetermined temperature for a second predetermined time period to obtain a cured object.
In an embodiment of the present disclosure, the predetermined retention period is in the range of 30 minutes to 150 minutes.
In an embodiment of the present disclosure, the graphene reinforced composition is casted and cured at a temperature in the range of 20 °C to 40 °C to obtain the cured object.
DETAILED DESCRIPTION
The present disclosure relates to the field of construction materials. Particularly, the present disclosure relates to graphene reinforced concrete material and a process for its preparation.
Embodiments, of the present disclosure, will now be described herein. Embodiments are provided so as to thoroughly and fully convey the scope of the present disclosure to the person skilled in the art. Numerous details are set forth, relating to specific components, and methods, to provide a complete understanding of embodiments of the present disclosure. It will be apparent to the person skilled in the art that the details provided in the embodiments should not be construed to limit the scope of the present disclosure. In some embodiments, well-known processes, well-known apparatus structures, and well-known techniques are not described in detail.
The terminology used, in the present disclosure, is only for the purpose of explaining a particular embodiment and such terminology shall not be considered to limit the scope of the present disclosure. As used in the present disclosure, the forms "a,” "an," and "the" may be intended to include the plural forms as well, unless the context clearly suggests otherwise. The terms "comprises," "comprising," “including,” and “having,” are open ended transitional phrases and therefore specify the presence of stated features, integers, steps, operations, elements, modules, units and/or components, but do not forbid the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof. The particular order of steps disclosed in the method and process of the present disclosure is not to be construed as necessarily requiring their performance as described or illustrated. It is also to be understood that additional or alternative steps may be employed.
As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed elements.
The terms first, second, third, etc., should not be construed to limit the scope of the present disclosure as the aforementioned terms may be only used to distinguish one element, component, region, layer or section from another component, region, layer or section. Terms such as first, second, third etc., when used herein do not imply a specific sequence or order unless clearly suggested by the present disclosure.
Concrete structures face challenges due to weak mechanical properties and susceptibility to cracks, necessitating frequent, costly maintenance. Reinforced concrete with steel re-bar helps resist tensile stresses but faces issues like corrosion from chloride ingress, impacting structural integrity and adding repair costs. Further, cement production emits significant amount of CO2 and is expensive, prompting a need to reduce cement usage without compromising strength. Furthermore, high heat from cement hydration causes thermal cracking in mass concrete, while long curing times delay construction. Adding additives can accelerate curing and improve properties, but multiple additives increase complexity and costs. Therefore, there is an urgent need for a multifunctional additive to create durable, strong, low-permeable, and environmentally friendly concrete.
The present disclosure provides a graphene reinforced concrete material that is exhibits improved compressive strength, improved flexural strength, improved split tensile strength, improved acid resistance, reduced water permeability, reduced chloride ingress, and reduced crack propagation as compared to conventional concrete material.
In an aspect the present disclosure relates to a graphene reinforced composition comprising:
a. a concrete composition; and
b. a non-aqueous graphene dispersion,
The non-aqueous graphene dispersion is uniformly distributed in the concrete composition, and the amount of graphene is in the range of 0.0002 mass% to 0.02 mass% with respect to the total mass of said concrete composition.
In an exemplary embodiment, the amount of graphene is 0.0005 mass% with respect to the total mass of the concrete composition. In another exemplary embodiment, the amount of graphene is 0.0004 mass% with respect to the total mass of the concrete composition. In yet another exemplary embodiment, the amount of graphene is 0.0006 mass% with respect to the total mass of the concrete composition. In still another exemplary embodiment, the amount of graphene is 0.0018 mass% with respect to the total mass of the concrete composition. In yet another exemplary embodiment, the amount of graphene is 0.0019 mass% with respect to the total mass of the concrete composition. In still another exemplary embodiment, the amount of graphene is 0.019 mass% with respect to the total mass of the concrete composition.
In an embodiment of the present disclosure, the non-aqueous dispersion is a homogeneous mixture of a graphene material dispersed in a non-aqueous fluid medium optionally with a surfactant.
In an embodiment of the present disclosure, the non-aqueous fluid medium is selected from the group consisting of monoethylene glycol (MEG), diethylene glycol (DEG), polyvinyl alcohol (PVA), ethanol and propanol. In an exemplary embodiment, the non-aqueous fluid medium is monoethylene glycol (MEG).
In an embodiment of the present disclosure, the concrete composition comprises cement, coarse aggregates, fine aggregates, fly ash and optionally ground granulated blast-furnace slag (GGBS). In an exemplary embodiment, the concrete composition comprises cement, coarse aggregates, fine aggregates, and fly ash. In another exemplary embodiment, the concrete composition comprises cement, coarse aggregates, fine aggregates, and ground granulated blast-furnace slag (GGBS).
In an embodiment of the present disclosure, the surfactant is at least one selected from the group consisting of cellulose, polyvinyl pyrrolidone (PVP), polycarboxylate ether, polyethylene oxide, dodecyl sulfate, lauryl sulfate, cetyltrimethylammonium bromide, polyethylene oxide and alkyl phenol ethoxylate. In an exemplary embodiment, the surfactant is polyvinyl pyrrolidone (PVP). In another exemplary embodiment, the surfactant is polycarboxylate ether.
In an embodiment of the present disclosure, the graphene material is at least one selected from the group consisting of graphene, graphene oxide, reduced graphene oxide, graphene nanoribbons, graphene quantum dots and doped graphene. In an exemplary embodiment, the graphene material is graphene.
In an embodiment of the present disclosure, the graphene comprises 70% to 85% of a single layer graphene and about 15% to 30% of a multilayer graphene. In an exemplary embodiment, the graphene comprises 80% to 85% of a single layer graphene and 15% to 20% of a multilayer graphene.
In an embodiment of the present disclosure, the multilayer graphene comprises two-layer graphene, three-layer graphene, four-layer graphene, five-layer graphene and any combination thereof.
