Title of Invention	"A METHOD OF PREPARATION OF NANOPARTICLES COATED CARBON FIBER"
Abstract	This invention relates to a method for preparation of nanoparticles coated carbon fibers or fabrics comprising the step of heating the carbon fibers or fabrics at a temperature of 100-700°C for a time period of 0.1-2 hours in air, coating of metal or metal oxide selected from nickel oxide, cobalt oxide, iron oxide, ruthenium oxide, palladium oxide, molybdenum oxide, irredium oxide , platinum and chromium oxide on carbon fibers or fabrics in the temperature range of 25 to 150°C for a period of 1 to 120 minutes by dip coating or sol-gel method or wet spraying as herein described, heating the coated fibers or fabrics in the temperature range of 50 to 500°C for a period of 0.1 to 2 hours to form a layer of metal or metal oxide followed by cooling, incorporation of the metal or metal oxide coated fibers or fabrics into reactor, connecting the reactor to a vacuum line to pump down to less than 200 mm Hg, incorporation of the inert gases into the reactor, incorporation of the inert gases and/or reducing gases into the reactor, de-oxygenation of the gases followed by removal of moisture, heating of metal or metal oxide layer of carbon fibers or fabrics at temperature of 400 to 900°C for 0.1 to 2 hours inert or reducing or mixture of inert and reducing atmosphere to obtain nanoparticles coated carbon fibers or fabrics.

Title of Invention

"A METHOD OF PREPARATION OF NANOPARTICLES COATED CARBON FIBER"

Abstract

This invention relates to a method for preparation of nanoparticles coated carbon fibers or fabrics comprising the step of heating the carbon fibers or fabrics at a temperature of 100-700°C for a time period of 0.1-2 hours in air, coating of metal or metal oxide selected from nickel oxide, cobalt oxide, iron oxide, ruthenium oxide, palladium oxide, molybdenum oxide, irredium oxide , platinum and chromium oxide on carbon fibers or fabrics in the temperature range of 25 to 150°C for a period of 1 to 120 minutes by dip coating or sol-gel method or wet spraying as herein described, heating the coated fibers or fabrics in the temperature range of 50 to 500°C for a period of 0.1 to 2 hours to form a layer of metal or metal oxide followed by cooling, incorporation of the metal or metal oxide coated fibers or fabrics into reactor, connecting the reactor to a vacuum line to pump down to less than 200 mm Hg, incorporation of the inert gases into the reactor, incorporation of the inert gases and/or reducing gases into the reactor, de-oxygenation of the gases followed by removal of moisture, heating of metal or metal oxide layer of carbon fibers or fabrics at temperature of 400 to 900°C for 0.1 to 2 hours inert or reducing or mixture of inert and reducing atmosphere to obtain nanoparticles coated carbon fibers or fabrics.

