F0RM2
THE PATENTS ACT, 1970
(39 of 1970)
COMPLETE SPECIFICATION (See section 10 and rule 13)
1. TITLE OF THE INVENTION "NANOTUBE POLYMER COMPOSITION"
2. APPLICANT
1. NAME : MAHANWAR PRAKASH ANNA
NATIONALITY: INDIAN
ADDRESS : DEPARTMENT OF POLYMER AND SURFACE ENGINEERING,
INSTITUTE OF CHEMICAL TECHNOLOGY
(DEEMED UNIVERSITY ), NATHALAL PARIKH MARG,
MATUNGA(EAST)
MUMBAI 400 019 INDIA.
2. NAME : BAMBOLE; VAISHALI ABHAY
NATIONALITY: INDIAN
ADDRESS : DEPARTMENT OF PHYSICS,
UNIVERSITY OF MUMBAI, V1DYANAGARI, KALINA, SANTACRUZ (EAST), MUMBAI 400 098 INDIA
The following specification particularly describes the invention and the manner in which it is to be performed:

FIELD OF INVENTION
The present invention is directed to improved nanotube a polymer composition that is made from a polymer blended with single wall carbon nanotubes that has been reacted with mixtures of organic materials. Nanotube polymer has the properties that when the specified carbon nanotubes chain is added to polymer, an exceptionally well dispersed a composites result which is useful as polymer nanocomposites. Background of Invention
Nanocomposites are materials that consist of partials of one compound with a mean diameter in the nano size range (l-100nm) dispersed throughout another material, commonly modified inorganic clay dispersed within an organic polymer. These polymer -clay nanocomposites (PCN) posses advantages properties compared to the polymer alone such as increased mechanical strength , reduced gaseous permeability and higher heat resistances ,even though the quantity of clay may be 5% or less. Nanocomposites materials have attracted great interest due to the wide range of alterations in the properties of the base polymer emended by the incorporation of clay (see for example Schmidt et al, Current Opm.Solid State Mat.Sci.(2002) 6,205-212; Choi et al. Chem. Mater.(2002) 14, 2936-2939; T.J. Pinnavaia and G.W. Beall, " polymer-clay nanocomposites ", Wiley, Chichester, 2001).
Carbon nanotubes and method for their manufacture are also known. In general, carbon nanotubes are elongated tubular bodies which are typically only a few atoms in circumferences. The carbon nanotubes are hollow and have a linear fullerenes structure, The length of the carbon nanotubes potentially may be millions of times greater than their

molecular-sized diameter. Both single wall carbon nanotubes (SWNTs), as well as multi-wall carbon nanotubes (MWCNTs) have been recognized.
Carbon nanotubes are currently being proposed for a number of applications since they posses a very desirable and unique combination of physical relating to, for example, strength and weight. Carbon nanotubes have also demonstrated conductivity, see Yakobson, B. I.,et al, American Scientist,85,(1997), 324-337; and Dresselhaus, M.S., et al,, Science of Fullerenes and carbon Nanotubes. 1996, San Diego; Academic press, pp.902-905. For example carbon nanotubes conduct heat and better than copper or gold and havelOO times the tensile strength but only sixth of the weight of steel. Carbon nanotubes may be produced having extraordinarily small size. For example, carbon nanotubes are produced that are approximately the size of DNA double helix (or approximately l/50,000th the width of a human hair)
Various techniques for producing carbon nano tubes have been developed. As examples, method of forming carbon nanotubes are described in US patent No. 5,753,088 and 5,482,601, the disclosures of which are hereby incorporated here in by reference. Three common techniques for producing carbon nanotubes are: 1) Laser vaporization technique; 2) electric arc technique, and 3) gas phase technique, which are discussed further below.
In general, the laser vaporization technique utilizes a pulsed laser to vaporize a graphite in producing the carbon nanotubes. The laser vaporization technique is further described by A.G. Rinzler et al. in Appl Phys., 1998, 67, 29. Generally the laser vaporization technique produces carbon nanotubes that have a diameter of approximately 1.1 to 1.3 nanometers (nm).