In an embodiment of the present disclosure, the reinforced exhibits at least one of the following properties:
• compressive strength in the range of 10% to 45% greater than the compressive strength of conventional concrete which is in the range of 20 N/mm2 to 115 N/mm2;
• flexural strength in the range of 10% to 40% greater than the flexural strength of conventional concrete which is in the range of 2 N/mm2 to 10 N/mm2;
• split tensile strength in the range of 5% to 45% greater than the split tensile strength of conventional concrete which is in the range of 1.5 N/mm2 to 8 N/mm2;
• chloride ingress in the range of 40% to 90% less than the chloride ingress of conventional concrete which is in the range of 3 x 10-12 m2 s-1 to 18 x 10-12 m2 s-1 ;
• water permeability in the range of 40% to 90% less than the water permeability of conventional concrete which is in the range of 2 mm to 30 mm;
• acid resistance (strength loss) in the range of 40% to 50% more than the acid resistance of conventional concrete in which strength loss is in the range of 8% to 35%; and
• sulphate resistance (length change) in the range of 80% to 85% more than the sulphate resistance of conventional concrete in which the length change is in the range of 0.012% to 0.07%.
In an exemplary embodiment, the compressive strength of conventional concrete which is in the range of 40 N/mm2 to 45 N/mm2, the flexural strength of the conventional concrete which is in the range of 4 N/mm2 to 7 N/mm2, the split tensile strength of conventional concrete which is in the range of 2 N/mm2 to 5 N/mm2; chloride ingress of the conventional concrete which is in the range of 9 x 10-12 m2 s-1 to 13 x 10-12 m2 s-1, the water permeability of conventional concrete which is in the range of 14 mm to 18 mm; acid resistance of conventional concrete in which strength loss is in the range of 18% to 20%, and the sulphate resistance of conventional concrete in which the length change is in the range of 0.025% to 0.03%.
In another aspect, the present disclosure relates to a process for the preparation of a graphene reinforced composition. The process comprises the steps of mixing predetermined amounts of a graphene material, a non-aqueous fluid medium, and optionally a surfactant at a speed in the range of 100 rpm to 10000 rpm, and for a first predetermined time period to obtain a non-aqueous graphene dispersion. The non-aqueous graphene dispersion is mixed to a concrete composition for a second predetermined time period to obtain the graphene reinforced composition.
The process is described in detail.
Predetermined amounts of a graphene material, a non-aqueous fluid medium, and optionally a surfactant are mixed at a speed in the range of 100 rpm to 10000 rpm, and for a first predetermined time period to obtain a non-aqueous graphene dispersion.
In an embodiment of the present disclosure, the predetermined amount of non-aqueous fluid medium is in the range of 55 mass% to 99.5 mass% with respect to the total mass of the non-aqueous graphene dispersion. In an exemplary embodiment, the predetermined amount of non-aqueous fluid medium is 98.8 mass% with respect to the total mass of the non-aqueous graphene dispersion. In another exemplary embodiment, the predetermined amount of non-aqueous fluid medium is 97.6 mass% with respect to the total mass of the non-aqueous graphene dispersion. In yet another exemplary embodiment, the predetermined amount of non-aqueous fluid medium is 59.4 mass% with respect to the total mass of the non-aqueous graphene dispersion. In still another exemplary embodiment, the predetermined amount of non-aqueous fluid medium is 99 mass% with respect to the total mass of the non-aqueous graphene dispersion.
In an embodiment of the present disclosure, the graphene material is at least one selected from the group consisting of graphene, graphene oxide, reduced graphene oxide, graphene nanoribbons, graphene quantum dots, and doped graphene. In an exemplary embodiment, the graphene material is graphene.
In an embodiment of the present disclosure, the predetermined amount of the graphene material is in the range of 0.001 mass% to 2 mass% with respect to the total mass of the non-aqueous graphene dispersion. In an exemplary embodiment, the predetermined amount of the graphene material is 1 mass% with respect to the total mass of the non-aqueous graphene dispersion. In another exemplary embodiment, the predetermined amount of the graphene material is 2 mass% with respect to the total mass of the non-aqueous graphene dispersion.
In an embodiment of the present disclosure, the graphene comprises 70% to 85% single layer graphene and about 15% to 30% multilayer graphene. In an exemplary embodiment, the graphene comprises 80% to 85% single layer graphene and about 15% to 20% multilayer graphene.
In an embodiment of the present disclosure, the non-aqueous fluid medium is at least one selected from the group consisting of monoethylene glycol (MEG), diethylene glycol (DEG), polyvinyl alcohol (PVA), ethanol and propanol. In an exemplary embodiment, the non-aqueous fluid medium is monoethylene glycol (MEG).
In an embodiment of the present disclosure, the surfactant is at least one selected from the group consisting of cellulose, polyvinyl pyrrolidone (PVP), polycarboxylate ether, polyethylene oxide, dodecyl sulfate, lauryl sulfate, cetyltrimethylammonium bromide, polyethylene oxide and alkyl phenol ethoxylate. In an exemplary embodiment, the surfactant is polyvinyl pyrrolidone (PVP). In another exemplary embodiment, the surfactant is polycarboxylate ether.
In an embodiment of the present disclosure, the predetermined amount of surfactant is in the range of 0 mass% to 45 mass% with respect to the total mass of the non-aqueous graphene dispersion. In an exemplary embodiment, the predetermined amount of surfactant is 0.2 mass% with respect to the total mass of the non-aqueous graphene dispersion. In another exemplary embodiment, the predetermined amount of surfactant is 0.4 mass% with respect to the total mass of the non-aqueous graphene dispersion. In yet exemplary embodiment, the predetermined amount of surfactant is 39.6 mass% with respect to the total mass of the non-aqueous graphene dispersion. In still exemplary embodiment, the predetermined amount of surfactant is 0 mass% with respect to the total mass of the non-aqueous graphene dispersion.
In an embodiment of the present disclosure, the first predetermined time period is in the range of 2 hours to 5 hours. In an exemplary embodiment, the first predetermined time period is 3 hours.
In an exemplary embodiment, the speed is 5000 rpm. In another exemplary embodiment, the speed is 8000 rpm. In yet another exemplary embodiment, the speed is 10000 rpm.