Full Text	Figure 14 shows I-V for as -received carbon fibers/fabrics and nanoparticles coated carbon fibers/fabrics Table 1 shows elemental analysis of nickel nanoparticles coated carbon fibers/fabrics Table 2 shows degradation temperatures corresponding to peak for as-received carbon fibers/fabrics and nanoparticles coated carbon fibers/fabrics in nitrogen atmosphere Table 3 shows degradation temperatures corresponding to peak for as-received carbon fibers/fabrics and nanoparticles coated carbon fibers/fabrics in oxygen environment Table 4 shows onset voltage of as-received carbon fibers/fabrics and nanoparticles coated carbon fibers/fabrics STATEMENT OF INVENTION According to this invention there is provide a method for preparation of nanoparticles coated carbon fibers or fabrics comprising the step of : - heating the carbon fibers or fabrics at a temperature of 100-700°C for a time period of 0.1-2 hours in air, - coating of metal or metal oxide selected from nickel oxide, cobalt oxide, iron oxide, ruthenium oxide, palladium oxide, molybdenum oxide, irredium oxide , platinum and chromium oxide on carbon fibers or fabrics in the temperature range of 25 to 150°C for a period of 1 to 120 minutes by dip coating or sol-gel method or wet spraying as herein described, - heating the coated fibers or fabrics in the temperature range of 50 to 500°C for a period of 0.1 to 2 hours to form a layer of metal or metal oxide followed by cooling, - incorporation of the metal or metal oxide coated fibers or fabrics into reactor, - connecting the reactor to a vacuum line to pump down to less than 200 mm Hg, - incorporation of the inert gases into the reactor, - incorporation of the inert gases and/or reducing gases into the reactor, - de-oxygenation of the gases followed by removal of moisture, - heating of metal or metal oxide layer of carbon fibers or fabrics at temperature of 400 to 900°C for 0.1 to 2 hours inert or reducing or mixture of inert and reducing atmosphere to obtain nanoparticles coated carbon fibers or fabrics. panels, main landing gear doors, nose radome, nose gear doors, outboard aileron, outboard flap, outboard spoilers, rudder, stabilizer torque box, strut forward, trailing edge panels, wing fixed leading edge, wing to body fairing, etc. EXPECTED OUTCOME 3: The composites made of nanoparticles coated carbon fibers/fabrics can also replace various existing components of AIRBUS-A340 commercial aircraft. Few of these are ailerons, apron, aft pylon fairings, belly fairing skin, CLG doors, elevator, fin box attachment, fin TE panels, fin LE tip, fin fairing, fuselage fairing, flap track fairing, HTP outer boxes, HTP, LE, HTP LE panels, MLG door, MLG bay top panel, MLG leg fairings, nacelle, NLG doors, outer flaps, pylon fairing, radome, rubber, spoilers, wing LE fillet, wing LE upper panels, wing LE lower panels, wing tip fence, etc EXPECTED OUTCOME 4: The composites made of nanoparticles coated carbon fibers/fabrics can be used in automobile industries. Few of these are leaf spring, shaft, outer body, etc. EXPECTED OUTCOME 5: The composites made of nanoparticles coated carbon fibers/fabrics can also be used to replace the conventional sport materials like tennis racket, golf shaft, etc. Example A A simple horizontal tubular reactor is used to coat metal/ metal oxide nanoparticles on carbon fiber/ fabric. This reactor has a quartz tube of 840 mm length with an outer diameter of 49 mm and inner diameter of 45 mm. It is constructed in such a way that the carbon fiber/fabric can be easily inserted and removed from the reactor. The reactor is heated in a three zone tubular furnace. A proportional temperature controller controls the furnace temperature in each zone. The temperature is kept around 500 to 900°C in the mid zone of furnace to facilitate the decomposition of precursor gases. The inlet and outlet temperatures were maintained in the range of 300 to 600°C. Nitrogen, helium, argon, chlorine, hydrogen, and mixtures of it are used as precursor gases. Each gas has its own function. Hydrogen/chlorine acts as a reducing gas and nitrogen/helium/argon acts as a carrier gas and also provides the inert atmosphere inside the reactor. The coating of catalyst i.e., iron (Fe), cobalt (Co), nickel (Ni), ruthenium (Ru), rhodium (Rh), palladium (Pd), iridium (Ir), platinum (Pt) chromium (Cr), molybdenum (Mo), etc on glass fiber(s)/fabric is done by the conventional dip coating/sol-gel/wet spraying technique (For composition: Tables: A to F). The carbon fiber/fabric is dipped in a bath containing nickel sulphate (NiSO4 6H2O, source of nickel), sodium hypophosphite (NaH2PO2 H2O, reducing agent), ammonium chloride (NH4Cl, complexing agent), tri-sodium citrate (Na3C6H5O7 2H2O, stabilizer), ammonium hydroxide (NH4OH, pH adjustment) for coating of nickel (Table A). The catalyst coated glass carbon fiber/fabric is kept in the middle zone of the reactor. The reactor is connected to a vacuum line and then pumped down to less than 200 mm Hg. This process is continued 10 times till it is free of oxygen. In the next step the temperature of reactor is increased in between 400 to 600°C in an inert atmosphere. The rate of inert gas flow is kept constant at 120 ml/min. After 5 to 10 minutes reducing gas is allowed to flow at the rate of 5 to 25 ml/min for 10 to 30 