Patent
US 10,052,302GREEN SYNTHESIS OF REDUCED GRAPHENE OXIDE SILICA NANOCOMPOSITE USING NIGELLA SATIVA SEEDS EXTRACT
MANAL AHMED GASMELSEED AWAD, AMEL LAREF
US
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US 10,052,302Patent drawings and their descriptions. Click a drawing to enlarge it.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A method of green synthesis of a reduced graphene oxide (rG O) silica (SiO 2) nanocomposite, comprising the sequential steps of: m ixing a quantity of soot in an acid while stirring to obtain a solution; adding a first oxidant gradually into the solution to oxidize the soot and obtain a first suspension; stirring the first suspension while maintaining a temperature of the suspension at about 35°C; adding Nigella sativa seed extract to the first suspension while raising the temperature of the suspension to about 60 0 C; adding a second oxidant to the suspension to form [[the]] reduced graphene oxide nanoparticles; isolating the formed reduced graphene oxide nanoparticles by centrifugation; suspending the reduced graphene oxide nanoparticles in water to form a second suspension; ultrasonicating the second suspension for about 60 minutes; centrifuging the second suspension at about 3000 rpm to remove any aggregates; adding a solution comprising tetraethyl orthosilicate (TE O S), concentrated aqueous ammonia solution and Nigella sativa seed extract under ultrasonication conditions to the second suspension to obtain a third suspension; increasing the temperature of the third suspension to about 90 ° C while stirring gradually for about 3 hours to form reduced graphene oxide-silicon dioxide nanocomposite suspension; and isolating the reduced graphene oxide-silicon dioxide nanocomposite by filtration. Currently amended
The method of green synthesis of a reduced graphene oxide (rGO) silica (Si O₂) nanocomposite according to claim 1, further comprising the steps of washing the graphene oxide-silicon dioxide nanocomposite suspension with water and drying the suspension at about 70°C. Original
The method of green synthesis of a reduced graphene oxide (rGO) silica (Si O₂) nanocomposite according to claim 1, wherein the acid is sulfuric acid. Original
The method of green synthesis of a reduced graphene oxide (rGO) silica (Si O₂) nanocomposite according to claim 1, wherein the first oxidant is potassium permanganate. Original
The method of green synthesis of a reduced graphene oxide (rGO) silica (SiO₂) nanocomposite according to claim 1, wherein the s e cond oxidant is hydrogen peroxide. Original
The method of green synthesis of a reduced graphene oxide (rGO) silica (SiO₂) nanocomposite according to claim 1, wherein adding the Nigella sa l iva seed extract is performed at a temperature of the suspension of about 60 ° C for about 15 minutes. Original
A reduced graphene oxide silica nanocomposite produced according to the method of claim 1. Withdrawn
A method of inhibiting the growth or proliferation of a cancer cell, comprising the step of contacting the cancer cell with an effective amount of the reduced graphene oxide- silica nanoparticles synthesized according to the method of claim 1. Withdrawn
Canceled
Embodiments described in the patent, grouped by the materials and process steps they use.
1 material1 process step
Preparation of extract from Nigella sativa seeds: seeds were washed with distilled water, about 30 grams of coarsely ground seeds were boiled in 150 mL of double distilled water for about 5 minutes, then centrifuged and filtered. The filtrate was collected and stored at 4°C until further use.
7 materials1 process step
Green synthesis of reduced graphene oxide (rGO) nanoparticles: soot was mixed in sulfuric acid with stirring; potassium permanganate was added gradually to oxidize the soot; the suspension was stirred at ~35°C; Nigella sativa seed extract was added while raising temperature to ~60°C for ~15 minutes; hydrogen peroxide was added to form rGO nanoparticles; nanoparticles were isolated by centrifugation; suspended in water; ultrasonicated for ~60 minutes; centrifuged at ~3000 rpm to remove aggregates. TEOS, concentrated aqueous ammonia solution, and Nigella sativa seed extract were added under ultrasonication to form a third suspension; temperature raised to ~90°C while stirring for ~3 hours to form rGO-SiO₂ nanocomposite suspension; isolated by filtration; washed with water and dried at ~70°C.
Materials described outside the worked examples.
concentrated aqueous ammonia solution
NH₃(aq)
reduced graphene oxide nanoparticles
Measurements and analyses referenced in the patent, with their drawing references.