The non-aqueous graphene dispersion is mixed to a concrete composition for a second predetermined time period to obtain the graphene reinforced composition.
In an embodiment of the present disclosure, the concrete composition comprises cement, coarse aggregates, fine aggregates, fly ash, and optionally ground granulated blast-furnace slag (GGBS), and admixture. In an exemplary embodiment, the concrete composition comprises cement, coarse aggregates, fine aggregates, fly ash, and admixture. In another exemplary embodiment, the concrete composition comprises cement, coarse aggregates, fine aggregates, ground granulated blast-furnace slag (GGBS), and an admixture.
In an embodiment of the present disclosure, the second predetermined time period is in the range of 20 hours to 30 hours. In an exemplary embodiment, the second predetermined time period is 24 hours.
In an embodiment of the present disclosure, the graphene reinforced composition is retained for a predetermined retention period followed by casting and curing at a predetermined temperature for a second predetermined time period to obtain a cured object.
In an embodiment of the present disclosure, the predetermined retention period is in the range of 30 minutes to 150 minutes. In an exemplary embodiment, the predetermined retention period is 120 minutes.
In an embodiment of the present disclosure, the graphene reinforced composition is casted and cured at a temperature in the range of 20 °C to 40 °C to obtain a cured object. In an exemplary embodiment, the curing temperature is 27 °C.
In an embodiment of the present disclosure, the admixture is a commercially available admixture.
In an embodiment of the present disclosure, a predetermined mass ratio of the non-aqueous graphene dispersion to the concrete composition is in the range of 1:450 to 1:2200. In an exemplary embodiment, the predetermined mass ratio of the non-aqueous graphene dispersion to the concrete composition is 1:1826. In another exemplary embodiment, the predetermined mass ratio of the non-aqueous graphene dispersion to the concrete composition is 1:2029. In yet another exemplary embodiment, the predetermined mass ratio of the non-aqueous graphene dispersion to the concrete composition is 1:1578. In still another exemplary embodiment, the predetermined mass ratio of the non-aqueous graphene dispersion to the concrete composition is 1:1940. In yet another exemplary embodiment, the predetermined mass ratio of the non-aqueous graphene dispersion to the concrete composition is 1:1905. In still another exemplary embodiment, the predetermined mass ratio of the non-aqueous graphene dispersion to the concrete composition is 1:533. In yet another exemplary embodiment, the predetermined mass ratio of the non-aqueous graphene dispersion to the concrete composition is 1:518.
In an embodiment of the present disclosure, the fracture toughness is in the range of 24% to 73% which is comparatively more as compared to the conventional concrete composition.
In an embodiment of the present disclosure, the strength loss has been reduced more than 50%.
In an embodiment of the present disclosure, the acid resistance has been increased more than 50%.
In an embodiment of the present disclosure, the sulphate resistance (length change) has been increased to more than 80%.
The cured object of the present disclosure demonstrates improved compressive strength, flexural strength, split tensile strength and reduced water permeability, chloride ingress, crack propagation compared to the conventional concrete.
Graphene is a two-dimensional carbon-based nanomaterial with high aspect ratio, hexagonal honeycomb structure and high surface area. It has unique shape, morphology, particle size, chemical functionalities comprising sp2 carbon network and oxygen functionalities, which makes it a potential multifunctional additive for the concrete reinforcement. By incorporating graphene in an amount in the range of 0.0002 mass% to 0.02 mass% with respect to the total cementitious content in the concrete composition can provide significant improvement to the cured object in view of the compressive strength, flexural strength, split tensile strength, crack resistance, thermal durability and reduced water permeability, and reduced chloride ingress. Additionally, it enables the use of lower amount of cement resulting in lower production cost and reduced carbon emission, without compromising the mechanical property and lifespan of the cured object.
Graphene facilitates mobility of ions, especially Ca2+, and hence increases the interaction between cement surface and the ions. This strong interaction accelerates the C-S-H nucleation and growth and thereby promotes the hydration of cement which results in improved crystallinity. Due to the crystallinity of C-S-H crystals along with strong Young’s modulus of graphene together results in C-S-H material with improved strength. Graphene sheets connect with ettringite, C-S-H gel and other crystals, forming a 3-D network structure which makes the cement matrix stronger and tougher. The so obtained 3-D network structure fills the micro cracks and voids in the cementitious matrix, prevents the connection of internal cracks, improves the density of cement-based materials, and makes the graphene reinforced concrete materials more resistant to water permeability and chloride ion ingress.
The graphene reinforced concrete material reduces the chloride ingress and reduces permeability to water that implies reduced steel rebar corrosion and consequent enhancement in the durability and lifespan of the concrete.
In an embodiment of the present disclosure, the graphene reinforced concrete can reduce the hydration time of the concrete which can result in reduced turnaround time.
There are many additives available commercially such as silicates, alkyl siliconates, slaked lime, oxides, fatty acid salts, natural pumice, polyacrylonitrile fibers, silica fumes, rice husk ash, carbon fiber, steel fiber and the like, which helps to improve some of the concrete properties. However, to achieve all these properties together, various additives are required to be added simultaneously, which increases the overall cost, cycle time and labour. But graphene as a single multifunctional additive can provide several properties together for the generation of mechanically strong, crack resistant, low permeable, thermally stable, durable, lightweight concrete with enhanced service life and reduced carbon footprint.
The foregoing description of the embodiments has been provided for purposes of illustration and not intended to limit the scope of the present disclosure. Individual components of a particular embodiment are generally not limited to that particular embodiment but are interchangeable. Such variations are not to be regarded as a departure from the present disclosure, and all such modifications are considered to be within the scope of the present disclosure.
The present disclosure is further described in light of the following experiments which are set forth for illustration purpose only and not to be construed for limiting the scope of the disclosure. The following experiments are scalable to industrial/commercial process.