minutes. Again after 5 to 10 minutes, temperature is increased to 500-900°C. The gases entered in the reactor through three different non-return valves. The flow rates of gases are measured by mass flow controller. The water circulation arrangement is made at inlet and exit of the reactors tube to keep the temperature at desired level. Water is also used as a coolant in the condenser. Any condensable in the reactor effluent is collected in a liquid collector where as noncondensables are sent to the exit flow, which is recorded by the pressure indicator dial and then vented to the atmosphere. The nanomaterial coated carbon fiber/fabric is characterized by XRD, TGA, SEM, IV, etc. Example B In this case the carbon fiber/fabric is dipped in a bath. The formulation of bath is given in Table B. The catalyst coated carbon fiber/fabric is placed inside the reactor for coating of nanomaterials. The experimental condition is same as mentioned in Example A. Example C In this case the carbon fiber/fabric is dipped in a bath. The formulation of bath is given in Table C. The catalyst coated carbon fiber/fabric is placed inside the reactor for coating of nanomaterials. The experimental condition is same as mentioned in Example A. It is to be understood that the process of the present invention is susceptible to modification, changes, adaptations by those skilled in the art. Such modifications, changes adaptations are intended to be within the scope of the present invention which is further set forth under the following claims:- WE CLAIM; 1. A method for preparation of nanoparticles coated carbon fibers or fabrics comprising the step of: - heating the carbon fibers or fabrics at a temperature of 100-700°C for a time period of 0.1-2 hours in air, - coating of metal or metal oxide selected from nickel oxide, cobalt oxide, iron oxide, ruthenium oxide, palladium oxide, molybdenum oxide, irredium oxide , platinum and chromium oxide on carbon fibers or fabrics in the temperature range of 25 to 150°C for a period of 1 to 120 minutes by dip coating or sol-gel method or wet spraying as herein described, - heating the coated fibers or fabrics in the temperature range of 50 to 500°C for a period of 0.1 to 2 hours to form a layer of metal or metal oxide followed by cooling, - incorporation of the metal or metal oxide coated fibers or fabrics into reactor, - connecting the reactor to a vacuum line to pump down to less than 200 mm Hg, - incorporation of the inert gases into the reactor, - incorporation of the inert gases and/or reducing gases into the reactor, - de-oxygenation of the gases followed by removal of moisture, - heating of metal or metal oxide layer of carbon fibers or fabrics at temperature of 400 to 900°C for 0.1 to 2 hours inert or reducing or mixture of inert and reducing atmosphere to obtain nanoparticles coated carbon fibers or fabrics. 2. A method for preparation of nanoparticles coated carbon fibers or fabrics as claimed in claim 1 wherein the coating metallic oxide comprises nickel oxide by nickel sulphate and sodium hypophosphite and sodium succinate and buffer solution; cobalt oxide by cobalt chloride or cobalt acetate or cobalt nitrate in acid or base solution; iron oxide by ferric nitrate or ferric sulphate or ferric acetate in alcohol or acid solution; ruthenium oxide by ruthenium nitrate solution; palladium oxide by palladium nitrate solution; molybdenum oxide by molybdenum acetate or ammonium molybdate solution; irredium oxide by iridium acetate solution; platinum by tetramine platinum bicarbonate or platinum acetate or platinum nitrate solution; chromium oxide by chromium acetate solution; rhodium oxide by rhodium acetate solution. 3. A method for preparation of nanoparticles coated carbon fibers or fabrics as claimed in claim 1 or 2, wherein the nanoparticles are Fe, Co, Ni, Ru, Rh, Pd, Ir, Pt, Cr, Mo, or mixtures of atleast two thereof. 4. A method for preparation of nanoparticles coated carbon fibers or fabrics as claimed in any of the preceding claims wherein the fibers is selected from the group comprising of rayon based carbon fiber, pitch based carbon fiber, polyacrylonitrile based carbon fiber; the inert atmosphere is selected from the group comprising of nitrogen, helium, argon, and mixtures thereof, the reducing gas selected from the group comprising of hydrogen, chlorine, and mixtures thereof. 5. A method for preparation of nanoparticles coated carbon fibers or fabrics as claimed in any of the preceding claims wherein the ratio of flow rate of inert gas to reducing gas is in the ratio of 1:0 to 10:1. 6. A method for preparation of nanoparticles coated carbon fibers or fabrics as claimed in any of the preceding claims wherein 50% of the nanoparticles are having a diameter less than 40 nm and 70% of the nanoparticles having a diameter less than 90 nm. 7. A method for preparation of nanoparticles coated carbon fibers or fabrics as claimed in any of the preceding claims wherein the density of nanoparticles are in the range of 1 to 90% (by weight). 8. A method for preparation of nanoparticles coated carbon fibers or fabrics as claimed in any of the preceding claims wherein the gases are de-oxygenated by passing them through an alkaline pyrogallol solution followed by removal of moisture by passing the gases through a silica gel bed.