X-ray diffraction pattern of green synthesized reduced graphene oxide/SiO₂ nanocomposite nanoparticles using Nigella sativa seed extract (Fig. 2)
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
mean diameter range (claim) | 1–500 nm | reduced graphene oxide-silica nanocomposite |
mean diameter range of rGO nanoparticles (description) | 5–100 nm |
Patent
Atlas literature
Patent
US 10,052,302Patent drawings and their descriptions. Click a drawing to enlarge it.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A method of green synthesis of a reduced graphene oxide (rG O) silica (SiO 2) nanocomposite, comprising the sequential steps of: m ixing a quantity of soot in an acid while stirring to obtain a solution; adding a first oxidant gradually into the solution to oxidize the soot and obtain a first suspension; stirring the first suspension while maintaining a temperature of the suspension at about 35°C; adding Nigella sativa seed extract to the first suspension while raising the temperature of the suspension to about 60 0 C; adding a second oxidant to the suspension to form [[the]] reduced graphene oxide nanoparticles; isolating the formed reduced graphene oxide nanoparticles by centrifugation; suspending the reduced graphene oxide nanoparticles in water to form a second suspension; ultrasonicating the second suspension for about 60 minutes; centrifuging the second suspension at about 3000 rpm to remove any aggregates; adding a solution comprising tetraethyl orthosilicate (TE O S), concentrated aqueous ammonia solution and Nigella sativa seed extract under ultrasonication conditions to the second suspension to obtain a third suspension; increasing the temperature of the third suspension to about 90 ° C while stirring gradually for about 3 hours to form reduced graphene oxide-silicon dioxide nanocomposite suspension; and isolating the reduced graphene oxide-silicon dioxide nanocomposite by filtration. Currently amended
The method of green synthesis of a reduced graphene oxide (rGO) silica (Si O₂) nanocomposite according to claim 1, further comprising the steps of washing the graphene oxide-silicon dioxide nanocomposite suspension with water and drying the suspension at about 70°C. Original
The method of green synthesis of a reduced graphene oxide (rGO) silica (Si O₂) nanocomposite according to claim 1, wherein the acid is sulfuric acid. Original
The method of green synthesis of a reduced graphene oxide (rGO) silica (Si O₂) nanocomposite according to claim 1, wherein the first oxidant is potassium permanganate. Original
The method of green synthesis of a reduced graphene oxide (rGO) silica (SiO₂) nanocomposite according to claim 1, wherein the s e cond oxidant is hydrogen peroxide. Original
The method of green synthesis of a reduced graphene oxide (rGO) silica (SiO₂) nanocomposite according to claim 1, wherein adding the Nigella sa l iva seed extract is performed at a temperature of the suspension of about 60 ° C for about 15 minutes. Original
A reduced graphene oxide silica nanocomposite produced according to the method of claim 1. Withdrawn
A method of inhibiting the growth or proliferation of a cancer cell, comprising the step of contacting the cancer cell with an effective amount of the reduced graphene oxide- silica nanoparticles synthesized according to the method of claim 1. Withdrawn
Canceled
Embodiments described in the patent, grouped by the materials and process steps they use.
1 material1 process step
Preparation of extract from Nigella sativa seeds: seeds were washed with distilled water, about 30 grams of coarsely ground seeds were boiled in 150 mL of double distilled water for about 5 minutes, then centrifuged and filtered. The filtrate was collected and stored at 4°C until further use.
7 materials1 process step
Green synthesis of reduced graphene oxide (rGO) nanoparticles: soot was mixed in sulfuric acid with stirring; potassium permanganate was added gradually to oxidize the soot; the suspension was stirred at ~35°C; Nigella sativa seed extract was added while raising temperature to ~60°C for ~15 minutes; hydrogen peroxide was added to form rGO nanoparticles; nanoparticles were isolated by centrifugation; suspended in water; ultrasonicated for ~60 minutes; centrifuged at ~3000 rpm to remove aggregates. TEOS, concentrated aqueous ammonia solution, and Nigella sativa seed extract were added under ultrasonication to form a third suspension; temperature raised to ~90°C while stirring for ~3 hours to form rGO-SiO₂ nanocomposite suspension; isolated by filtration; washed with water and dried at ~70°C.
Materials described outside the worked examples.
concentrated aqueous ammonia solution
NH₃(aq)
reduced graphene oxide nanoparticles
Measurements and analyses referenced in the patent, with their drawing references.