EXPERIMENTAL DETAILS
EXPERIMENT 1: Process for the preparation of a graphene reinforced composition in accordance with the present disclosure
Examples 1 to 6: Preparation of non-aqueous graphene dispersion
Example 1
10 g of graphene was mixed with 988 g of monoethylene glycol (MEG) and 2 g of polyvinyl pyrrolidone in a high shear mixer at a speed of 8000 rpm for 3 hours to obtain a non-aqueous graphene dispersion.
Example 2
20 g of graphene was mixed with 976 g of monoethylene glycol (MEG) and 4 g of polyvinyl pyrrolidone in a high shear mixer at a speed of 10000 rpm for 3 hours to obtain a non-aqueous graphene dispersion.
Example 3
10 g of graphene was mixed with 594 g of monoethylene glycol (MEG) and 396 g of polycarboxylate ether in a high shear mixer at a speed of 8000 rpm for 3 hours to obtain a non-aqueous graphene dispersion.
Example 4
20 g of graphene was mixed with 780 g of monoethylene glycol (MEG) and 200 g of polycarboxylate ether in a high shear mixer at a speed of 10000 rpm for 3 hours to obtain a non-aqueous graphene dispersion.
Example 5
10 g of graphene was mixed with 990 g of monoethylene glycol (MEG) in a high shear mixer at a speed of 5000 rpm for 3 hours to obtain a non-aqueous graphene dispersion.
Example 6
20 g of graphene was mixed with 980 g of monoethylene glycol (MEG) in a high shear mixer at a speed of 8000 rpm for 3 hours to obtain a non-aqueous graphene dispersion.
Stability studies of non-aqueous graphene dispersion
The formation of MEG based non-aqueous dispersion was optimized and stability of the dispersions using different surfactants with different amounts were studied in order to understand the impact of surfactant and amount of graphene on the stability of the non-aqueous graphene dispersion in Examples 1 to 6. Table 1 summarizes the result of the stability studies.
Table 1: Result of Stability studies
Example Amount of Graphene with respect to the non-aqueous graphene dispersion (mass%) Amount of the Surfactant with respect to the non-aqueous graphene dispersion (mass%) Amount of non-aqueous solvent (MEG) with respect to the non-aqueous graphene dispersion (mass%) Stability
Example 1 1 0.2 98.8 8 months
Example 2 2 0.4 97.6 7 months
Example 3 1 39.6 59.4 5 months
Example 4 2 20 78 4 months
Example 5 1 0 99 5 months
Example 6 2 0 98 4 months
When the amount of graphene is in the range of 1 mass% to 2 mass% with the amount of surfactant in the range of 0 mass% to 39.6 mass%, the dispersion is stable from 4 to 8 months. The concentration of graphene and surfactant have been optimized to achieve the highest stability. It was observed that Example 1, wherein the amount of graphene is 1 mass% and the amount of the surfactant (PVP) is 0.2 mass% with respect to the total amount of the non-aqueous dispersion showed maximum stability up to 8 months.
Examples 7 to 13: Preparation of graphene reinforced composition in accordance with the present disclosure
Example 7
1033 kg of coarse aggregates (20 mm and 10 mm) aggregates were mixed with 769 kg of sand (fine aggregates) for 1 minute to obtain a mixture of coarse and fine aggregates. 360 kg of cement along with 80 kg of fly ash were added to the so-obtained mixture of coarse and fine aggregates and mixed for another one minute to obtain a mixture. 165 kg of water was added followed by immediately adding 3.09 kg of admixture to the so-obtained mixture and mixed for 2 minutes to obtain a concrete composition. 1.32 kg of the non-aqueous graphene dispersion obtained in Example 1 was added and mixed for 1 minute to obtain a graphene reinforced composition (0.0005 mass% graphene with respect to the total mass of the concrete composition). The workability of the graphene reinforced composition was checked. The graphene reinforced composition was retained for 120 minutes followed by casting and curing at 27 °C for 24 hours to obtain a cured object.
Example 8
1215 kg of coarse aggregates (20 mm and 10 mm) aggregates were mixed with 759 kg of sand (fine aggregates) for 1 minute to obtain a mixture of coarse and fine aggregates. 330 kg of cement along with 90 kg of fly ash were added to the so-obtained mixture of coarse and fine aggregates and mixed for another one minute to obtain a mixture. 160 kg of water was added followed by immediately adding 2.5 kg of admixture to the so-obtained mixture and mixed for 2 minutes to obtain a concrete composition. 1.26 kg of the non-aqueous graphene dispersion obtained in Example 1 was added and mixed for 1 minute to obtain a graphene reinforced composition (0.0004 mass% graphene with respect to the total mass of the concrete composition).The workability of the graphene reinforced composition was checked. The graphene reinforced composition was retained for 120 minutes followed by casting and curing at 27 °C for 24 hours to obtain a cured object.
Example 9
993 kg of coarse aggregates (20 mm and 10 mm) aggregates were mixed with 749 kg of sand (fine aggregates) for 1 minute to obtain a mixture of coarse and fine aggregates. 386 kg of cement along with 129 kg of fly ash were added to the so-obtained mixture of coarse and fine aggregates and mixed for another one minute to obtain a mixture. 170 kg of water was added followed by immediately adding 3.09 kg of admixture to the so-obtained mixture and mixed for 2 minutes to obtain a concrete composition. 1.54 kg of the non-aqueous graphene dispersion obtained in Example 1 was added and mixed for 1 minute to obtain a graphene reinforced composition (0.0006 mass% graphene with respect to the total mass of the concrete composition). The workability of the graphene reinforced composition was checked. The concrete mixture was retained for 120 minutes followed by casting and curing at 27 °C for 24 hours to obtain a cured object.
Example 10
1148 kg of coarse aggregates (20 mm and 10 mm) aggregates were mixed with 698 kg of sand (fine aggregates) for 1 minute to obtain a mixture of coarse and fine aggregates. 340 kg of cement along with 85 kg of ground granulated blast-furnace slag (GGBS) were added to the so-obtained mixture of coarse and fine aggregates and mixed for another one minute to obtain a mixture. 189 kg of water was added followed by immediately adding 3.80 kg of admixture to the so-obtained mixture and mixed for 2 minutes to obtain a concrete composition. 1.27 kg of the non-aqueous graphene dispersion obtained in Example 1 was added and mixed for 1 minute to obtain a graphene reinforced composition (0.0005 mass% graphene with respect to the total mass of the concrete composition). The workability of the graphene reinforced composition was checked. The graphene reinforced composition was retained for 120 minutes followed by casting and curing at 27 °C for 24 hours to obtain a cured object.
