Title of Invention

FLUORESCENT COMPOSITION FOR GENERATING BLUE COLOUR IN SOLID STATE LIGHTING HAVING NS2 ACTIVATED ALKALI-ALKALINE EARTH COMPOUNDS

Abstract With the advent of GaN technology LEDs emitting around 390 nm have become available. These diodes are coated with phosphor blend, which on excitation by 390 nm emit in white. During last decade solid state lighting has emerged as a new area. The UV LED approach starts with a w-{/K(near UV)-emitting LED chip that energies phosphors designed to emit light in the visible spectrum by the phosphors. The colour mixing approach starts with discrete coloured sources and uses colour mixing optics to blend together the light output from these sources to create white light emission. We have developed new, highly intense blue emitting phosphors for n-UV diodes. They have not been patented so far. These phosphors will serve as indigenous replacement for blue component of phosphor blend for n-UV LED lamps. Our search for new, henceforth unreported phosphors led us to very efficient blue emitting ns2 doped Alkali-Alkaline Earth oxides, with a general formula I^a.^^yns2^)where, M1: Any one or two alkaline earth metals from Ca, Sr or Ba A/": Any alkali metal from Li or K ns2: Activator, any one metal out of Pb or Bi x: a fraction between 0.02-0.001. y: a fraction between 0-0.005
Full Text FORM 2
THE PATENT ACT, 1970 (39 of 1970)
&
The Patent Rules, 2003
-PRQVtSONAU COMPLETE SPECIFICATION
(see section 10 and rule 13)
1. TITLE OF THE INVENTION ;
Blue Fluorescent composition for solid state lighting and preparation method thereof



2. APPLICANTS
(a) NAME : Shri Ramdeobaba Kamla Nehru Engineering College,
Katol Road, Nagpur
(b) NATIONALITY: Indian
(c) ADDRESS : Physics Department,
Shri Ramdeobaba Kamla Nehru Engineering College, * Gittikhadan, Katol Road, Nagpur 440 013, Maharashtra, India
3. PREAMBLE TO THE DESCRIPTION :
The following specifications particularly describe and ascertain the nature of the invention and the manner in which the invention is to be performed

PROPOSED AMENDMENTOF COMPLETE SPECIFICATION IN PATENT APPLICATION NO. 81/MUM/2009
1. PROPOSED AMENDMENT NO. 1: in Column No. 3 of page 1 of Form No. 2, i.e
the complete specification, under Preamble to the description, the contents
thereof starting from the words "the following specification upto ... bottle"
be deleted and in pface thereof the words "The present application is a Blue Fluorescent composition for solid state lighting and preparation and method thereof and pertains to a totally new unreported highly efficient blue emitting phosphors for SSL application which would serve as blue component of the blend of phosphors to be applied on n-UV LED so as to convert near UV (typically 350-390 nm) emission to visible light. These phosphors will serve as indigenous replacement for blue component of phosphor blend for n-UV LED lamps." be inserted.
2. PROPOSED AMENDMENT NO. 2 : In detailed description of the Invention
starting at page 4 of the complete specification, add illustration no. 4 & 5 at the
end of page 5 as under :
Add "4. Typical preparation of (Sr,Ca)O.Pb : Ca0.69Sr0.30:Pb0.01 was prepared by precipitation method. Calculated weights of Ca(N03)2.4H20(1.629g)/ ), Sr(N03)2 (0.634 g) and Pb(NO3)2(0.033lg), were dissolved in 100 ml of double distilled water and was added to previous solution drop by drop till precipitation occurs. The solution was filtered and dried at 60°C - 80°C till precipitation is complete and precipitate dried completely. Solid powder was then heated for one and a half hours at 950°C. Resulting sample was collected and sealed a bottle. (excitation wavelength - 340 nm and 360 nm, emission wavelength - 470 nm) graphs of the following phosphor are being provided in figure 5.

General Formulae Phosphor for which graphs are provided
(Ca,Sr)0:Pb Ca0.69Sr0.3O:Pb0.01