X-ray diffraction pattern of green synthesized reduced graphene oxide/SiO₂ nanocomposite nanoparticles using Nigella sativa seed extract (Fig. 2)
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
mean diameter range (claim) | 1–500 nm | reduced graphene oxide-silica nanocomposite |
mean diameter range of rGO nanoparticles (description) | 5–100 nm |
Patent
Atlas literature
Patent
US 10,052,302Patent drawings and their descriptions. Click a drawing to enlarge it.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A method of green synthesis of a reduced graphene oxide (rG O) silica (SiO 2) nanocomposite, comprising the sequential steps of: m ixing a quantity of soot in an acid while stirring to obtain a solution; adding a first oxidant gradually into the solution to oxidize the soot and obtain a first suspension; stirring the first suspension while maintaining a temperature of the suspension at about 35°C; adding Nigella sativa seed extract to the first suspension while raising the temperature of the suspension to about 60 0 C; adding a second oxidant to the suspension to form [[the]] reduced graphene oxide nanoparticles; isolating the formed reduced graphene oxide nanoparticles by centrifugation; suspending the reduced graphene oxide nanoparticles in water to form a second suspension; ultrasonicating the second suspension for about 60 minutes; centrifuging the second suspension at about 3000 rpm to remove any aggregates; adding a solution comprising tetraethyl orthosilicate (TE O S), concentrated aqueous ammonia solution and Nigella sativa seed extract under ultrasonication conditions to the second suspension to obtain a third suspension; increasing the temperature of the third suspension to about 90 ° C while stirring gradually for about 3 hours to form reduced graphene oxide-silicon dioxide nanocomposite suspension; and isolating the reduced graphene oxide-silicon dioxide nanocomposite by filtration. Currently amended
The method of green synthesis of a reduced graphene oxide (rGO) silica (Si O₂) nanocomposite according to claim 1, further comprising the steps of washing the graphene oxide-silicon dioxide nanocomposite suspension with water and drying the suspension at about 70°C. Original
The method of green synthesis of a reduced graphene oxide (rGO) silica (Si O₂) nanocomposite according to claim 1, wherein the acid is sulfuric acid. Original
The method of green synthesis of a reduced graphene oxide (rGO) silica (Si O₂) nanocomposite according to claim 1, wherein the first oxidant is potassium permanganate. Original
The method of green synthesis of a reduced graphene oxide (rGO) silica (SiO₂) nanocomposite according to claim 1, wherein the s e cond oxidant is hydrogen peroxide. Original
The method of green synthesis of a reduced graphene oxide (rGO) silica (SiO₂) nanocomposite according to claim 1, wherein adding the Nigella sa l iva seed extract is performed at a temperature of the suspension of about 60 ° C for about 15 minutes. Original
A reduced graphene oxide silica nanocomposite produced according to the method of claim 1. Withdrawn
A method of inhibiting the growth or proliferation of a cancer cell, comprising the step of contacting the cancer cell with an effective amount of the reduced graphene oxide- silica nanoparticles synthesized according to the method of claim 1. Withdrawn
Canceled
Embodiments described in the patent, grouped by the materials and process steps they use.
1 material1 process step
Preparation of extract from Nigella sativa seeds: seeds were washed with distilled water, about 30 grams of coarsely ground seeds were boiled in 150 mL of double distilled water for about 5 minutes, then centrifuged and filtered. The filtrate was collected and stored at 4°C until further use.
7 materials1 process step
Green synthesis of reduced graphene oxide (rGO) nanoparticles: soot was mixed in sulfuric acid with stirring; potassium permanganate was added gradually to oxidize the soot; the suspension was stirred at ~35°C; Nigella sativa seed extract was added while raising temperature to ~60°C for ~15 minutes; hydrogen peroxide was added to form rGO nanoparticles; nanoparticles were isolated by centrifugation; suspended in water; ultrasonicated for ~60 minutes; centrifuged at ~3000 rpm to remove aggregates. TEOS, concentrated aqueous ammonia solution, and Nigella sativa seed extract were added under ultrasonication to form a third suspension; temperature raised to ~90°C while stirring for ~3 hours to form rGO-SiO₂ nanocomposite suspension; isolated by filtration; washed with water and dried at ~70°C.
Materials described outside the worked examples.
concentrated aqueous ammonia solution
NH₃(aq)
reduced graphene oxide nanoparticles
Measurements and analyses referenced in the patent, with their drawing references.