Example 11
1241 kg of coarse aggregates (20 mm and 10 mm) aggregates were mixed with 740 kg of sand (fine aggregates) for 1 minute to obtain a mixture of coarse and fine aggregates. 360 kg of cement along with 90 kg of ground granulated blast-furnace slag (GGBS) were added to the so-obtained mixture of coarse and fine aggregates and mixed for another one minute to obtain a mixture. 138 kg of water was added followed by immediately adding 3.65 kg of admixture to the so-obtained mixture and mixed for 2 minutes to obtain a concrete composition. 1.35 kg of the non-aqueous graphene dispersion obtained in Example 1 was added and mixed for 1 minute to obtain a graphene reinforced composition (0.0005 mass% graphene with respect to the total mass of the concrete composition). The workability of the graphene reinforced composition was checked. The graphene reinforced composition was retained for 120 minutes followed by casting and curing at 27 °C for 24 hours to obtain a cured object.
Example 12
1218 kg of coarse aggregates (20 mm and 10 mm) aggregates were mixed with 812 kg of sand (fine aggregates) for 1 minute to obtain a mixture of coarse and fine aggregates. 440 kg of cement along with 60 kg of ground granulated blast-furnace slag (GGBS) were added to the so-obtained mixture of coarse and fine aggregates and mixed for another one minute to obtain a mixture. 130 kg of water was added followed by immediately adding 5 kg of admixture to the so-obtained mixture and mixed for 2 minutes to obtain a concrete composition. 5 kg of the non-aqueous graphene dispersion obtained in Example 1 was added and mixed for 1 minute to obtain a graphene reinforced composition (0.0018 mass% graphene with respect to the total mass of the concrete composition). The workability of the graphene reinforced composition was checked. The graphene reinforced composition was retained for 120 minutes followed by casting and curing at 27 °C for 24 hours to obtain a cured object.
Example 13
1199 kg of coarse aggregates (20 mm and 10 mm) aggregates were mixed with 730 kg of sand (fine aggregates) for 1 minute to obtain a mixture of coarse and fine aggregates. 450 kg of cement along with 50 kg of ground granulated blast-furnace slag (GGBS) were added to the so-obtained mixture of coarse and fine aggregates and mixed for another one minute to obtain a mixture. 160 kg of water was added followed by immediately adding 3.5 kg of admixture to the so-obtained mixture and mixed for 2 minutes to obtain a concrete composition. 5 kg of the non-aqueous dispersion obtained in Example 1 was added and mixed for 1 minute to obtain a graphene reinforced composition (0.0019 mass% graphene with respect to the total mass of the concrete composition). The workability of the graphene reinforced composition was checked. The graphene reinforced composition was retained for 120 minutes followed by casting and curing at 27 °C for 24 hours to obtain a cured object.
Example 14
1199 kg of coarse aggregates (20 mm and 10 mm) aggregates were mixed with 730 kg of sand (fine aggregates) for 1 minute to obtain a mixture of coarse and fine aggregates. 450 kg of cement along with 50 kg of ground granulated blast-furnace slag (GGBS) were added to the so-obtained mixture of coarse and fine aggregates and mixed for another one minute to obtain a mixture. 160 kg of water was added followed by immediately adding 3.5 kg of admixture to the so-obtained mixture and mixed for 2 minutes to obtain a concrete composition. 25 kg of the non-aqueous dispersion obtained in Example 2 was added and mixed for 1 minute to obtain a graphene reinforced composition (0.019 mass% graphene with respect to the total mass of the concrete composition). The workability of the graphene reinforced composition was checked. The graphene reinforced composition was retained for 120 minutes followed by casting and curing at 27 °C for 24 hours to obtain a cured object.
Comparative Example 1 (aqueous graphene dispersion)
1218 kg of coarse aggregates (20 mm and 10 mm) aggregates were mixed with 812 kg of sand (fine aggregates) for 1 minute to obtain a mixture of coarse and fine aggregates. 440 kg of cement along with 60 kg of ground granulated blast-furnace slag (GGBS) were added to the so-obtained mixture of coarse and fine aggregates and mixed for another one minute to obtain a mixture. 63 kg of water was added followed by immediately adding 5 kg of admixture to the so-obtained mixture and mixed for 2 minutes to obtain a concrete composition. 5 kg of the aqueous graphene dispersion was added in 61 kg of water and mixed in so obtained concrete composition for 1 minute to obtain a graphene reinforced composition (0.002 mass% graphene with respect to the total mass of the concrete composition). The workability of the graphene reinforced composition was checked. The graphene reinforced composition was retained for 120 minutes followed by casting and curing at 27 °C for 24 hours to obtain a cured object.
Comparative Example 2 (concrete composition without graphene)
1218 kg of coarse aggregates (20 mm and 10 mm) aggregates were mixed with 812 kg of sand (fine aggregates) for 1 minute to obtain a mixture of coarse and fine aggregates. 440 kg of cement along with 60 kg of ground granulated blast-furnace slag (GGBS) were added to the so-obtained mixture of coarse and fine aggregates and mixed for another one minute to obtain a mixture. 130 kg of water was added followed by immediately adding 5 kg of admixture to the so-obtained mixture and mixed for 2 minutes to obtain a concrete composition. The concrete composition was retained for 120 minutes followed by casting and curing at 27 °C for 24 hours to obtain a cured object.
