Title of Invention	"METHOD FOR PREPARATION OF ZINC OXIDE NANOPARTICLE SYNTHESIS USING SOLAR ENERGY"
Abstract	Present invention reports a novel method for the synthesis of zinc oxide nanoparticles using solar energy as a driving force. Zinc oxide nanoparticles are synthesized by zinc acetate as a precursor with 1,4-butanediol as a solvent and the use of solar energy as an energy source. The process was carried out in presence or absence of capping agent. Starch was used as a capping agent. The process is novel as it does not require any other conventional and expensive energy source. This method avoids high temperature heating i.e. calcinations in the zinc oxide nanoparticles synthesis reported in the conventional methods. The size of zinc oxide nanoparticles were found to be in the range of 1-100 nm.

Title of Invention

"METHOD FOR PREPARATION OF ZINC OXIDE NANOPARTICLE SYNTHESIS USING SOLAR ENERGY"

Abstract

Present invention reports a novel method for the synthesis of zinc oxide nanoparticles using solar energy as a driving force. Zinc oxide nanoparticles are synthesized by zinc acetate as a precursor with 1,4-butanediol as a solvent and the use of solar energy as an energy source. The process was carried out in presence or absence of capping agent. Starch was used as a capping agent. The process is novel as it does not require any other conventional and expensive energy source. This method avoids high temperature heating i.e. calcinations in the zinc oxide nanoparticles synthesis reported in the conventional methods. The size of zinc oxide nanoparticles were found to be in the range of 1-100 nm.

