Abstract: The present invention precisely provides a process of synthesizing conducting polymers with a filler material coated over a carbon foam substrate in aqueous medium, said process comprising the steps of using blank carbon foam as antistatic shield material; adding 0.05 - 0.2 M aniline to 0.05 - 0.2 M pyrrole monomers; mixing 0.05 - 0.2 M Sodium dodecyl Sulphate (SDS) solution into the mixture of second step; homogenizing at 10000 - 15000 rpm for 2 hrs to form a stable emulsion, wherein after homogenization the carbon foam used as substrate cut with the dimension of 50mmx70mm on which coating is performed; adding 0.05 - 0.2 gm graphene to the resultant mixture; adding 0.05 - 0.2 M APS dropwise to the resultant mixture; and shaking up to 6 hrs prepared sample was filtered, washed and dried in oven at 50 °C in order to get the final product.
[001] The present invention relates to development of Conducting Polymer assisted carbon foam composite as antistatic shield material for electrostatically sensitive components or for forming packages and protecting them from potentially damages from unusual electrostatic charges. The primary objective of the invention to design conducting polymer assisted carbon foam composite incorporating filler materials and by selecting a medium of synthesis of prepared composite.
BACKGROUND AND PRIOR ARTS OF THE INVENTION
[002] The phenomena connected with electrostatic charge have an important impact on polymeric materials. While there are helpful aspects of static charge in some areas such as electrets filters, this charge is generally regarded as having a negative impact on processes and products. Polymeric materials or products can be made conductive, electrostatic dissipative (ESD) and antistatic by various means. Whenever two surfaces are rubbed together, electrons are transferred from one surface to the other, thus creating a charge. When a surface has the ability to resist the generation of charge it is said to be antistatic, while the ESD property refers to the ability of a material to conduct electricity either on the surface or through the volume of the material. Antistatic packaging materials are generally prepared by blending polymer matrices with conductive polymers or fillers, allowing the formation of new polymeric materials with unique electrical properties. For antistatic applications, the magnitude of the volume electrical
_1 Q _C _1
conductivity of packaging materials ranges from 10 to 10 S cm .A variety of conductive materials like carbon blacks, carbon fibres, carbon nanotubes, metallic powders, flakes or fibres, and glass spheres or glass fibres coated with metals can be incorporated in conventional polymers. In the past four decades, conducting polymers have emerged as potential materials for high tech and futuristic applications due to tunable conductivity and sensitivity toward external stimuli. In
the present invention Poly(aniline-co-pyrrole) assisted carbon foam has been utilised as antistatic encasing material.
[003] Following are the works done so far in the field of Conducting Polymers based antistatic shield Materials:-
[004] EP 0554588 Bl relates to a sheet or web material having antistatic properties. A sheet material is developed that comprising of a hydrophobic resin support or paper support coated with at least one hydrophobic resin layer wherein said resin support or resin layer is coated with a transparent antistatic layer containing as an essential component an oxidatively polymerized polythiophene with conjugated polymer backbone in the presence of a polymeric polyanion compound. The antistatic layer is coated with an overlying adhering barrier layer applied from aqueous polymer dispersion, i. e. polymer latex, wherein said polymer has hydrophilic functionality sufficient to render said overlying layer adherent to a thereon coated hydrophilic colloid-containing layer.
[005] US 20100190924 Al discloses electrically conductive and non-conductive polymer composite materials suitable for use in electrically conductive materials, electromagnetic wave shielding materials, heating elements, antistatic materials, is substitutes for existing polymer composites, and the like. The patent also relates to methods of making the electrically conductive and non-conductive polymer composite materials. The conducting polymer composite is the blend of conducting polymer and conducting filler wherein the conducting filler is electro-conductive fillers selected from the group consisting of graphite, carbon black, carbon fiber, carbon nanofiber, carbon nanotubes, intrinsically conducting materials, and mixtures thereof. The patent provides rapid, facile and low-cost methods for making conductive and non-conductive polymer composites, wherein the polymer composites are manufactured by in situ polymerization at room temperature. Within a short period time (preferentially for example, less than 10 minutes) after being administered, the composition forms a network that develops
with high strength and functional (for example, electrically conductive) composites. The resulting composites can be molded into any shape and/or size and exhibits excellent mechanical properties. According to one aspect, the invention provides methods for making polymer composites from cyanoacrylate monomers and starches as filler by in situ polymerization. In another aspect, the invention provides methods for making conducting polymer composites from using the polymerized cyanoacrylate-starch polymer composites as a matrix.