EXPERIMENT 2: Functional analysis of the graphene reinforced concrete composition
The cured object of the present disclosure when compared to the conventional concrete of Comparative Example 2 exhibited improvement in the functional properties. The cured object of the present disclosure exhibited:
• compressive strength in the range of 10% to 45% greater than the compressive strength of a conventional concrete which is in the range of 40 N/mm2 to 47 N/mm2;
• flexural strength in the range of 10% to 40% greater than the flexural strength of a conventional concrete which is in the range of 4 N/mm2 to 7 N/mm2;
• split tensile strength in the range of 5% to 45% greater than the split tensile strength of a conventional concrete which is in the range of 2 N/mm2 to 5 N/mm2;
• chloride ingress in the range of 40% to 90% less than the chloride ingress of a convention concrete which is in the range of 9 x 10-12 m2 s-1 to 13 x 10-12 m2 s-1 ;
• water permeability in the range of 40% to 90% less than the water permeability of a conventional concrete which is in the range of 14 mm to 18 mm;
• acid resistance (strength loss) in the range of 40% to 50% more than the acid resistance of a conventional concrete in which strength loss is in the range of 8% to 35%; and
• sulphate resistance (length change) in the range of 80% to 85% more than the sulphate resistance of a conventional concrete in which the length change is in the range of 0.012% to 0.07%.
A comparison with respect to the functional performance of the cured object of the present disclosure was done to analyse the impact of the amount of graphene, post quick curing, on the properties such as compressive strength, flexural strength, split tensile strength, water permeability, rapid chloride migration test (RCMT), acid resistance strength (strength loss), and sulphate resistance (length change).
The results are summarized in Table 2.

Example Concentration of Graphene in mass% wrt total reinforced concrete Concentration of Graphene in total concrete (ppm) Compressive strength (N/mm2) (percentage increase) Flexural strength (N/mm2) (percentage increase) Split tensile strength (N/mm2) (percentage increase) Water permeability (mm) (percentage reduction) Rapid Chloride Migration Test (RCMT) (10-12 m2s-1) (percentage reduction Acid resistance (strength loss %) Sulphate Resistance
(Length Change%)
Comparative Example 2 (type II concrete composition) (Control) 0 0 43.4 5.67 3.24 16 11.06 20.63 0.026
Comparative Example 1 0.002 20 47.2 (8.75%) 5.87 (3.53%) 3.43 (5.86%) 13 (18.75%) 9.97 (9.85%) 16.87 0.012
Example 12
(present disclosure) 0.002 20 52.13 (20.11%) 7.74 (36.51%) 3.5 (8.02%)
9 (43.75%) 6.6 (40.33%) 15.02 0.009
Example 14
(present disclosure) 0.019 190 62.93 (45%) 8 (41.09%) 4.6 (41.9%) 1.7 (89.3%) 1.2 (89.15%) 9.26 0.004
Table 2: Results of the functional analysis of cured object of the present disclosure with conventional concrete composition (type II)


Form Table 2 it is observed that varying concentrations of graphene affect material properties such as compressive strength, flexural strength, split tensile strength, water permeability, chloride migration resistance, and acid resistance. A significant improvement as graphene concentration increases was observed. The highest strength (62.93 N/mm², a 45% increase) is observed at the highest graphene concentration (0.02 mass%). Consistent improvement in Flexural strength was also observed, with the most substantial increase (41.09%) at 0.02 mass%. Similar trends were observed for the split tensile strength. A moderate increase across all graphene concentrations, with the highest (41.9%) at 0.02 mass% was observed.
A noticeable reduction in water permeability was observed as graphene concentration increased. The maximum reduction (89.3%) occurred at 0.02 mass% graphene, indicating graphene's effectiveness in improving impermeability. Chloride ion permeability decreased substantially with higher graphene concentrations. At 0.02 mass% graphene, there was an 89.15% reduction, highlighting graphene's ability to enhance resistance against chloride-induced degradation. The strength loss due to acid was reduced with increasing graphene concentration. The strength loss drop was from 20.63% (control) to 9.26% (0.02 mass% graphene), reflecting graphene's potential in corrosive environments. From the results it is also evident that the graphene reinforced concrete composition of the present disclosure will give the same results/improvements over any type of conventional concrete composition/material.
EXPERIMENT 3: Comparison of non-aqueous (MEG) based graphene dispersion with aqueous graphene dispersion.
Strength studies
The graphene reinforced concrete composition in accordance with Example 13 of the present disclosure was compared with graphene reinforced concrete composition having graphene dispersed in an aqueous solution obtained in Comparative Example 2. In comparison to the water-based graphene dispersion, MEG based dispersion revealed superior performance when used to prepare the concrete composition. The functional performance of a graphene reinforced concrete composition obtained in Example 13 was evaluated to understand the impact of solvent on the properties of flexural strength, compressive strength and split tensile strength. The results of the comparative study after 7 days of curing are summarized in Table 3.
Table 3: Effect of solvent on the properties of the cured object after 7 days of curing.
Property
Comparative Example 1 (Aqueous graphene dispersion)
Comparative Example 2
(Control) Example 13 in accordance with the present disclosure
Flexural strength (MPa) 5.57 (21%) 4.57 6.40 (40%)
Compressive strength (MPa) 45.73 (5.36%) 43.40 51.77 (19.28%)
Split tensile strength (MPa) 3.30 (2%) 3.24 3.50 (8.02%)
From Table 3, a substantial improvement is observed in both examples, with Example 13 showing nearly double the percentage increase compared to Comparative Example 2. This indicated that there is a significant enhancement in the flexural strength of the cured object of the present disclosure. A modest improvement in compressive strength was seen in Comparative Example 2, but Example 13 demonstrated a notable enhancement of around four times the percentage increase. This suggested that the disclosed methodology yields a stronger material under compressive loads. A similar trend was observed in split tensile strength. Marginal improvement was observed in Comparative Example 2, whereas Example 13 shows a meaningful boost in tensile strength. Highlights the potential of the present disclosure to enhance performance under tensile stress.