Full Text	FORM 2 THE PATENTS ACT, 1970 (39 OF 1970) & THE PATENTS RULES, 2003 COMPLETE SPECIFICATION (Section 10 and rule 13 ) 1. "Method for Zinc oxide nanoparticle synthesis using solar Energy." 2. (a) Bhanage Bhalchandra Mahadeo (b) Department of Chemistry, Institute of Chemical Technology, Nathalal Parekh Marg., Matunga. Mumbai 400019, Maharashtra, India. (c) INDIAN. The following specification particularly describes the invention and the manner in which it is to be performed. FIELD OF THE INVENTION The metal oxide nanoparticle synthesis is in high demand due to their extensive range of applications in various fields. From last few decades different types of methods have been developed for the synthesis. The novel method for metal oxide nanoparticles synthesis has been studied in this invention, which deals with the synthesis of zinc oxide nanoparticles using naturally available solar energy as an energy source. Application of solar energy makes this technique greener, economically cheaper and safer as compared reported methods. The obtained nanoparticles are in the range of 1-100 nm size. BACKGROUND OF THE INVENTION In the field of Material science nanomaterial synthesis had proven the greatest demand due to its frequent applications in fields like electronics, photonics, catalysis and biomedical sensing. Nanoparticles are showing their characteristic properties which are different from bulk because of large surface to volume ratio. Zinc oxide nanoparticles, have been attracting much attention due to wide range of applications in solar cells, gas sensors, optoelectronic devices, light emitting diodes optical waveguides and laser diodes. Till date different techniques are developed for the synthesis of zinc oxide nanocrystallites, including sol gel method, microwave synthesis, wet chemical synthesis, hydrothermal synthesis, chemical vapor deposition. However most of these techniques tend to be expensive due to the use of sophisticated equipments or setup and the use of conventional energy sources like hydrocarbons, electricity etc as a driving force for the synthesis. In addition these conventional energy sources are directly or indirectly responsible for the problem of global warming by continuous emission of carbon dioxide. So the attention has been put up to develop the greener and cheaper method for the synthesis of zinc oxide nanoparticles by replacement of conventional energy sources with available renewable energy sources like sunlight, wind, rain, tides, and geothermal heat. Solar energy is widely considered to be the largest source of carbon neutral renewable energy source. As compared to chemical reagent, sunlight is non-toxic, non-polluting, and traceless in chemical processes. Earlier, nanoparticles synthesis using solar energy was used for the synthesis of gold. Y. Luo [Materials Letters 2008, 62, 3770-3772] reported the Size-controlled preparation of dendrimer-protected gold nanoparticles by application of sunlight. Followed to this X. Luo [Colloid Journal 2009, 71, 281-284.] reported the one step dendrimer-protected gold nanoparticles by solar energy. In addition to this recently, Chien et al. [Green Chem. 2011, 13, 1162-1166] reported the synthesis of gold nanoparticles in which they exposed gold salt to sunlight for 5 h. However these methods cannot be extended further due to different amount of solar radiation and different intensity of solar radiation required for other metal or metal oxide nanoparticles. Therefore these methods cannot be extended further for other metal or metal oxide nanoparticles synthesis. The intention of this creation is to provide the strategy which is economical for the synthesis of zinc oxide nanoparticle by replacing conventional energy source like heat, electricity, hydrocarbons etc. by using renewable energy sources like sunlight, wind, rain, tides, and geothermal heat. The use of solar radiations in zinc oxide nanoparticles synthesis makes the technique specifically different than those reported previously. In literature there is no method which shows zinc oxide nanoparticles synthesis using solar radiation. SUMMARY OF THE INVENTION: The major aspect of the present invention is associated with the zinc oxide nanoparticles synthesis by the application of solar energy. Since the energy source is naturally available and it does not require any sophisticated equipment or setup this synthesis protocol observed to be economical compared to the reported methods. This method avoids higher temperature heating step i.e. calcinations step which is essential in the conventional synthesis. Use of solar energy and starch make the protocol green, clean and safe. DETAIL DESCRIPTION OF THE INVENTION: This innovation include the synthesis of zinc oxide nanoparticles using solar radiations as an energy source using 1,4-butane diol as a solvent and with/without using capping agent. Starch may be used as a capping agent An Important feature of the present invention relates to develop novel method for the synthesis of zinc oxide nanoparticles using environmentally available energy source. The scheme higher temperature heating step i.e. calcinations step. The characterisation of zinc oxide nanoparticle synthesised by this technique was done by various analytical methods like UV-vis spectroscopy, X-ray diffraction (XRD), Transmission Electron Microscopy (TEM), Field Emission Gun-Scanning Electron Microscopy (FEG-SEM), Energy dispersive X-ray Spectral analysis (EDS) which established that ZnO nanoparticles are formed in the nano range of 1-100 nm. Until now, there is not a single report which is known for the preparation of zinc oxide nanoparticles using solar energy as an energy source. So here we are reporting economically cheaper and greener way for the synthesis of zinc oxide nanoparticles. The process of the invention is described in detail in the example given below that is presented by the way of illustration only and should not be confined to limit the scope of the present invention. EXAMPLE 1: In a typical synthesis of zinc oxide nanoparticles a mixture of 1 g zinc acetate, 0.2 g starch as a capping agent and 5 mL 1,4-butanediol as a solvent was taken in a 50 mL glass beaker. This mixture was irradiated under solar radiations concentrated by Fresnel lens at noon in summer for 6 hrs. To isolate synthesized zinc oxide nanoparticles the reaction mixture was centrifuged at 8000 rpm for 25 min. The obtained precipitate was washed thrice with distilled water and absolute ethanol then dried at 80 °C for 5 hrs under vacuum. EXAMPLE 2: The charge similar to that of given in examplel here the volume of 1,4-butanediol was doubled i.e. 10 mL and the reaction mixture was irradiated by solar radiations (The radiations were concentrated by using 'Fresnel lens') for 6 h. at noon time. EXAMPLE 3: The charge similar to that of given in example 1 was taken except that the reaction mixture was irradiated by solar radiations (The radiations were concentrated by using 'Fresnel lens') for 10 h at noon time. EXAMPLE 4: The charge similar to that of given in examplel but here the reaction was carried out in absence of capping agent (starch) and the reaction mixture was irradiated by solar radiations (The radiations were concentrated by using 'Fresnel lens') for 6 h at noon time. EXAMPLE 5: The charge similar to that of given in example 4 was taken except that the reaction mixture was irradiated by solar radiations (The radiations were concentrated by using 'Fresnel lens') for 10 hat noon time. EXAMPLE 6: The charge similar to that of given in example 4 here the volume of 1,4-butanediol was doubled i.e. 10 mL and the reaction mixture was irradiated by solar radiations (The radiations were concentrated by using 'Fresnel lens') for 6 h. at noon time. In all above examples the white colour precipitate formation indicates the zinc oxide nanoparticle synthesis which further supported by the UV-vis analysis in which the λmax obtained at 367.40 nm which due to the zinc oxide nanoparticles [Figure 1], Crystalline pattern of synthesized zinc oxide nanoparticles was determined by the XRD analysis [Figure 2]. The particle shape and size were characterised by transmission electron microscopy [Figure 3], The particle size and shape also confirmed by Field Emission Gun-Scanning Electron Microscopy (FEG-SEM). The elemental analysis was done by Energy -dispersive X-ray Spectral analysis (EDS) showing the presence of Zn and 0 only [Figure 4]. I Claim: 1. A method for preparation of zinc oxide nanoparticles in the range of 1 -100 nm using solar energy irradiation with a solution of zinc acetate as a precursor and 1,4-butanediol as a solvent with/without starch as a capping agent. 2. A process as claimed in claim 1, wherein the metal precursors are selected from Zinc acetate, Zinc nitrate, Zinc chloride, Zinc Carbonate. 3. A process as claimed in claim 1, wherein solvents are selected from ethylene glycol, 1,2-propylene glycol, 1,3-propylene glycol, 1,4-butanediol. 4. A process as claimed in claim 1, wherein capping agents are selected from starch, Poly (vinyl pyrrolidone)[ PVP (MW-30000)], Poly (vinyl pyrrolidone)[ PVP ( MW-40000)]. 5. A process as claimed in claim 1, wherein the reaction is in the temperature range of 30-90 °C under atmospheric pressure. 6. A process as claimed in claim 1, wherein time required are selected from 3h to 20 h. 7. A process as claimed in claiml wherein concentration of zinc precursor is in the range of I mmol-100 mmol.