Full Text

Figure 14 shows I-V for as -received carbon fibers/fabrics and nanoparticles coated carbon fibers/fabrics
Table 1 shows elemental analysis of nickel nanoparticles coated
carbon fibers/fabrics
Table 2 shows degradation temperatures corresponding to peak for
as-received carbon fibers/fabrics and nanoparticles coated carbon fibers/fabrics in nitrogen atmosphere
Table 3 shows degradation temperatures corresponding to peak for
as-received carbon fibers/fabrics and nanoparticles coated carbon fibers/fabrics in oxygen environment
Table 4 shows onset voltage of as-received carbon fibers/fabrics and
nanoparticles coated carbon fibers/fabrics
STATEMENT OF INVENTION
According to this invention there is provide a method for preparation of nanoparticles coated carbon fibers or fabrics comprising the step of :
- heating the carbon fibers or fabrics at a temperature of 100-700°C for a time period of 0.1-2 hours in air,
- coating of metal or metal oxide selected from nickel oxide, cobalt oxide, iron oxide, ruthenium oxide, palladium oxide, molybdenum oxide, irredium oxide , platinum and chromium oxide on carbon fibers or fabrics in the temperature range of 25 to 150°C for a period of 1 to 120 minutes by dip coating or sol-gel method or wet spraying as herein described,
- heating the coated fibers or fabrics in the temperature range of 50 to 500°C for a period of 0.1 to 2 hours to form a layer of metal or metal oxide followed by cooling,
- incorporation of the metal or metal oxide coated fibers or fabrics into reactor,
- connecting the reactor to a vacuum line to pump down to less than 200 mm Hg,
- incorporation of the inert gases into the reactor,
- incorporation of the inert gases and/or reducing gases into the reactor,
- de-oxygenation of the gases followed by removal of moisture,
- heating of metal or metal oxide layer of carbon fibers or fabrics at temperature of 400 to 900°C for 0.1 to 2 hours inert or reducing or mixture of inert and reducing atmosphere to obtain nanoparticles coated carbon fibers or fabrics.

panels, main landing gear doors, nose radome, nose gear doors, outboard aileron, outboard flap, outboard spoilers, rudder, stabilizer torque box, strut forward, trailing edge panels, wing fixed leading edge, wing to body fairing, etc.
EXPECTED OUTCOME 3: The composites made of nanoparticles coated carbon fibers/fabrics can also replace various existing components of AIRBUS-A340 commercial aircraft. Few of these are ailerons, apron, aft pylon fairings, belly fairing skin, CLG doors, elevator, fin box attachment, fin TE panels, fin LE tip, fin fairing, fuselage fairing, flap track fairing, HTP outer boxes, HTP, LE, HTP LE panels, MLG door, MLG bay top panel, MLG leg fairings, nacelle, NLG doors, outer flaps, pylon fairing, radome, rubber, spoilers, wing LE fillet, wing LE upper panels, wing LE lower panels, wing tip fence, etc
EXPECTED OUTCOME 4: The composites made of nanoparticles coated carbon fibers/fabrics can be used in automobile industries. Few of these are leaf spring, shaft, outer body, etc.
EXPECTED OUTCOME 5: The composites made of nanoparticles coated carbon fibers/fabrics can also be used to replace the conventional sport materials like tennis racket, golf shaft, etc.
Example A
A simple horizontal tubular reactor is used to coat metal/ metal oxide nanoparticles on carbon fiber/ fabric. This reactor has a quartz tube of 840 mm length with an outer diameter of 49 mm and inner diameter of 45 mm. It is constructed in such a way that the carbon fiber/fabric can be easily inserted and removed from the reactor. The reactor is heated in a three zone tubular furnace. A proportional temperature controller controls the furnace temperature in each zone. The temperature is kept around 500 to 900°C in the mid zone of furnace to facilitate the decomposition of precursor gases. The inlet and outlet temperatures were maintained in the range of 300 to 600°C. Nitrogen, helium, argon, chlorine, hydrogen, and mixtures of it are used as precursor gases. Each gas has its own function. Hydrogen/chlorine acts as a reducing gas and nitrogen/helium/argon acts as a carrier gas and also provides the inert atmosphere inside the reactor. The coating of catalyst i.e., iron (Fe), cobalt (Co), nickel (Ni), ruthenium (Ru), rhodium (Rh), palladium (Pd), iridium (Ir), platinum (Pt) chromium (Cr), molybdenum (Mo), etc on glass fiber(s)/fabric is done by the conventional dip coating/sol-gel/wet spraying technique (For composition: Tables: A to F). The carbon fiber/fabric is dipped in a bath containing nickel sulphate (NiSO4 6H2O,