Processability
MEG based graphene dispersion provided much better processability of concrete compared to water-based graphene dispersion. Generally, admixture covers all cement particles for the retention period, so that concrete remains in plastic stage. But due to addition of water-based graphene dispersion in concrete, it immediately accelerates cement hydration process in retention period itself resulting in drop in retention period. After the retention period is over the concrete is not processable anymore. Whereas MEG based graphene dispersion actually remains inactive for longer duration in concrete, afterwards accelerates cement hydration process. Hence, much better retention period and improved processability is obtained in case of MEG-based graphene dispersion. Moreover, slump height can be managed by extra admixture dosages in case of MEG-based graphene dispersion which is not possible for water-based graphene Ink. In case of water-based graphene dispersion after adding graphene, hydration starts, so even addition the admixture to maintain slump height, does not work. Whereas in case of MEG-based dispersion hydration did not start immediately after addition of the dispersion. So admixture can be added if required, to maintain the slump height.
The major reason of not using water-based dispersions is due to user demand of handling concrete. Generally concrete needs to be transported from batching plant to site, so handling period is needed before placing of concrete. Depending on site distance and workability requirement, higher retention period is required. As MEG based graphene dispersion does not affect any workability parameters of concrete and market can easily adopt Graphene dispersion without compromising initial plasticity. Table 4 summarizes the comparison of retention time of concrete material with water-based dispersion and concrete material with MEG based dispersion.
Table 4: the comparison of retention time of concrete material with water-based dispersion and concrete material with MEG based dispersion.
Example Retention time
Comparative Example 2(Control) 2 hours
Comparative Example 1 (aqueous dispersion) 30 minutes
Example 13 (present disclosure) 2 hrs

The non-aqueous graphene dispersion of the present disclosure does not affect the workability of the concrete when compared to the control (Comparative Example 1). In contrast, water-based graphene dispersions accelerate the cement hydration process, resulting in a significantly reduced retention time. Once the retention period ends, the concrete becomes unworkable. The combination of graphene with a non-aqueous solvent, such as MEG, offers excellent performance, significantly enhancing flexural strength, compressive strength, and tensile strength, while also improving retention time.
Ease of operation
In case of water-based graphene dispersions, due to presence of water in the graphene dispersion, overall, WC (Water cement Ratio) got disturbed. Each time water content correction was required based on Graphene dispersion dosages. In MEG-based Graphene dispersion, no WC ratio changes occurred and hence no such correction was required. Therefore, without affecting the existing concrete-making process the addition of the MEG based dispersion can be easily done. It makes the overall process much easier.
TECHNICAL ADVANCEMNT
The present disclosure described hereinabove has several technical advantages including, but not limited to, the realization of:
- a graphene reinforced concrete material, that:
• exhibits improvement in compressive strength, flexural strength, split tensile strength;
• exhibits reduced chloride ingress and permeability to water;
• exhibits reduced steel rebar corrosion and consequent enhancement in durability and lifespan;
• exhibits enhanced acid resistance;
• exhibits reduced hydration time; and
• does not affect the workability and processability,
- and a process for the preparation of a graphene reinforced concrete material that:
• is simple and efficient.
Throughout this specification the word “comprises,” or variations such as “comprises” or “comprising, will be understood to imply the inclusion of a stated element, integer or step,” or group of elements, integers, or steps, but not the exclusion of any other element, integer or step, or group of elements, integers, or steps.
The use of the expression “at least” or “at least one” suggests the use of one or more elements or ingredients or quantities, as the use may be in the embodiment of the invention to achieve one or more of the desired objects or results. While certain embodiments of the inventions have been described, these embodiments have been presented by way of example only and are not intended to limit the scope of the inventions. Variations or modifications to the formulation of this invention, within the scope of the invention, may occur to those skilled in the art upon reviewing the disclosure herein. Such variations or modifications are well within the spirit of this invention.
The numerical values given for various physical parameters, dimensions and quantities are only approximate values and it is envisaged that the values higher than the numerical value assigned to the physical parameters, dimensions and quantities fall within the scope of the invention unless there is a statement in the specification to the contrary.
While considerable emphasis has been placed herein on the specific features of the preferred embodiment, it will be appreciated that many additional features can be added and that many changes can be made in the preferred embodiment without departing from the principles of the disclosure. These and other changes in the preferred embodiment of the disclosure will be apparent to those skilled in the art from the disclosure herein, whereby it is to be distinctly understood that the foregoing descriptive matter is to be interpreted merely as illustrative of the disclosure and not as a limitation. ,CLAIMS:WE CLAIM:
1. A graphene reinforced composition comprising:
a. a concrete composition; and
b. a non-aqueous graphene dispersion,
wherein said non-aqueous graphene dispersion is uniformly distributed in said concrete composition; and the amount of graphene is in the range of 0.0002 mass% to 0.02 mass% with respect to the total mass of said concrete composition.
2. The reinforced composition as claimed in claim 1, wherein said non-aqueous dispersion is a homogeneous mixture of a graphene material dispersed in a non-aqueous fluid medium optionally with a surfactant.
3. The reinforced composition as claimed in claim 2, wherein said non-aqueous fluid medium is selected from the group consisting of monoethylene glycol (MEG), diethylene glycol (DEG), polyvinyl alcohol (PVA), ethanol and propanol.
4. The reinforced composition as claimed in claim 1, wherein said concrete composition comprises cement, coarse aggregates, fine aggregates, fly ash and optionally ground granulated blast-furnace slag (GGBS).
5. The reinforced composition as claimed in claim 2, wherein said surfactant is at least one selected from the group consisting of cellulose, polyvinyl pyrrolidone (PVP), polycarboxylate ether, polyethylene oxide, dodecyl sulfate, lauryl sulfate, cetyltrimethylammonium bromide, polyethylene oxide and alkyl phenol ethoxylate.
6. The reinforced composition as claimed in claim 2, wherein said graphene material is at least one selected from the group consisting of graphene, graphene oxide, reduced graphene oxide, graphene nano ribbons, graphene quantum dots and doped graphene.
7. The reinforced composition as claimed in claim 6, wherein said graphene comprises 70% to 85% of a single layer graphene and 15% to 30% of a multilayer graphene.
8. The reinforced composition as claimed in claim 7, wherein said multilayer graphene comprises two-layer graphene, three-layer graphene, four-layer graphene, five-layer graphene and any combination thereof.