X-ray diffraction pattern of green synthesized reduced graphene oxide/SiO₂ nanocomposite nanoparticles using Nigella sativa seed extract (Fig. 2)
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
mean diameter range (claim) | 1–500 nm | reduced graphene oxide-silica nanocomposite |
mean diameter range of rGO nanoparticles (description) | 5–100 nm |
Patent
Atlas literature
Patent
US 10,052,302Patent drawings and their descriptions. Click a drawing to enlarge it.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A method of green synthesis of a reduced graphene oxide (rG O) silica (SiO 2) nanocomposite, comprising the sequential steps of: m ixing a quantity of soot in an acid while stirring to obtain a solution; adding a first oxidant gradually into the solution to oxidize the soot and obtain a first suspension; stirring the first suspension while maintaining a temperature of the suspension at about 35°C; adding Nigella sativa seed extract to the first suspension while raising the temperature of the suspension to about 60 0 C; adding a second oxidant to the suspension to form [[the]] reduced graphene oxide nanoparticles; isolating the formed reduced graphene oxide nanoparticles by centrifugation; suspending the reduced graphene oxide nanoparticles in water to form a second suspension; ultrasonicating the second suspension for about 60 minutes; centrifuging the second suspension at about 3000 rpm to remove any aggregates; adding a solution comprising tetraethyl orthosilicate (TE O S), concentrated aqueous ammonia solution and Nigella sativa seed extract under ultrasonication conditions to the second suspension to obtain a third suspension; increasing the temperature of the third suspension to about 90 ° C while stirring gradually for about 3 hours to form reduced graphene oxide-silicon dioxide nanocomposite suspension; and isolating the reduced graphene oxide-silicon dioxide nanocomposite by filtration. Currently amended
The method of green synthesis of a reduced graphene oxide (rGO) silica (Si O₂) nanocomposite according to claim 1, further comprising the steps of washing the graphene oxide-silicon dioxide nanocomposite suspension with water and drying the suspension at about 70°C. Original
The method of green synthesis of a reduced graphene oxide (rGO) silica (Si O₂) nanocomposite according to claim 1, wherein the acid is sulfuric acid. Original
The method of green synthesis of a reduced graphene oxide (rGO) silica (Si O₂) nanocomposite according to claim 1, wherein the first oxidant is potassium permanganate. Original
The method of green synthesis of a reduced graphene oxide (rGO) silica (SiO₂) nanocomposite according to claim 1, wherein the s e cond oxidant is hydrogen peroxide. Original
The method of green synthesis of a reduced graphene oxide (rGO) silica (SiO₂) nanocomposite according to claim 1, wherein adding the Nigella sa l iva seed extract is performed at a temperature of the suspension of about 60 ° C for about 15 minutes. Original
A reduced graphene oxide silica nanocomposite produced according to the method of claim 1. Withdrawn
A method of inhibiting the growth or proliferation of a cancer cell, comprising the step of contacting the cancer cell with an effective amount of the reduced graphene oxide- silica nanoparticles synthesized according to the method of claim 1. Withdrawn
Canceled
Embodiments described in the patent, grouped by the materials and process steps they use.
1 material1 process step
Preparation of extract from Nigella sativa seeds: seeds were washed with distilled water, about 30 grams of coarsely ground seeds were boiled in 150 mL of double distilled water for about 5 minutes, then centrifuged and filtered. The filtrate was collected and stored at 4°C until further use.
7 materials1 process step
Green synthesis of reduced graphene oxide (rGO) nanoparticles: soot was mixed in sulfuric acid with stirring; potassium permanganate was added gradually to oxidize the soot; the suspension was stirred at ~35°C; Nigella sativa seed extract was added while raising temperature to ~60°C for ~15 minutes; hydrogen peroxide was added to form rGO nanoparticles; nanoparticles were isolated by centrifugation; suspended in water; ultrasonicated for ~60 minutes; centrifuged at ~3000 rpm to remove aggregates. TEOS, concentrated aqueous ammonia solution, and Nigella sativa seed extract were added under ultrasonication to form a third suspension; temperature raised to ~90°C while stirring for ~3 hours to form rGO-SiO₂ nanocomposite suspension; isolated by filtration; washed with water and dried at ~70°C.
Materials described outside the worked examples.
concentrated aqueous ammonia solution
NH₃(aq)
reduced graphene oxide nanoparticles
Measurements and analyses referenced in the patent, with their drawing references.