source of nickel), sodium hypophosphite (NaH2PO2 H2O, reducing agent), ammonium chloride (NH4Cl, complexing agent), tri-sodium citrate (Na3C6H5O7 2H2O, stabilizer), ammonium hydroxide (NH4OH, pH adjustment) for coating of nickel (Table A). The catalyst coated glass carbon fiber/fabric is kept in the middle zone of the reactor. The reactor is connected to a vacuum line and then pumped down to less than 200 mm Hg. This process is continued 10 times till it is free of oxygen. In the next step the temperature of reactor is increased in between 400 to 600°C in an inert atmosphere. The rate of inert gas flow is kept constant at 120 ml/min. After 5 to 10 minutes reducing gas is allowed to flow at the rate of 5 to 25 ml/min for 10 to 30 minutes. Again after 5 to 10 minutes, temperature is increased to 500-900°C. The gases entered in the reactor through three different non-return valves. The flow rates of gases are measured by mass flow controller. The water circulation arrangement is made at inlet and exit of the reactors tube to keep the temperature at desired level. Water is also used as a coolant in the condenser. Any condensable in the reactor effluent is collected in a liquid collector where as noncondensables are sent to the exit flow, which is recorded by the pressure indicator dial and then vented to the atmosphere. The nanomaterial coated carbon fiber/fabric is characterized by XRD, TGA, SEM, IV, etc.
Example B
In this case the carbon fiber/fabric is dipped in a bath. The formulation of bath is given in Table B. The catalyst coated carbon fiber/fabric is placed inside the reactor for coating of nanomaterials. The experimental condition is same as mentioned in Example A.
Example C
In this case the carbon fiber/fabric is dipped in a bath. The formulation of bath is given in Table C. The catalyst coated carbon fiber/fabric is placed inside the reactor for coating of nanomaterials. The experimental condition is same as mentioned in Example A.
It is to be understood that the process of the present invention is susceptible to modification, changes, adaptations by those skilled in the art. Such modifications, changes adaptations are intended to be within the scope of the present invention which is further set forth under the following claims:-

WE CLAIM;
1. A method for preparation of nanoparticles coated carbon fibers or
fabrics comprising the step of:
- heating the carbon fibers or fabrics at a temperature of 100-700°C for a time period of 0.1-2 hours in air,
- coating of metal or metal oxide selected from nickel oxide, cobalt oxide, iron oxide, ruthenium oxide, palladium oxide, molybdenum oxide, irredium oxide , platinum and chromium oxide on carbon fibers or fabrics in the temperature range of 25 to 150°C for a period of 1 to 120 minutes by dip coating or sol-gel method or wet spraying as herein described,
- heating the coated fibers or fabrics in the temperature range of 50 to 500°C for a period of 0.1 to 2 hours to form a layer of metal or metal oxide followed by cooling,
- incorporation of the metal or metal oxide coated fibers or fabrics into reactor,
- connecting the reactor to a vacuum line to pump down to less than 200 mm Hg,
- incorporation of the inert gases into the reactor,
- incorporation of the inert gases and/or reducing gases into the reactor,
- de-oxygenation of the gases followed by removal of moisture,
- heating of metal or metal oxide layer of carbon fibers or fabrics at temperature of 400 to 900°C for 0.1 to 2 hours inert or reducing or mixture of inert and reducing atmosphere to obtain nanoparticles coated carbon fibers or fabrics.
2. A method for preparation of nanoparticles coated carbon fibers or
fabrics as claimed in claim 1 wherein the coating metallic oxide
comprises nickel oxide by nickel sulphate and sodium
hypophosphite and sodium succinate and buffer solution; cobalt
oxide by cobalt chloride or cobalt acetate or cobalt nitrate in acid
or base solution; iron oxide by ferric nitrate or ferric sulphate or
ferric acetate in alcohol or acid solution; ruthenium oxide by