5. Typical preparation of SrO:Pb : Sr.0.999O:Pb 0.001 was prepared by precipitation method. Calculated weights of Sr(N03)2(3g) and Pb(N03)2 (0.0046g), were dissolved in 100 ml of double distilled water with a few drops of Nitric Acid. Calculated quantity of (NH4)2(C03) (1.362g) was dissolved in double distilled water and was added to previous solution drop by drop till precipitation occurs. The solution was filtered and dried at 60CC - 80° C till it precipitated and dried completely. Solid powder was then heated for one and half hours at 950°C. Resulting samples were collected and sealed into a bottle. (Excitation wavelength - 268 nm, Emission wavelength - 450 nm).
Sr0.998O:Pb 0.002 was prepared by precipitation method. Calculated weights of Sr(N03)2(3g) and Pb(N03)2 (0.0094g), were dissolved in 100 ml of double distilled water with a few drops of Nitric Acid. Calculated quantity of (NH4)2(C03) (1.363g) was dissolved in double distilled water and was added to previous solution drop by drop till precipitation occurs. The solution was filtered and dried at 60°C - 80°C till it precipitated and dried completely. Solid powder was then heated for one and half hours at 950°C. Resulting samples were collected and sealed into a bottle. (Excitation wavelength - 268 nm, Emission wavelength -450nm).
Graphs of following phosphor are provided in figure 6.

General Formulae Phosphor for which graphs are provided
SrO:Pb Sr099O:Pb0.001

Sr0.99sO-Pb 0.002
Applicant states that preparation via above method and as per the above illustrations, has yielded to the desired results as claimed by the applicant, i.e. Blue Fluorescent or solid state lighting by low cost phosphor which can be excited by mere UV light, suitable for a solid state lighting based on the general formulae M1.x.yi.M11y:ns2xO where ns2 ions are the activators in alkali-alkaline earth oxide hosts."
3. PROPOSED AMENDMENT NO. 3: In Page no. 6 of the complete specification under the heading of Claims, Claim no. 1 to 5 be permitted to be corrected and replaced as following :
" 1. A Blue Fluorescent composition for solid state lighting and preparation method thereof wherein ns2 i.e. (Bi3+, Pb2+) which is activated alkali-alkaline earth oxide phosphor compositions having a general formula
Ml (I^y). Muy ns2xO where,

M: Any one or two alkaline earth metals from Ca, Sr or Ba
MII Any one alkali metal from Li or K
ns : Activator, any one metal out of Pb or Bi
x a fraction between 0.02-0.001.
y: a fraction between 0-0.005 which is achieved by the
aforesaid composition
2. A ns2 i.e. (Bi3+, Pb2+) which is an activator in the phosphor composition as claimed in claim 1, which is achieved by the composition Sr 0.98 O: Bi o.02
3. A ns2 i.e. (Bi3+, Pb2+) which is an activator in the phosphor composition as claimed in claim 1, which is also achieved by the composition Sr0. 994K0.005O:Bi0. 001
4. A ns2 i.e. (Bi3+, Pb2+) which is an activator in the phosphor composition as claimed in claim 1, which is also achieved by the composition (Sro.799 ,Ca0.2)O:Bi0.001
5. A process for synthesizing a ns2 i.e. (Bi3+, Pb2+) which is an activator in the phosphor composition, achieved via the process comprising steps, i.e.
a. dissolving alkaline earth nitrates, alkali carbonates, and ns nitrates
in double distilled water with a few drops of nitric acid.
b. Precipitating the corresponding carbonate with ammonium
carbonate
c. Filtering and drying the carbonates obtained in (b) at 60-80°C
d. Annealing the carbonates obtained in (c) for one and a half hour at
950°C to obtain the white crystalline phosphor powder
e. Sealing the obtained compositions after carrying steps sequencing
from (a) to (d) in a bottle.
4. PROPOSED AMENDMENT No. 4 : Claim No. 6 be permitted to be deleted and claim no. 7 & 8 be read as claim nos. 6 & 7 respectively as under:

" 6. A process as claimed in claim 5 above, wherein step (d), annealing is carried out at a temperature range of 950 for 1.5-2 hours,
7. ns i.e. (Bi3+, Pb +) doped Alkali-Alkaline Earth Oxide Phosphor compositions and Preparation thereof to be used as blue emitting component of the blend of Solid State Lighting Phosphor as used in n-UV LED substantially such as herein described with drawings and foregoing examples."
5. PROPOSED AMENDMENTNo. 5 : Title appearing on page 2 of specification under the headings - descriptions be deleted.
6. PROPOSED AMENDMENT: Figures No. 5 & 6 be permitted to be added as under after Figure 4 of the Drawings.
Figure 5:




PROPOSED AMENDMENTOF COMPLETE SPECIFICATION IN PATENT APPLICATION NO. 81/MUM/2009
1. PROPOSED AMENDMENT NO. 1: in Column No. 3 of page 1 of Form No. 2, i.e
the complete specification, under Preamble to the description, the contents
thereof starting from the words "the following specification upto ... bottle"
be deleted and in pface thereof the words "The present application is a Blue Fluorescent composition for solid state lighting and preparation and method thereof and pertains to a totally new unreported highly efficient blue emitting phosphors for SSL application which would serve as blue component of the blend of phosphors to be applied on n-UV LED so as to convert near UV (typically 350-390 nm) emission to visible light. These phosphors will serve as indigenous replacement for blue component of phosphor blend for n-UV LED lamps." be inserted.
2. PROPOSED AMENDMENT NO. 2 : In detailed description of the Invention
starting at page 4 of the complete specification, add illustration no. 4 & 5 at the
end of page 5 as under :
Add "4. Typical preparation of (Sr,Ca)O.Pb : Ca0.69Sr0.30:Pb0.01 was prepared by precipitation method. Calculated weights of Ca(N03)2.4H20(1.629g)/ ), Sr(N03)2 (0.634 g) and Pb(NO3)2(0.033lg), were dissolved in 100 ml of double distilled water and was added to previous solution drop by drop till precipitation occurs. The solution was filtered and dried at 60°C - 80°C till precipitation is complete and precipitate dried completely. Solid powder was then heated for one and a half hours at 950°C. Resulting sample was collected and sealed a bottle. (excitation wavelength - 340 nm and 360 nm, emission wavelength - 470 nm) graphs of the following phosphor are being provided in figure 5.

General Formulae Phosphor for which graphs are provided
(Ca,Sr)0:Pb Ca0.69Sr0.3O:Pb0.01

5. Typical preparation of SrO:Pb : Sr.0.999O:Pb 0.001 was prepared by precipitation method. Calculated weights of Sr(N03)2(3g) and Pb(N03)2 (0.0046g), were dissolved in 100 ml of double distilled water with a few drops of Nitric Acid. Calculated quantity of (NH4)2(C03) (1.362g) was dissolved in double distilled water and was added to previous solution drop by drop till precipitation occurs. The solution was filtered and dried at 60CC - 80° C till it precipitated and dried completely. Solid powder was then heated for one and half hours at 950°C. Resulting samples were collected and sealed into a bottle. (Excitation wavelength - 268 nm, Emission wavelength - 450 nm).
Sr0.998O:Pb 0.002 was prepared by precipitation method. Calculated weights of Sr(N03)2(3g) and Pb(N03)2 (0.0094g), were dissolved in 100 ml of double distilled water with a few drops of Nitric Acid. Calculated quantity of (NH4)2(C03) (1.363g) was dissolved in double distilled water and was added to previous solution drop by drop till precipitation occurs. The solution was filtered and dried at 60°C - 80°C till it precipitated and dried completely. Solid powder was then heated for one and half hours at 950°C. Resulting samples were collected and sealed into a bottle. (Excitation wavelength - 268 nm, Emission wavelength -450nm).
Graphs of following phosphor are provided in figure 6.

General Formulae Phosphor for which graphs are provided
SrO:Pb Sr099O:Pb0.001

Sr0.99sO-Pb 0.002
Applicant states that preparation via above method and as per the above illustrations, has yielded to the desired results as claimed by the applicant, i.e. Blue Fluorescent or solid state lighting by low cost phosphor which can be excited by mere UV light, suitable for a solid state lighting based on the general formulae M1.x.yi.M11y:ns2xO where ns2 ions are the activators in alkali-alkaline earth oxide hosts."
3. PROPOSED AMENDMENT NO. 3: In Page no. 6 of the complete specification under the heading of Claims, Claim no. 1 to 5 be permitted to be corrected and replaced as following :
" 1. A Blue Fluorescent composition for solid state lighting and preparation method thereof wherein ns2 i.e. (Bi3+, Pb2+) which is activated alkali-alkaline earth oxide phosphor compositions having a general formula
Ml (I^y). Muy ns2xO where,