[006] US 20150284141 Al relates to multi-layered materials as anti-static shield comprising an electrically conductive layer and a support layer. This invention relates to anti-static materials which protect devices which are sensitive to electrostatic discharge and/or shock. The electrically conductive layer consists of an electrically conductive polymer or an electrically conductive polymer composite. The conjugated conductive polymer used for making electrically conductive layer comprises poly(phenylenevinylenes), polyfluorenes, poly(spirobifluorenes), polythiophenes, poly(p-phenylenes), poly(anilines), poly(pyrroles), copolymers thereof, or mixtures thereof.
[007] WO 2013127500 Al discloses the fabrication of a layered structure which can be employed in the field of polarization filters, in particular for shielding polarization filters from electrostatic discharge and electromagnetic radiation. The shielding can serve on the one hand to increase the stability of polarization filters and on the other hand to improve the quality of the filters. The patent furthermore relates to a process for the production of a layered structure which can be employed as shielding for polarization filters, and a device having a layered construction according to the patent. The layered structure according to invention comprises cellulose ester as polarizer layer and at least one conductor layer comprising a conductive polymer. The conductive polymer is chosen from the
group consisting of a thiophene, a polyacetylene, a polyparaphenylene, a polyaniline and a polypyrrole or a mixture of at least two of these.
OBJECTS OF THE INVENTION:
[008] The primary objective of the present invention is development of Conducting Polymer-assisted carbon foam as antistatic shield material for electronic components, chip carriers, electrostatically sensitive components and protecting them from potentially damages from electrostatic charges.
[009] Another objective of the invention to design conducting polymer composite incorporating filler materials and by selecting a medium of synthesis of prepared composite.
SUMMARY OF THE INVENTION
[0010] The present invention provides a process of synthesizing conducting polymers with a filler material coated over a carbon foam substrate in aqueous medium. The method comprising synthesis of conducting polymer Poly(aniline-co-pyrrole) coated over carbon foam substrate in an aqueous medium; testing the antistatic properties by John Chubb Instrument (JCI 155 v5) charge decay test unit; and ntistatic performance of prepared composite (50 x 70 mm Dimensions) by measuring the time on applying the positive as well as negative high corona voltage of 5000 V on the surface of material to be tested and recorded the decay time at 10 % cutoff.
[0011] The present invention precisely provides a process of synthesizing conducting polymers with a filler material coated over a carbon foam substrate in aqueous medium, said process comprising the steps of using blank carbon fibre as antistatic shield material; adding 0.05 - 0.2 M aniline to 0.05 - 0.2 M pyrrole
monomers; mixing 0.05 - 0.2 M Sodium dodecyl Sulphate (SDS) solution into the mixture of second step; homogenizing at 10000 - 15000 rpm for 2 hrs to form a stable emulsion, wherein after homogenization the carbon foam used as substrate cut with the dimension of 50mmx70mm on which coating is performed; mixing the resultant emulsion with carbon foam; adding 0.05 - 0.2 gm graphene to the resultant mixture; adding 0.05 - 0.2 M APS dropwise to the resultant mixture; and shaking up to 6 hrs prepared sample was filtered, washed and dried in oven at 50 °C in order to get the final product.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] In the drawings accompanying this specification:-
Fig. 1: Schematic of the synthesis of Poly(aniline-co-pyrrole)-deposited carbon foam composite by chemical oxidative polymerization process.
Fig. 2: XRD pattern of (a) Carbon foam (b) Poly(aniline-co-pyrrole)-Carbon Foam (c) Poly(aniline-co-pyrrole)-Carbon Foam-Graphene Composite
Fig. 3: FE-SEM images of (a) bare carbon foam (b) Poly(aniline-co-pyrrole)-Carbon Foam (c) Poly(aniline-co-pyrrole)-Graphene composite grafted on carbon foam
Fig. 4: Antistatic results of (a) Carbon Foam (b) Poly(aniline-co-pyrrole)-Carbon Foam (c) Poly(aniline-co-pyrrole)-Carbon Foam-Graphene composite
DETAILED DESCRIPTION OF THE INVENTION
[0013] At the very outset of the detailed description, it may be understood that the ensuing description only illustrates a particular form of this invention. However, such a particular form is only exemplary embodiment, and without intending to imply any limitation on the scope of this invention. Accordingly, the description is
to be understood as an exemplary embodiment and teaching of invention and not intended to be taken restrictively.