Another technique for producing carbon nanotubes is the electric arc technique in which carbon nanotubes are synthesized utilizing an electric arc discharge. As an example, single-walled nanotubes (SWNTs) my be synthesized by an electric arc discharge under helium atmosphere with the graphite anode filled with a mixture of metallic catalysts and graphite powder (Ni:Y:C), as described more fully by C. Journet et al. in Mature (London), 388 (1997), 756. Typically, such SWNTs are produced as closed packed bundles (or ropes) with such bundles having diameters ranging from 5 to 20 nm. Generally, the SWNTs are well-aligned in a two dimensional periodic triangular lattice bonded by van der Walls interactions. The electric arc technique of producing carbon nanotubes is further described by C. Journct and P. Bernier in Appl. Phys. A, 67,2 utilizing such an electric arc technique, the average carbon nanotubes diameter is typically approximately 1.3 to 1.5nm and the triangular lattice parameter is approximately 1.7 nm.
In one aspect of the invention, a composition is providing that is a composite including a homogeneous mixture of nanofillers and a polymer. The average practical sizes of the nanoparticles are advantageous not more that about 500nm, such as about lnm to about 500nm. Other preferred sizes include an average practical size of not more than about 250nm, preferably average size of not more than about l00nm and most preferably an average practical size of not more than about 50nm. Typical average particles sizes include about lnm to about 250 nm, about lnm to about l00nm and lnmto about 50nm.
In further forms of the invention, at least about 30%, preferably at [east about 50% and further preferable at least about 75% of the particulate ceramic has an average

particle size of not more than about 400nm, preferable not more than about 300nm, further preferable not more than about 200nm, more preferably not more than about l00nm and most preferably not more than about 50nm to about l00nm.
The compositions may be prepared by melt mixing the polymer and nano fillers and maybe processed using conventional processing methods for thermoplastics and thermoset polymer as known in the art, including injection molding, compression molding, extrusion, transfer molding, solution casting or in-situ polymerization. Homogeneous mixing of the two phases, so that the two components will be sufficiently intermingled, may be achieved by variety of methods including polymer mixing methods known to the arts, including, for examples, blending, extrusion and solvent suspension. Carrier solvents may be utilized as a carrier, for example, the polymer, nano fillers, or both, or particle surface treatment may be applied to facilities homogeneous mixing. US7479516 discloses nanocomposites wherein the host matrix is a polymermatrix and the polymer matrix comprises polyethersultones and carbon nanotube/polymer nanocomposites were fabricated using functionalized, solubilized single walled carbon nanotubes.Nanocomposite comprises of functionalized, solubilized nanomaterial comprises a functionalized and solubilized single walled carbon nanotube. multiwalled carbon nanotube, carbon nanoparticle, carbon nanosheet, carbon nanofiber, carbon nanorope, carbon nanoribbion, carbon nanorefibril, carbon nanoneedle, carbon nanohorn, carbon nanocone, carbon nanoscroll, carbon nanodot or a combination. US7220484 discloses nanocomposites comprising a nanoreinforcing material(e,g. layered clay) a polymer matrix(e.g. a polyolefin) and a epoxy functionalized graft polymer compatible with the polymer matrix( e.g., epoxy grafted polyolefin) wherein the nano