M: Any one or two alkaline earth metals from Ca, Sr or Ba
MII Any one alkali metal from Li or K
ns : Activator, any one metal out of Pb or Bi
x a fraction between 0.02-0.001.
y: a fraction between 0-0.005 which is achieved by the
aforesaid composition
2. A ns2 i.e. (Bi3+, Pb2+) which is an activator in the phosphor composition as claimed in claim 1, which is achieved by the composition Sr 0.98 O: Bi o.02
3. A ns2 i.e. (Bi3+, Pb2+) which is an activator in the phosphor composition as claimed in claim 1, which is also achieved by the composition Sr0. 994K0.005O:Bi0. 001
4. A ns2 i.e. (Bi3+, Pb2+) which is an activator in the phosphor composition as claimed in claim 1, which is also achieved by the composition (Sro.799 ,Ca0.2)O:Bi0.001
5. A process for synthesizing a ns2 i.e. (Bi3+, Pb2+) which is an activator in the phosphor composition, achieved via the process comprising steps, i.e.
a. dissolving alkaline earth nitrates, alkali carbonates, and ns nitrates
in double distilled water with a few drops of nitric acid.
b. Precipitating the corresponding carbonate with ammonium
carbonate
c. Filtering and drying the carbonates obtained in (b) at 60-80°C
d. Annealing the carbonates obtained in (c) for one and a half hour at
950°C to obtain the white crystalline phosphor powder
e. Sealing the obtained compositions after carrying steps sequencing
from (a) to (d) in a bottle.
4. PROPOSED AMENDMENT No. 4 : Claim No. 6 be permitted to be deleted and claim no. 7 & 8 be read as claim nos. 6 & 7 respectively as under:

" 6. A process as claimed in claim 5 above, wherein step (d), annealing is carried out at a temperature range of 950 for 1.5-2 hours,
7. ns i.e. (Bi3+, Pb +) doped Alkali-Alkaline Earth Oxide Phosphor compositions and Preparation thereof to be used as blue emitting component of the blend of Solid State Lighting Phosphor as used in n-UV LED substantially such as herein described with drawings and foregoing examples."
5. PROPOSED AMENDMENTNo. 5 : Title appearing on page 2 of specification under the headings - descriptions be deleted.
6. PROPOSED AMENDMENT: Figures No. 5 & 6 be permitted to be added as under after Figure 4 of the Drawings.
Figure 5:

Documents:

360-MUMNP-2005-FORM 13(14-5-2012).pdf

81-MUM-2009-ABSTRACT(25-2-2013).pdf

81-mum-2009-abstract.doc

81-mum-2009-abstract.pdf

81-MUM-2009-CLAIMS(AMENDED)-(25-2-2013).pdf

81-mum-2009-claims.doc

81-mum-2009-claims.pdf

81-mum-2009-correspondence.pdf

81-mum-2009-description(complete).doc

81-mum-2009-description(complete).pdf

81-MUM-2009-DRAWING(25-2-2013).pdf

81-mum-2009-drawing.pdf

81-mum-2009-form 1.pdf

81-MUM-2009-FORM 13(8-5-2012).pdf

81-mum-2009-form 18.pdf

81-MUM-2009-FORM 2(TITLE PAGE)-(25-2-2013).pdf

81-mum-2009-form 2(title page).pdf

81-mum-2009-form 2.doc

81-mum-2009-form 2.pdf

81-mum-2009-form 3.pdf

81-mum-2009-form 5.pdf

81-MUM-2009-MARKED COPY(25-2-2013).pdf

81-MUM-2009-REPLY TO EXAMINATION REPORT(8-5-2012).pdf

81-MUM-2009-REPLY TO HEARING(25-2-2013).pdf

81-MUM-2009-SPECIFICATION(AMENDED)-(25-2-2013).pdf

81-MUM-2009-SPECIFICATION(AMENDED)-(8-5-2012).pdf

abstract1.jpg


Patent Number 255675
Indian Patent Application Number 81/MUM/2009
PG Journal Number 11/2013
Publication Date 15-Mar-2013
Grant Date 14-Mar-2013
Date of Filing 13-Jan-2009
Name of Patentee SHRI RAMDEOBABA KAMLA NEHRU ENGINEERING COLLEGE NAGPUR
Applicant Address PHYSICS DEPARTMENT, SHRI RAMDEOBABA KAMLA NEHRU ENGINEERING COLLEGE, GITTIKHADAN, KATOL ROAD, NAGPUR 440 013.
Inventors:
# Inventor's Name Inventor's Address
1 DEEPAK RADHESHYAM TAIKAR C/O PHYSICS DEPARTMENT, SHRI RAMDEOBABA KAMLA NEHRU ENGINEERING COLLEGE, GITTIKHADAN, KATOL ROAD, NAGPUR 440 013.
2 S. V. MOHARIL PHYSICS DEPARTMENT, NAGPUR UNIVERSITY CAMPUS, RTM NAGPUR UNIVERSITY, NAGPUR 440 010.
3 CHARUSHEELA PRAMOD JOSHI PHYSICS DEPARTMENT, SHRI RAMDEOBABA KAMLA NEHRU ENGINEERING COLLEGE, GITTIKHADAN, KATOL ROAD, NAGPUR 440 013.
PCT International Classification Number C09K11/85; C09K11/77
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 NA