[0014] Throughout the description and claims of this specification, the phrases "comprise" and "contain" and variations of them mean "including but not limited to", and are not intended to exclude other moieties, additives, components, integers or steps. Thus, the singular encompasses the plural unless the context otherwise requires. Wherever there is an indefinite article used, the specification is to be understood as contemplating plurality as well as singularity, unless the context requires otherwise.
[0015] Features, integers, characteristics, compounds, chemical moieties or groups described in conjunction with a particular aspect, embodiment or example of the invention are to be understood to be applicable to any other aspect, embodiment or example described herein unless incompatible therewith. All of the features disclosed in this specification (including any accompanying claims, abstract and drawings), and/or all of the steps of any method or process so disclosed, may be combined in any combination, except combinations where at least some of such features and/or steps are mutually exclusive. The invention is not restricted to the details of any foregoing embodiments. The invention extends to any novel one, or any novel combination, of the features disclosed in this specification including any accompanying claims, abstract and drawings or any parts thereof, or to any novel one, or any novel combination, of the steps of any method or process so disclosed.
[0016] The reader's attention is directed to all papers and documents which are filed concurrently with or previous to this specification in connection with this application and which are open to public inspection with this specification, and
the contents of all such papers and documents are incorporated herein by reference. Post filing patents, original peer reviewed research paper shall be published.
5 [0017] Materials and Reagents Used: Pyrrole and Aniline (99% Sigma-Aldrich) was purified by distillation at reduced pressure and stored in a refrigerator before use. Sodium dodecyl sulfonate (SDS) (Merck chemicals, India) used as a dopant, Ammonium per sulphate (APS) (Merck chemicals, India) used as oxidant and hydroxyl peroxide (H2O2, 30% solution) (Merck chemicals, India) used as a co-10 oxidant. Acetone, methanol, and chloroform are all analytical grade reagents purchased from Rankem Limited, India, and were used as received. Graphene (XG Sciences, United States) was used as such without any purification. Double deionized water (specific resistivity of 10 Ω cm) was used to prepare aqueous solutions. Carbon Foam purchased from Toray, USA.
15
[0018] The present invention describes a process for synthesizing Poly(aniline-co-pyrrole) with Graphene deposit over carbon foam by using SDS as dopant, APS as oxidant and carbon foam as substrate in an aqueous medium. The method comprises synthesizing Poly(aniline-co-pyrrole) with graphene as filler deposited
20 over carbon foam substrate wherein SDS and APS used as dopant and oxidant during the oxidative polymerization of aniline and pyrrole monomers, then testing the antistatic properties by John Chubb Instrument (JCI 155 v5) charge decay test unit. Antistatic performance of prepared composite (50 x 70 mm dimensions) by measuring the time on applying the positive as well as negative high corona
25 voltage of 5000 V on the surface of material to be tested and recorded the decay time at 10 % cutoff. The polymer chosen for deposition over carbon foam substrate is Poly(aniline-co-pyrrole) and the like. The medium of polymerisation was aqueous i.e. deionised water used as solvent and the like. The dopant and oxidant chosen was Sodium dodecyl sulphate (SDS) and ammonium per sulphate
8
(APS) during the polymerization of monomer thiophene and the like. The conducting polymer encapsulated with graphene and deposited over carbon foam substrate. The prepared samples tested by John Chubb Instrument (JCI 155 v5) charge decay test unit. The antistatic performance of prepared composite (50 x 70 5 mm2 Dimensions) evaluated by measuring the decay time on applying the positive as well as negative high corona voltage of 5000 V on the surface of material to be tested and recorded the decay time at 10 % cutoff.
[0019] The Poly(aniline-co-pyrrole) coated over carbon foam was prepared by in-10 situ chemical oxidative polymerization of aniline and pyrrole monomers in the presence of APS. Initially, 0.05 – 0.2 M aniline and pyrrole monomers and 0.05 – 0.2 M SDS used as dopant was taken in a beaker and then homogenized at 10000 – 15000 rpm for 2 hrs in ultrasonicator to form a stable emulsion. After homogenization, the carbon foam used as substrate cut with the dimension of 15 50mm×70mm on which coating will perform is put into the emulsion of above prepared mixture and allowed to soak with the emulsion. After those 0.05 – 0.2 M APS taken into the burette and was added drop wise to the solution with continuous shaking on a rotary shaker by providing 0-10 C temperature to the reaction by placing large ice cubes around the rotary shaker for 24 hrs.