reinforcing material is layered clay, nano- fibers, nano-whiskers, carbon nanotubes, metal- oxide nanotubes, metallic oxides, metallic sulfides, metallic layered hydroxides or mixtures thereof.
US20050191490 discloses nanocomposites comprising: a) a nano-reinforcing material; b) a polymer matrix and c) an epoxy functionalized graft polymer compatible with the polymer matrix wherein the nano reinforcing material is layered clay, nano fibers, nano-whiskers, carbon nanotubes, metal oxide nanotubes, metallic oxides, metallic sulfides, metallic layered hydroxides or a mixtures thereof.
The present invention describes the nanocomposites of the carbon nano plated chains filled Polyethersulfone (PES) which gives a better mechanical, electrical and Theological properties than pure Polyethersulfone (PES) and other micro and nanoclay composites at a very low concentration of the carbon nanoplated chains which can be molded into any desired shape using different molds. The carbon nano plated chains used in the present invention differs from the carbon nanotubes in the sense that most of the carbon nanotubes are having a tubular structure. The tubes may either a single walled or multiwalled and according which they are nomenclature as single walled carbon (SWCNT) nanotubes and multiwalled carbon nanotubes (MWCNT). The carbon nanoplated chains are having platelet structures which are entangled in each to form the chains of these plates which provide them more strength than the carbon nanotubes. The carbon nano plated chains used in the present study were derived from the biomass and average particle size of carbon nanoplated chains used in the present invention was 20-30 nm. Hence these carbon nanoplated chains when incorporated into the polymer matrix provide them a higher strength than any other nanofiller. Poly (arylene ether Sulfone)s

are a family of high performance engineering thermoplastic materials with high glass transition temperature, high thermal stability, good mechanical properties, and excellent resistance to hydrolysis and oxidation. Their outstanding properties have resulted in several important commercial Sulfone or Ketone containing products, such as bispheno! A Polyethersulfone (PES), Udel® (BP-Amoco); poly(ethersulfone), Victrex®(ICI); poly(arylene ether ether ketone) (PEEK). Victrex® PEEK (ICI); poly(arylene ether ketone) (PEK), Stilan® (Raychem Corporation); and poly(arylene etherketone ether ketone ketone) (PEKEKK). Ultrapek® (BASF), Polyehtersulfones haven been widely used as engineering thermoplastics due to their good mechanical properties and thermal stability, which depend on their unique structures. In the Polyethersulfone (PES) main chain, the bond energy of an aliphatic carbon-oxygen ether linkage (84.0 kcal/mol) is slightly higher than that of the carbon-carbon counterpart (83.1 kcal/mol).
OBJECTIVE OF INVENTION
Objective of the present invention is to provide improved nanotube polymer composition that is made from a polymer blended with single wall carbon nanotubes that has been reacted with the mixtures of organic materials.
Another objective of the invention is to provide a carbon nano plated/ polymer composition using a thermoplastic polymer i.e. polyethersulfone. The nano plates used are easily dispersed into polyethersulfone to form a composition useful as nanocomposites.

Another objective of the present invention to produce the nanocomposites of carbon nano plated chain in the Polyethersulfone (PES) matrix and method of producing the same. Yet another objective of the present invention is to produce the nanocomposite of mixture of carbon nano plated chain with Polyethersulfone (PES) with improved mechanical, Electrical and Rheological properties useful for the material of construction in various fields.
Summary of Invention
The present disclosure is directed to Nanotube polymer composition comprising of polymer and single wall carbon nanotubes in mixture of organic materials, wherein polymer is thermoplastic polymer as Polyethersulfone (PES) and composition is Polyethersulfone filled with carbon nanoplated chain with 0.5 to 2.0 weight % loading in the Polyethersulfone (PES) prepared by melt mixing preffered in Polyethersulfone (PES) matrix, composition further comprises of homogenous mixture of nanofilters/ nanoparticles. The composition further comprises particulate ceramic at least about 30 %, preferably at least about 70 % with particulate ceramic has average particle size about 1 to 400 nm., size preferably about 1 to 200 nm & has average particle size about 1 to l00nm.
The present composition is Polyethersulfone (PES) filled with carbon nanoplated chains having a very good solvent resistance to the strong solvents. The carbon nanotubes are single walled carbon nanotubes (SWCNT) and multiwalled carbon nanotubes (MWCNT) in structure and exhibits more strength than conventional single walled carbon nanotubes (SWCNT) and multiwalled carbon nanotubes (MWCNT). The organic material is selected from such as methyl ethyl ketone (MEK), methylene dichloride (MDC) and