Full Text

FORM 2
THE PATENTS ACT, 1970
(39 OF 1970)
&
THE PATENTS RULES, 2003
COMPLETE SPECIFICATION
(Section 10 and rule 13 )
1. "Method for Zinc oxide nanoparticle synthesis using solar Energy."
2. (a) Bhanage Bhalchandra Mahadeo
(b) Department of Chemistry, Institute of Chemical Technology, Nathalal Parekh Marg., Matunga. Mumbai 400019, Maharashtra, India.
(c) INDIAN.
The following specification particularly describes the invention and the manner in which it is to be performed.

FIELD OF THE INVENTION
The metal oxide nanoparticle synthesis is in high demand due to their extensive range of applications in various fields. From last few decades different types of methods have been developed for the synthesis. The novel method for metal oxide nanoparticles synthesis has been studied in this invention, which deals with the synthesis of zinc oxide nanoparticles using naturally available solar energy as an energy source. Application of solar energy makes this technique greener, economically cheaper and safer as compared reported methods. The obtained nanoparticles are in the range of 1-100 nm size.
BACKGROUND OF THE INVENTION
In the field of Material science nanomaterial synthesis had proven the greatest demand due to its frequent applications in fields like electronics, photonics, catalysis and biomedical sensing. Nanoparticles are showing their characteristic properties which are different from bulk because of large surface to volume ratio.
Zinc oxide nanoparticles, have been attracting much attention due to wide range of applications in solar cells, gas sensors, optoelectronic devices, light emitting diodes optical waveguides and laser diodes. Till date different techniques are developed for the synthesis of zinc oxide nanocrystallites, including sol gel method, microwave synthesis, wet chemical synthesis, hydrothermal synthesis, chemical vapor deposition. However most of these techniques tend to be expensive due to the use of sophisticated equipments or setup and the use of conventional energy sources like hydrocarbons, electricity etc as a driving force for the synthesis. In addition these conventional energy sources are directly or indirectly responsible for the problem of global