20
[0020] For the preparation of SDS doped Poly(aniline-co-pyrrole) deposited on Carbon Foam with Graphene, the protocol used at the first Step is to take 0.05 – 0.2 M aniline and pyrrole monomers and 0.05 – 0.2 M Sodium dodecyl Sulphate (SDS) solution was taken in beaker and then homogenized at 10000 - 15000 rpm 25 for 2 hrs to form a stable emulsion. After that, obtained product in step 1 is mixed with the carbon foam with dimensions 50 mm×70 mm by put into the emulsion solution. Then, 0.05 – 0.2 gm graphene is added into the above prepared mixture with carbon foam. Then, 0.05 – 0.2 M APS solution act as oxidant for polymerisation reaction is taken in a burette and added drop wise to the above
9
prepared solution with continuously shaking on a rotary shaker by providing 0-5 ºC temperature to the reaction by placing large ice cubes. Then after continuous shaking up to 6hrs prepared sample was filtered, washed and dried in oven at 50 °C in order to get final product.
5
Embodiments
[0021] In one embodiment of the invention, the monomers chosen for study were aniline and pyrrole.
[0022] In another embodiment of the invention, the substrate used for deposition 10 of Poly(aniline-co-pyrrole) layer on the Carbon foam.
[0023] In another embodiment of the invention, the medium of polymerization choose is aqueous (Deionized Water used as solvent).
[0024] In another embodiment of the invention, the dopant and oxidant chosen for above study was Sodium Dodecyl sulphate (SDS) and Ammonium per Sulphate 15 (APS).
[0025] In yet another embodiment of the invention, the temperature of the polymerization condition was kept between 0-5°C.
[0026] In yet another embodiment of the invention, dopant to monomer and oxidant to monomer ratio was kept 1:1.
20 [0027] In still another embodiment of the invention, the medium for the study was aqueous i.e. deionised water used as solvent.
[0028] In still another embodiment of the invention, the polymerisation reaction time was kept between 6-8 hours.
[0029] In further embodiment of the invention, the obtained composite was dried 25 in vacuum oven at 50°C.
10
[0030] In still further embodiment of the invention, the prepared samples antistatic properties tested by John Chubb Instrument (JCI 155 v5) charge decay test unit.
Table 1: Room temperature anti-static decay (s) time from JCI plots
S. No. Sample Antistatic Decay (s)
1/e 10%
1. Carbon Foam 0.169 0.51
2. Poly(aniline-co- 0.146 0.43 pyrrole)-Carbon
Foam
3. Poly(aniline-co- 0.138 0.28
pyrrole)-Graphene-
Carbon Foam
5
[0031] The following examples are given to illustrate the process of the present invention and should not be construed to limit the scope of the present invention. However, the best mode requirement is served through the examples.
Example 1
10 Synthesis of SDS doped Poly(aniline-co-pyrrole) deposited on Carbon Foam:
[0032] The Poly(aniline-co-pyrrole) coated over carbon foam was prepared by in-situ chemical oxidative polymerization of aniline and pyrrole monomers in the presence of APS. Initially, 0.1 M aniline and pyrrole monomers was taken and 0.1 M SDS used as dopant was taken in a beaker and then homogenized at 12000 rpm 15 for 2 hrs in ultrasonicator to form a stable emulsion. After homogenization, the carbon foam used as substrate cut with the dimension of 50mm×70mm on which
11
coating will be performed, is put into the emulsion of above prepared mixture and allowed to soak with the emulsion. After those 0.1 M APS taken into the burette and was added drop wise to the solution with continuous shaking on a rotary shaker by providing 0-5 °C temperature to the reaction by placing large ice cubes around the rotary shaker for 24 hrs.
Example 2
Synthesis of SDS doped Poly(aniline-co-pyirole) deposited on Carbon Foam with Graphene:
[0033] In the first step, O.IM aniline and pyrrole monomers and O.IM Sodium dodecyl Sulphate (SDS) solution was taken in beaker and then homogenized at 10000 - 15000 rpm for 2 hrs to form a stable emulsion. After that, obtained product in step 1 is mixed with the carbon foam with dimensions 50mmx70mm by put into the emulsion solution. Then, O.lgm graphene is added into the above prepared mixture with carbon foam. Then, 0.1M APS solution act as oxidant for polymerisation reaction is taken in a burette and added drop wise to the above prepared solution with continuously shaking on a rotary shaker by providing 0-5 °C temperature to the reaction by placing large ice cubes. Then after continuous shaking up to 6 hrs prepared sample was filtered, washed and dried in oven at 50 °C in order to get the final product.