combination thereof. The nanofillers/ nanoparticles have of size about 1 nm to 500 nm, preferably about 100 nm to 400 nm, more preferably about 100 nm to 250 nm.
BRIEF DESCRIPTION OF THE DRAWING
For a more complete understanding of the present invention, reference is made to the following description taken in conjunction with the accompanying drawing. It is to be expressly understood, however, that each of the figures is provided for the purpose of illustration and description only and is not intended as a definition of the limits of the present invention.
Figure 1: Transmission Electron Microscopy (TEM) at the 1 μm scale of carbon nanoplated chain. Figure 2: Transmission Electron Microscopy (TEM) at the 500nm scale of carbon nanoplated
chain. Figure 3: Transmission Electron Microscopy (TEM) at the 200 nm scale of carbon nanoplated
chain. Figure 4: Tensile Strength and Tensile Modulus of Nanocomposites of PES/Carbon Nano Plated Chain.
Figure 5: Flexural Strength and Flexural Modulus of Nanocomposites of PES/Carbon Nano Plated Chain.
Figure 6: Impact Strength of Nanocomposites of PES/Carbon Nano Plated Chain. Figure 7; Dielectric Strength of Nanocomposites of PES/Carbon Nano Plated Chain.

DETAILED DESCRIPTION OF INVENTION.
In present invention improved nanotube polymer composition has been disclosed which is made from a polymer blended with single wall carbon nanotubes by reacting with mixtures of organic materials.
Nanotube polymer composition comprises homogeneous mixture of nano fillers and a polymer. The average particle sizes of the nanoparticles are advantageous not more than 500nm, such as about lnm to about 500nm. Other preferred sizes include an average particle size of not more than about 250nm, preferably average particle size of not more than about 50nm. Typical average particle sizes include about lnm to about 250nm, about lnm to about l00nm and preferred lnm to about 50nm.
Nanotube polymer composition further comprises at least about 30%, preferably at least about 50% and further preferably at least about 75% of the particulate ceramic which has an average particle size of not more than about 400nm, preferably not more than about 300nm, further preferably not more than about 200nm, more preferably not more than about l00nm and most preferably not more than about 50nm to about lOOnm. The composition may be prepared by melt mixing the polymer and nano fillers and may be processed using conventional processing methods for thermoplastics and thermoset polymer, including injection molding, compression molding, extrusion, transfer molding, solution casting or in-situ polymerization. Homogeneous mixing of the two phases, so that the two components will be sufficiently intermingled, may be achieved by variety of methods including polymer mixing methods known in the art, including for examples, blending, extrusion and solvent suspension. Carrier solvents may be utilized as a carrier

for examples, the polymer, nano filler, or both, or particles surface treatment may be
applied to facilities homogeneous mixing.
Nanocomposite of present invention comprises carbon nano plated chains filled
polyethersulfones (PES) which gives a better mechanical, electrical and rheological
properties than pure polyethersulfone(PES) and other micro and nanoclay composites at a
very low concentration of the carbon nanoplated chains which can be molded into any
desired shape using different molds.
The present invention further discloses method for the exfoliation and dispersion
/solubilization of exfoliated nanomaterials. Carbon nano plated chain is typically bundled
or rope, which bundles or ropes must be undone at least in part, i.e exfoliated to enable
the dispersion/solublization and functionalization of the nanomaterials. The method
comprises mixing nanomaterials, a poly(ethersulfone) having a polymer backbone of "n"
monomer units comprising at least one electron withdrawing substituents. and wherein
"n" is from about 3 to about 200.Embodiments further provide for fine tuning of
dispersion behavior by having manipulation groups on the peripheral substituents of the
polymer.
Nanotube polymer composition of present invention can be used in a aerospace, marine,
electrical and electronic, relatively strong and stiff materials, method for making such
composities and devices and tools that include composites.
Nanotube polymer compositions are manufacture by melt extrusion, the various
components(antioxidant) may be mixed simultaneous!y(prior to extrusion) in order to
disperse the active ingrident throughout the nanocomposites materials, although the
mixing sequence can influence the product structure and performances and represents