warming by continuous emission of carbon dioxide. So the attention has been put up to develop the greener and cheaper method for the synthesis of zinc oxide nanoparticles by replacement of conventional energy sources with available renewable energy sources like sunlight, wind, rain, tides, and geothermal heat.
Solar energy is widely considered to be the largest source of carbon neutral renewable energy source. As compared to chemical reagent, sunlight is non-toxic, non-polluting, and traceless in chemical processes. Earlier, nanoparticles synthesis using solar energy was used for the synthesis of gold. Y. Luo [Materials Letters 2008, 62, 3770-3772] reported the Size-controlled preparation of dendrimer-protected gold nanoparticles by application of sunlight. Followed to this X. Luo [Colloid Journal 2009, 71, 281-284.] reported the one step dendrimer-protected gold nanoparticles by solar energy. In addition to this recently, Chien et al. [Green Chem. 2011, 13, 1162-1166] reported the synthesis of gold nanoparticles in which they exposed gold salt to sunlight for 5 h. However these methods cannot be extended further due to different amount of solar radiation and different intensity of solar radiation required for other metal or metal oxide nanoparticles. Therefore these methods cannot be extended further for other metal or metal oxide nanoparticles synthesis.
The intention of this creation is to provide the strategy which is economical for the synthesis of zinc oxide nanoparticle by replacing conventional energy source like heat, electricity, hydrocarbons etc. by using renewable energy sources like sunlight, wind, rain, tides, and geothermal heat. The use of solar radiations in zinc oxide nanoparticles synthesis makes the technique specifically different than those reported previously. In literature there is no method which shows zinc oxide nanoparticles synthesis using solar radiation.

SUMMARY OF THE INVENTION:
The major aspect of the present invention is associated with the zinc oxide nanoparticles synthesis by the application of solar energy. Since the energy source is naturally available and it does not require any sophisticated equipment or setup this synthesis protocol observed to be economical compared to the reported methods. This method avoids higher temperature heating step i.e. calcinations step which is essential in the conventional synthesis. Use of solar energy and starch make the protocol green, clean and safe.
DETAIL DESCRIPTION OF THE INVENTION:
This innovation include the synthesis of zinc oxide nanoparticles using solar radiations as an energy source using 1,4-butane diol as a solvent and with/without using capping agent. Starch may be used as a capping agent
An Important feature of the present invention relates to develop novel method for the synthesis of zinc oxide nanoparticles using environmentally available energy source. The scheme higher temperature heating step i.e. calcinations step.
The characterisation of zinc oxide nanoparticle synthesised by this technique was done by various analytical methods like UV-vis spectroscopy, X-ray diffraction (XRD), Transmission Electron Microscopy (TEM), Field Emission Gun-Scanning Electron Microscopy (FEG-SEM), Energy dispersive X-ray Spectral analysis (EDS) which established that ZnO nanoparticles are formed in the nano range of 1-100 nm.

Until now, there is not a single report which is known for the preparation of zinc oxide nanoparticles using solar energy as an energy source. So here we are reporting economically cheaper and greener way for the synthesis of zinc oxide nanoparticles.
The process of the invention is described in detail in the example given below that is presented by the way of illustration only and should not be confined to limit the scope of the present invention.
EXAMPLE 1:
In a typical synthesis of zinc oxide nanoparticles a mixture of 1 g zinc acetate, 0.2 g starch as a capping agent and 5 mL 1,4-butanediol as a solvent was taken in a 50 mL glass beaker. This mixture was irradiated under solar radiations concentrated by Fresnel lens at noon in summer for 6 hrs. To isolate synthesized zinc oxide nanoparticles the reaction mixture was centrifuged at 8000 rpm for 25 min. The obtained precipitate was washed thrice with distilled water and absolute ethanol then dried at 80 °C for 5 hrs under vacuum.
EXAMPLE 2:
The charge similar to that of given in examplel here the volume of 1,4-butanediol was doubled i.e. 10 mL and the reaction mixture was irradiated by solar radiations (The radiations were concentrated by using 'Fresnel lens') for 6 h. at noon time.
EXAMPLE 3:
The charge similar to that of given in example 1 was taken except that the reaction mixture was irradiated by solar radiations (The radiations were concentrated by using 'Fresnel lens') for 10 h at noon time.