We Claim:
A process for preparing polymer-graphene grafted carbon foam composite as an antistatic shield material, said process comprising the steps of:
a) using blank carbon foam as antistatic shield material;
b) adding 0.05 - 0.2 M aniline to 0.05 - 0.2 M pyrrole monomers;
c) mixing 0.05 - 0.2 M Sodium dodecyl Sulphate (SDS) solution into the mixture of second step;
d) homogenizing at 10000 - 15000 rpm for 2 hrs to form a stable emulsion;
e) mixing the resultant emulsion with carbon foam;
f) adding 0.05 - 0.2 gm graphene to the resultant mixture;
g) adding 0.05 - 0.2 M APS dropwise to the resultant mixture; and
h) shaking up to 6 hrs prepared sample was filtered, washed and dried in oven at 50 °C in order to get the final product.
The process as claimed in claim 1, wherein 0.1 M aniline is added.
The process as claimed in claim 1, wherein 0.1 M pyrole is added.
The process as claimed in claim 1, wherein 0.1 M SDS is added.
The process as claimed in claim 1, wherein 0.1 M APS is added.
The process as claimed in claim 1, wherein homogenization is performed at 12000 rpm.
The process as claimed in claim 1, wherein after homogenization the carbon foam used as substrate cut with the dimension of 50mmx70mm on which coating is performed.
The process as claimed in claim 1, wherein 0.1 gm graphene is added.
The process as claimed in claim 1, wherein said shaking on a rotary shaker is performed at 0-5 °C temperature, wherein further said cooling is performed by placing ice cubes.
| # | Name | Date |
|---|---|---|
| 1 | 201811016784-STATEMENT OF UNDERTAKING (FORM 3) [03-05-2018(online)].pdf | 2018-05-03 |
| 2 | 201811016784-FORM 1 [03-05-2018(online)].pdf | 2018-05-03 |
| 3 | 201811016784-DRAWINGS [03-05-2018(online)].pdf | 2018-05-03 |
| 4 | 201811016784-DECLARATION OF INVENTORSHIP (FORM 5) [03-05-2018(online)].pdf | 2018-05-03 |
| 5 | 201811016784-COMPLETE SPECIFICATION [03-05-2018(online)].pdf | 2018-05-03 |
| 6 | abstract.jpg | 2018-06-21 |
| 7 | 201811016784-FORM 18 [01-02-2022(online)].pdf | 2022-02-01 |
| 8 | 201811016784-POA [09-05-2022(online)].pdf | 2022-05-09 |
| 9 | 201811016784-FORM 13 [09-05-2022(online)].pdf | 2022-05-09 |
| 10 | 201811016784-AMENDED DOCUMENTS [09-05-2022(online)].pdf | 2022-05-09 |
| 11 | 201811016784-FER.pdf | 2022-07-20 |
| 12 | 201811016784-OTHERS [18-01-2023(online)].pdf | 2023-01-18 |
| 13 | 201811016784-FER_SER_REPLY [18-01-2023(online)].pdf | 2023-01-18 |
| 14 | 201811016784-CORRESPONDENCE [18-01-2023(online)].pdf | 2023-01-18 |
| 15 | 201811016784-COMPLETE SPECIFICATION [18-01-2023(online)].pdf | 2023-01-18 |
| 16 | 201811016784-CLAIMS [18-01-2023(online)].pdf | 2023-01-18 |
| 17 | 201811016784-US(14)-HearingNotice-(HearingDate-04-09-2023).pdf | 2023-08-18 |
| 18 | 201811016784-Proof of Right [02-09-2023(online)].pdf | 2023-09-02 |
| 19 | 201811016784-Correspondence to notify the Controller [02-09-2023(online)].pdf | 2023-09-02 |
| 20 | 201811016784-Written submissions and relevant documents [16-09-2023(online)].pdf | 2023-09-16 |
| 21 | 201811016784-RELEVANT DOCUMENTS [16-09-2023(online)].pdf | 2023-09-16 |
| 22 | 201811016784-PETITION UNDER RULE 137 [16-09-2023(online)].pdf | 2023-09-16 |
| 23 | 201811016784-Annexure [16-09-2023(online)].pdf | 2023-09-16 |
| 24 | 201811016784-PatentCertificate25-09-2023.pdf | 2023-09-25 |
| 25 | 201811016784-IntimationOfGrant25-09-2023.pdf | 2023-09-25 |
| 1 | SearchHistory(10)E_19-07-2022.pdf |