another means by which the properties and release charactrestic of the composition may
be controlled.Other factor such as the choice of extrusion screw geometries may
influence the sturctureand performance of the extrudate.
One of the embodiment of the invention is that amount of carbon nanoplated chain used
in the nanocomposites of the current invention will carry depending upon the desired
properties in the final nanocomposites and generally range from amount 0.1 to 15% by
weight based on total weight of composition.
One of the embodiments of the invention is that composites can carry from 85% up to
about 99.9% by weight of the total composition depending on desired application. The
preffered polymer content can be 90% to 99.9%; more preferably 96 to 99.5%.
One of the embodiment of the invention is that PES powder is mixed with nanofillers, the
various kind of nanofillers can be used i.e ceramic, diamond powder, layered silicates.
clays, nano fibers etc. and microfillers, mica and silica (5-30 by wt.%) in high speed
mixer using 80 rpm then in blended in ZE twin screw, Berstott Ze-25 with L/D 40:1 with
speed of 220 rpm using temperature profile as zone-1 330°C zone -2 350 °C and extrudate
is quenched in water and palletized to obtain pallets.
One of the embodiments of the invention is that before molding the granules is predried
for 3 hrs at 180 °C and molded using injection molding machine LTM-Demag Italy using
a temperature profile in zone -1 340°C zone-2 360°C and zone-3 370°C and nozzle
390 °C and is cooled at room temperature to build a proper crystallinity.
One of the embodiments of the invention is that injection molded specimens were
conditioned for stress relaxation for 24 hrs at room temperature and then characterized
for the mechanical, thermal, electrical and weathering properties.

One of the embodiments of the invention is that carbon nanoplated chains are having
platelet structures which are entangled in each to form the chains of these plates which
provide them more strength than the carbon nanotubes.
One of the embodiments of the invention is thatcarbon nano plated chains used in the
present study were derived from the biomass and average particle size of carbon
nanoplated chains used in the present invention was 2G-30nm.
Hence these carbon nanoplated chains when incorporated into the polymer matrix
provide them a higher strength than any other nanofiller. Poly(arylene ether sulfone)s are
a family of high performance engineering thermoplastic material with high glas transition
temperature , high thermal stability, good mechanical properties, and excellent resistance
to hydrolysis and oxidation.
As describes herein preferred embodiments of nanocomposites for use in application requiring a aerospace, marine, electrical and electronics, relatively strong and stiff materials, method for making such composites and devices and tools that include composites.
The present invention will be now illustrated with the examples. The examples are by the way of illustration only and in no way restrict the scope of invention. Example 1:
Carbon nano plated chain 0,1% by weight was mixed with PES powder in high speed mixer for 30 min at 220 rpm. Then it was melt blended in twin screw extruder at temperature profile of 320-370°C. The extrudate was cooled and palletized for further processing. The pallets were then conditioned for 24 Hrs. at room temperature to build a