ruthenium nitrate solution; palladium oxide by palladium nitrate solution; molybdenum oxide by molybdenum acetate or ammonium molybdate solution; irredium oxide by iridium acetate solution; platinum by tetramine platinum bicarbonate or platinum acetate or platinum nitrate solution; chromium oxide by chromium acetate solution; rhodium oxide by rhodium acetate solution.
3. A method for preparation of nanoparticles coated carbon fibers or
fabrics as claimed in claim 1 or 2, wherein the nanoparticles are
Fe, Co, Ni, Ru, Rh, Pd, Ir, Pt, Cr, Mo, or mixtures of atleast two
thereof.
4. A method for preparation of nanoparticles coated carbon fibers or
fabrics as claimed in any of the preceding claims wherein the fibers
is selected from the group comprising of rayon based carbon fiber,
pitch based carbon fiber, polyacrylonitrile based carbon fiber; the
inert atmosphere is selected from the group comprising of nitrogen,
helium, argon, and mixtures thereof, the reducing gas selected
from the group comprising of hydrogen, chlorine, and mixtures
thereof.
5. A method for preparation of nanoparticles coated carbon fibers or
fabrics as claimed in any of the preceding claims wherein the ratio
of flow rate of inert gas to reducing gas is in the ratio of 1:0 to
10:1.
6. A method for preparation of nanoparticles coated carbon fibers or fabrics as claimed in any of the preceding claims wherein 50% of the nanoparticles are having a diameter less than 40 nm and 70% of the nanoparticles having a diameter less than 90 nm.
7. A method for preparation of nanoparticles coated carbon fibers or fabrics as claimed in any of the preceding claims wherein the density of nanoparticles are in the range of 1 to 90% (by weight).
8. A method for preparation of nanoparticles coated carbon fibers or fabrics as claimed in any of the preceding claims wherein the gases are de-oxygenated by passing them through an alkaline pyrogallol solution followed by removal of moisture by passing the gases through a silica gel bed.

Documents:

3063-DEL-2005-Abstract-(14-07-2011).pdf

3063-DEL-2005-Claims-(14-07-2011).pdf

3063-DEL-2005-Correspondence Others-(14-07-2011).pdf

3063-DEL-2005-Drawings-(14-07-2011).pdf

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Patent Number

250274

Indian Patent Application Number

3063/DEL/2005

PG Journal Number

51/2011

Publication Date

23-Dec-2011

Grant Date

21-Dec-2011

Date of Filing

16-Nov-2005

Name of Patentee

INDIAN INSTITUTE OF TECHNOLOGY

Applicant Address

KANPUR,KANPUR-208016, AN INDIAN

Inventors:

#	Inventor's Name	Inventor's Address
1	KAMAL KRISHNA KAR	INDIAN INSTITUTE OF TECHNOLOGY, KANPUR,KANPUR-208016
2	PRABHAT KUMAR AGNIHOTRI	INDIAN INSTITUTE OF TECHNOLOGY, KANPUR,KANPUR-208016
3	SANJAY DAS GUPTA	SATELLITE CENTRE, INDIAN SPACE RESEARCH ORGANISATION (ISRO) AIRPORT ROAD, VIMANPURA, BANGALORE-560017,INDIA

PCT International Classification Number

C23C 2/00

PCT International Application Number

N/A

PCT International Filing date

PCT Conventions:

#	PCT Application Number	Date of Convention	Priority Country
1			NA