9. The reinforced composition as claimed in claim 1, exhibits at least one of the following properties:
• compressive strength in the range of 10% to 45% greater than the compressive strength of conventional concrete which is in the range of 20 N/mm2 to 115 N/mm2;
• flexural strength in the range of 10% to 40% greater than the flexural strength of conventional concrete which is in the range of 2 N/mm2 to 10 N/mm2;
• split tensile strength in the range of 5% to 45% greater than the split tensile strength of conventional concrete which is in the range of 1.5 N/mm2 to 8 N/mm2;
• chloride ingress in the range of 40% to 90% less than the chloride ingress of conventional concrete which is in the range of 3 x 10-12 m2 s-1 to 18 x 10-12 m2 s-1 ;
• water permeability in the range of 40% to 90% less than the water permeability of conventional concrete which is in the range of 2 mm to 30 mm;
• acid resistance (strength loss) in the range of 40% to 50% more than the acid resistance of conventional concrete in which strength loss is in the range of 8% to 35%; and
• sulphate resistance (length change) in the range of 80% to 85% more than the sulphate resistance of conventional concrete in which the length change is in the range of 0.012% to 0.07%.

10. A process for the preparation of a graphene reinforced composition, said process comprising the following steps:
a) mixing predetermined amounts of a graphene material, a non-aqueous fluid medium, and optionally a surfactant at a speed in the range of 100 rpm to 10000 rpm for a first predetermined time period to obtain a non-aqueous graphene dispersion; and
b) mixing said non-aqueous graphene dispersion to a concrete composition for a second predetermined time period to obtain said graphene reinforced composition.
11. The process as claimed in claim 10, wherein said concrete composition comprises cement, coarse aggregates, fine aggregates, fly ash, and optionally ground granulated blast-furnace slag (GGBS), and an admixture.
12. The process as claimed in claim 10, wherein said surfactant is at least one selected from the group consisting of cellulose, polyvinyl pyrrolidone (PVP), polycarboxylate ether, polyethylene oxide, dodecyl sulfate, lauryl sulfate, cetyltrimethylammonium bromide, polyethylene oxide and alkyl phenol ethoxylate.
13. The process as claimed in claim 10, wherein said non-aqueous fluid medium is at least one selected from the group consisting of monoethylene glycol (MEG), diethylene glycol (DEG), polyvinyl alcohol (PVA), ethanol and propanol.
14. The process as claimed in claim 10, wherein said graphene material is at least one selected from the group consisting of graphene, graphene oxide, reduced graphene oxide, graphene nanoribbons, graphene quantum dots and doped graphene.
15. The process as claimed in claim 14, wherein said graphene comprises 70% to 85% single layer graphene and 15% to 30% multilayer graphene.
16. The process as claimed in claim 10, wherein said first predetermined time period is in the range of 2 hours to 5 hours.
17. The process as claimed in claim 10, wherein said predetermined temperature is in the range of 20 °C to 40 °C.
18. The process as claimed in claim 10, wherein said second predetermined time period is in the range of 20 hours to 30 hours.
19. The process as claimed in claim 10, wherein said predetermined amount of said graphene material is in the range of 0.001 mass% to 2 mass% with respect to the total mass of said non-aqueous graphene dispersion.
20. The process as claimed in claim 10, wherein said predetermined amount of non-aqueous fluid medium is in the range of 55 mass% to 99.5 mass% with respect to the total mass of said non-aqueous graphene dispersion.
21. The process as claimed in claim 10, wherein said predetermined amount of surfactant is in the range of 0 mass% to 45 mass% to the total mass of said non-aqueous graphene dispersion.
22. The process as claimed in claim 10, wherein said graphene reinforced composition is retained for a predetermined retention period followed by casting and curing at a predetermined temperature for a second predetermined time period to obtain a cured object.
23. The process as claimed in claim 22, wherein said predetermined retention period is in the range of 30 minutes to 150 minutes.
24. The process as claimed in claim 10, wherein said graphene reinforced composition is casted and cured at a temperature in the range of 20 °C to 40 °C to obtain said cured object.
Dated this 30th Day of January 2025

_______________________________
MOHAN RAJKUMAR DEWAN, IN/PA – 25
OF R. K. DEWAN & CO.
AUTHORIZED AGENT OF APPLICANT

Documents

Application Documents

# Name Date
1 202421006157-STATEMENT OF UNDERTAKING (FORM 3) [30-01-2024(online)].pdf 2024-01-30
2 202421006157-PROVISIONAL SPECIFICATION [30-01-2024(online)].pdf 2024-01-30
3 202421006157-PROOF OF RIGHT [30-01-2024(online)].pdf 2024-01-30
4 202421006157-FORM 1 [30-01-2024(online)].pdf 2024-01-30
5 202421006157-DECLARATION OF INVENTORSHIP (FORM 5) [30-01-2024(online)].pdf 2024-01-30
6 202421006157-FORM-26 [31-01-2024(online)].pdf 2024-01-31
7 202421006157-Proof of Right [22-02-2024(online)].pdf 2024-02-22
8 202421006157-MARKED COPIES OF AMENDEMENTS [15-11-2024(online)].pdf 2024-11-15
9 202421006157-FORM 13 [15-11-2024(online)].pdf 2024-11-15
10 202421006157-AMMENDED DOCUMENTS [15-11-2024(online)].pdf 2024-11-15
11 202421006157-FORM-5 [30-01-2025(online)].pdf 2025-01-30
12 202421006157-FORM 18 [30-01-2025(online)].pdf 2025-01-30
13 202421006157-ENDORSEMENT BY INVENTORS [30-01-2025(online)].pdf 2025-01-30
14 202421006157-COMPLETE SPECIFICATION [30-01-2025(online)].pdf 2025-01-30
15 202421006157-Request Letter-Correspondence [30-05-2025(online)].pdf 2025-05-30
16 202421006157-Power of Attorney [30-05-2025(online)].pdf 2025-05-30
17 202421006157-Covering Letter [30-05-2025(online)].pdf 2025-05-30