proper crystallinity and injections moulded to desired shape using proper mould and were then characterized for mechanical, electrical, thermal and Theological properties. Example 2:
Carbon nano plated chain 0.5% by weight was mixed with PES powder in high speed mixer for 30 min at 220 rpm. Then it was melt blended in twin screw extruder at temperature profile of 320-370°C, The extrudate was cooled and palletized for further processing. The pallets were then conditioned for 24 Hrs. at room temperature to build a proper crystallinity and injections moulded to desired shape using proper mould and were then characterized for mechanical, electrical, thermal and rheological properties. Example 3:
Carbon nano plated chain 1% by weight was mixed with PES powder in high speed mixer for 30 min at 220 rpm. Then it was melt blended in twin screw extruder at temperature profile of 320-370°C. The extrudate was cooled and palletized for further processing. The pallets were then conditioned for 24 Hrs. at room temperature to build a proper crystallinity and injections moulded to desired shape using proper mould and were then characterized for mechanical, electrical, thermal and rheological properties. Example 4:
Carbon nano plated chain 1.5% by weight was mixed with PES powder in high speed mixer for 30 min at 220 rpm. Then it was melt blended in twin screw extruder at temperature profile of 320-370°C. The extrudate was cooled and palletized for further processing. The pallets were then conditioned for 24 Hrs. at room temperature to build a proper crystallinity and injections moulded to desired shape using proper mould and were then characterized for mechanical, electrical, thermal and rheological properties.

Example 5:
Carbon nano plated chain 2% by weight was mixed with PES powder in high speed mixer for 30 min at 220 rpm. Then it was melt blended in twin screw extruder at temperature profile of 320-370oC. The extrudate was cooled and palletized for further processing. The pallets were then conditioned for 24 Hrs. at room temperature to build a proper crystallinity and injections moulded to desired shape using proper mould and were then characterized for mechanical, electrical, thermal and Theological properties.

We Claim:
1) Nanotube polymer composition comprising of polymer and single wall carbon nanotubes in mixture of organic materials.
2) Nanotube polymer composition as claimed in claim ] wherein polymer is thermoplastic polymer as Polyethersulfone (PES).
3) Nanotube polymer composition as claimed in claim 1 wherein composition is Polyethersulfone filled with carbon nanoplated chain with 0.5 to 2.0 weight % loading in the Polyethersulfone (PES) prepared by melt mixing.
4) Nanotube polymer composition as claimed in claim 1 wherein carbon nanotubes are single walled carbon nanotubes (SWCNT) and multiwalled carbon nanotubes (MWCNT) in structure and exhibits more strength than conventional single walled carbon nanotubes (SWCNT) and multiwalled carbon nanotubes (MWCNT).
5) Nanotube polymer composition as claimed in claim l,wherein composition is Polyethersulfone filled with carbon nanoplated chain with 0.5 to 2 weight % loading of carbon nanoplated chain in Polyethersulfone (PES) matrix.
6) Nanotube polymer composition as claimed in claim 1, wherein composition is Polyethersulfone (PES) Filled with carbon nanoplated chains having a very good solvent resistance to the strong solvents.
7) Nanotube polymer composition as claimed in claim I, wherein organic material is selected from such as methyl ethyl ketone (MEK) , methylene dichloride (MDC) and combination thereof.
8) Nanotube polymer composition as claimed in claim 1, wherein composition further comprises of homogenous mixture of nanofillers/nanoparticles.

9) Nanotube polymer composition as claimed in claim 8, wherein nanofillers/ nanoparticles have of size about 1 nm to 500 nm.
10)Nanotube polymer composition as claimed in claim 9, wherein nanofillers/ nanoparticles have of size preferably about 100 nm to 400 nm.
ll)Nanotube polymer composition as claimed in claim 8, wherein nanofillers/ nanoparticles have of size more preferably about 100 nm to 250 nm.
12) "Nanotube polymer composition as claimed in claim 1, wherein composition further comprises particulate ceramic at least about 30 %.
13) Nanotube polymer composition as claimed in claim 1, wherein composition further comprises particulate ceramic preferably at least about 70 %.
14) Nanotube polymer composition as claimed in claim 12. wherein particulate ceramic has average particle size about 1 to 400 nm.
15) Nanotube polymer composition as claimed in claim 12. wherein particulate ceramic has average particle size preferably about 1 to 200 nm.
16) Nanotube polymer composition as claimed in claim 12, wherein particulate ceramic has average particle size about 1 to 100 nm.