EXAMPLE 4:
The charge similar to that of given in examplel but here the reaction was carried out in absence of capping agent (starch) and the reaction mixture was irradiated by solar radiations (The radiations were concentrated by using 'Fresnel lens') for 6 h at noon time.
EXAMPLE 5:
The charge similar to that of given in example 4 was taken except that the reaction mixture was irradiated by solar radiations (The radiations were concentrated by using 'Fresnel lens') for 10 hat noon time.
EXAMPLE 6:
The charge similar to that of given in example 4 here the volume of 1,4-butanediol was doubled i.e. 10 mL and the reaction mixture was irradiated by solar radiations (The radiations were concentrated by using 'Fresnel lens') for 6 h. at noon time.
In all above examples the white colour precipitate formation indicates the zinc oxide nanoparticle synthesis which further supported by the UV-vis analysis in which the λmax obtained at 367.40 nm which due to the zinc oxide nanoparticles [Figure 1], Crystalline pattern of synthesized zinc oxide nanoparticles was determined by the XRD analysis [Figure 2]. The particle shape and size were characterised by transmission electron microscopy [Figure 3], The particle size and shape also confirmed by Field Emission Gun-Scanning Electron Microscopy (FEG-SEM). The elemental analysis was done by Energy -dispersive X-ray Spectral analysis (EDS) showing the presence of Zn and 0 only [Figure 4].

I Claim:
1. A method for preparation of zinc oxide nanoparticles in the range of 1 -100 nm using solar energy irradiation with a solution of zinc acetate as a precursor and 1,4-butanediol as a solvent with/without starch as a capping agent.
2. A process as claimed in claim 1, wherein the metal precursors are selected from Zinc acetate, Zinc nitrate, Zinc chloride, Zinc Carbonate.
3. A process as claimed in claim 1, wherein solvents are selected from ethylene glycol, 1,2-propylene glycol, 1,3-propylene glycol, 1,4-butanediol.
4. A process as claimed in claim 1, wherein capping agents are selected from starch, Poly (vinyl pyrrolidone)[ PVP (MW-30000)], Poly (vinyl pyrrolidone)[ PVP ( MW-40000)].
5. A process as claimed in claim 1, wherein the reaction is in the temperature range of 30-90 °C under atmospheric pressure.
6. A process as claimed in claim 1, wherein time required are selected from 3h to 20 h.
7. A process as claimed in claiml wherein concentration of zinc precursor is in the range of I mmol-100 mmol.

Documents:

http://ipindiaonline.gov.in/patentsearch/GrantedSearch/viewdoc.aspx?id=PvNwSgX3nXkSmYFeeIJESg==&loc=vsnutRQWHdTHa1EUofPtPQ==

« Previous Patent

Next Patent »

Patent Number

271216

Indian Patent Application Number

3275/MUM/2011

PG Journal Number

07/2016

Publication Date

12-Feb-2016

Grant Date

09-Feb-2016

Date of Filing

22-Nov-2011

Name of Patentee

BHANAGE BHALCHANDRA MAHADEO

Applicant Address

DEPARTMENT OF CHEMISTERY INSTITUTE OF CHEMICAL TECHNOLOGY NATHALAL PAREKH MARG, MATUNGA (EAST), MUMBAI- 400 019 MAHARASHTRA, INDIA

Inventors:

#	Inventor's Name	Inventor's Address
1	LANKE SATISH ROHIDAS	DEPARTMENT OF CHEMISTERY INSTITUTE OF CHEMICAL TECHNOLOGY NATHALAL PAREKH MARG, MATUNGA (EAST), MUMBAI- 400 019 MAHARASHTRA, INDIA
2	PANDIT ANIRUDDHA BHALCHANDRA	DEPARTMENT OF CHEMISTERY INSTITUTE OF CHEMICAL TECHNOLOGY NATHALAL PAREKH MARG, MATUNGA (EAST), MUMBAI- 400 019 MAHARASHTRA, INDIA
3	PATIL ANIRUDDHA BALKRISHNA	DEPARTMENT OF CHEMISTERY INSTITUTE OF CHEMICAL TECHNOLOGY NATHALAL PAREKH MARG, MATUNGA (EAST), MUMBAI- 400 019 MAHARASHTRA, INDIA
4	BHANAGE BHALCHANDRA MAHADEO	DEPARTMENT OF CHEMISTERY INSTITUTE OF CHEMICAL TECHNOLOGY NATHALAL PAREKH MARG, MATUNGA (EAST), MUMBAI- 400 019 MAHARASHTRA, INDIA

PCT International Classification Number

B82Y30/00

PCT International Application Number

N/A

PCT International Filing date

PCT Conventions:

#	PCT Application Number	Date of Convention	Priority Country
1			NA