X-ray diffraction pattern of green synthesized reduced graphene oxide/SiO₂ nanocomposite nanoparticles using Nigella sativa seed extract (Fig. 2)
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
mean diameter range (claim) | 1–500 nm | reduced graphene oxide-silica nanocomposite |
mean diameter range of rGO nanoparticles (description) | 5–100 nm |
Particle size distribution of green synthesized reduced graphene oxide/SiO₂ nanocomposite using Nigella sativa seed extract (Fig. 3)
Transmission electron micrographs of reduced graphene oxide decorated with SiO₂ nanocomposite using Nigella sativa seed extract (Figs. 4A and 4B)
Scanning electron micrograph of green synthesized reduced graphene oxide decorated with SiO₂ nanocomposite using Nigella sativa seed extract (Fig. 5)
EDS pattern of green synthesized reduced graphene oxide nanoparticles using Nigella sativa seed extract showing four dominant peaks for boron, carbon, oxygen and silicon atoms (Fig. 6)
Cytotoxic activity of reduced graphene oxide/SiO₂ nanocomposite synthesized from Nigella sativa seed extract against breast carcinoma cells (MCF-7 cell line) (Fig. 7)
Cytotoxic activity of reduced graphene oxide SiO₂ nanocomposite synthesized from Nigella sativa seed extract against Hepatocellular carcinoma cells (HepG-2 cell line) (Fig. 8)
reduced graphene oxide nanoparticles |
Thickness | ≥ 5 nm | — |
Thickness | 1–100 nm | — |
Thickness | 20–30 cm | — |
Particle size distribution of green synthesized reduced graphene oxide/SiO₂ nanocomposite using Nigella sativa seed extract (Fig. 3)
Transmission electron micrographs of reduced graphene oxide decorated with SiO₂ nanocomposite using Nigella sativa seed extract (Figs. 4A and 4B)
Scanning electron micrograph of green synthesized reduced graphene oxide decorated with SiO₂ nanocomposite using Nigella sativa seed extract (Fig. 5)
EDS pattern of green synthesized reduced graphene oxide nanoparticles using Nigella sativa seed extract showing four dominant peaks for boron, carbon, oxygen and silicon atoms (Fig. 6)
Cytotoxic activity of reduced graphene oxide/SiO₂ nanocomposite synthesized from Nigella sativa seed extract against breast carcinoma cells (MCF-7 cell line) (Fig. 7)
Cytotoxic activity of reduced graphene oxide SiO₂ nanocomposite synthesized from Nigella sativa seed extract against Hepatocellular carcinoma cells (HepG-2 cell line) (Fig. 8)
reduced graphene oxide nanoparticles |
Thickness | ≥ 5 nm | — |
Thickness | 1–100 nm | — |
Thickness | 20–30 cm | — |
Particle size distribution of green synthesized reduced graphene oxide/SiO₂ nanocomposite using Nigella sativa seed extract (Fig. 3)
Transmission electron micrographs of reduced graphene oxide decorated with SiO₂ nanocomposite using Nigella sativa seed extract (Figs. 4A and 4B)
Scanning electron micrograph of green synthesized reduced graphene oxide decorated with SiO₂ nanocomposite using Nigella sativa seed extract (Fig. 5)
EDS pattern of green synthesized reduced graphene oxide nanoparticles using Nigella sativa seed extract showing four dominant peaks for boron, carbon, oxygen and silicon atoms (Fig. 6)
Cytotoxic activity of reduced graphene oxide/SiO₂ nanocomposite synthesized from Nigella sativa seed extract against breast carcinoma cells (MCF-7 cell line) (Fig. 7)
Cytotoxic activity of reduced graphene oxide SiO₂ nanocomposite synthesized from Nigella sativa seed extract against Hepatocellular carcinoma cells (HepG-2 cell line) (Fig. 8)
reduced graphene oxide nanoparticles |
Thickness | ≥ 5 nm | — |
Thickness | 1–100 nm | — |
Thickness | 20–30 cm | — |
Particle size distribution of green synthesized reduced graphene oxide/SiO₂ nanocomposite using Nigella sativa seed extract (Fig. 3)
Transmission electron micrographs of reduced graphene oxide decorated with SiO₂ nanocomposite using Nigella sativa seed extract (Figs. 4A and 4B)
Scanning electron micrograph of green synthesized reduced graphene oxide decorated with SiO₂ nanocomposite using Nigella sativa seed extract (Fig. 5)
EDS pattern of green synthesized reduced graphene oxide nanoparticles using Nigella sativa seed extract showing four dominant peaks for boron, carbon, oxygen and silicon atoms (Fig. 6)
Cytotoxic activity of reduced graphene oxide/SiO₂ nanocomposite synthesized from Nigella sativa seed extract against breast carcinoma cells (MCF-7 cell line) (Fig. 7)
Cytotoxic activity of reduced graphene oxide SiO₂ nanocomposite synthesized from Nigella sativa seed extract against Hepatocellular carcinoma cells (HepG-2 cell line) (Fig. 8)
reduced graphene oxide nanoparticles |
Thickness | ≥ 5 nm | — |
Thickness | 1–100 nm | — |
Thickness | 20–30 cm | — |