US20030116501A1 - Process for preparing immobilized nano-sized metal particles - Google Patents
Process for preparing immobilized nano-sized metal particles Download PDFInfo
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- US20030116501A1 US20030116501A1 US10/032,206 US3220601A US2003116501A1 US 20030116501 A1 US20030116501 A1 US 20030116501A1 US 3220601 A US3220601 A US 3220601A US 2003116501 A1 US2003116501 A1 US 2003116501A1
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- 239000002105 nanoparticle Substances 0.000 title claims abstract description 23
- 239000002923 metal particle Substances 0.000 title claims description 12
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 238000000034 method Methods 0.000 claims abstract description 35
- 239000002184 metal Substances 0.000 claims abstract description 18
- 229910052751 metal Inorganic materials 0.000 claims abstract description 18
- 241000233866 Fungi Species 0.000 claims abstract description 17
- 229910052737 gold Inorganic materials 0.000 claims abstract description 13
- 150000002739 metals Chemical class 0.000 claims abstract description 7
- 229910052709 silver Inorganic materials 0.000 claims abstract description 6
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 4
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 3
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 3
- 229910052703 rhodium Inorganic materials 0.000 claims abstract description 3
- 229910052707 ruthenium Inorganic materials 0.000 claims abstract description 3
- 230000002538 fungal effect Effects 0.000 claims description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 229910021645 metal ion Inorganic materials 0.000 claims description 21
- 238000005119 centrifugation Methods 0.000 claims description 18
- 241000082085 Verticillium <Phyllachorales> Species 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 239000001963 growth medium Substances 0.000 claims description 10
- 239000002028 Biomass Substances 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 5
- 230000002378 acidificating effect Effects 0.000 claims description 4
- 238000011534 incubation Methods 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- 150000004649 carbonic acid derivatives Chemical class 0.000 claims description 2
- 150000004820 halides Chemical class 0.000 claims description 2
- 150000002823 nitrates Chemical class 0.000 claims description 2
- 239000011541 reaction mixture Substances 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 239000008223 sterile water Substances 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 abstract description 7
- -1 metals ions Chemical class 0.000 abstract description 5
- 238000010170 biological method Methods 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 4
- 239000000243 solution Substances 0.000 description 26
- 210000004027 cell Anatomy 0.000 description 17
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 11
- 239000010931 gold Substances 0.000 description 11
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 10
- 229920000742 Cotton Polymers 0.000 description 8
- 238000002474 experimental method Methods 0.000 description 8
- 238000001914 filtration Methods 0.000 description 8
- 238000011081 inoculation Methods 0.000 description 8
- 239000002609 medium Substances 0.000 description 8
- 238000004458 analytical method Methods 0.000 description 7
- 230000015572 biosynthetic process Effects 0.000 description 7
- 238000005259 measurement Methods 0.000 description 6
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 6
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 6
- 239000002245 particle Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000012620 biological material Substances 0.000 description 4
- 238000001506 fluorescence spectroscopy Methods 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 229910004042 HAuCl4 Inorganic materials 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- 230000036983 biotransformation Effects 0.000 description 3
- 238000005266 casting Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000000053 physical method Methods 0.000 description 3
- 238000004626 scanning electron microscopy Methods 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- 238000011179 visual inspection Methods 0.000 description 3
- 235000012431 wafers Nutrition 0.000 description 3
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 2
- 239000012736 aqueous medium Substances 0.000 description 2
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(II) nitrate Inorganic materials [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 2
- 238000003608 radiolysis reaction Methods 0.000 description 2
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 description 1
- 229910002621 H2PtCl6 Inorganic materials 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000010415 colloidal nanoparticle Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005251 gamma ray Effects 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 230000003100 immobilizing effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 238000001451 molecular beam epitaxy Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000012163 sequencing technique Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P1/00—Preparation of compounds or compositions, not provided for in groups C12P3/00 - C12P39/00, by using microorganisms or enzymes
- C12P1/02—Preparation of compounds or compositions, not provided for in groups C12P3/00 - C12P39/00, by using microorganisms or enzymes by using fungi
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12N—MICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA
- C12N1/00—Microorganisms, e.g. protozoa; Compositions thereof; Processes of propagating, maintaining or preserving microorganisms or compositions thereof; Processes of preparing or isolating a composition containing a microorganism; Culture media therefor
- C12N1/14—Fungi; Culture media therefor
- C12N1/145—Fungal isolates
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P3/00—Preparation of elements or inorganic compounds except carbon dioxide
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12R—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES C12C - C12Q, RELATING TO MICROORGANISMS
- C12R2001/00—Microorganisms ; Processes using microorganisms
- C12R2001/645—Fungi ; Processes using fungi
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S977/00—Nanotechnology
- Y10S977/70—Nanostructure
- Y10S977/701—Integrated with dissimilar structures on a common substrate
- Y10S977/702—Integrated with dissimilar structures on a common substrate having biological material component
- Y10S977/703—Cellular
Definitions
- the present invention relates to a process for preparing immobilized nano-sized metal particles. More particularly, the present invention relates to a new and improved process employing an efficient, easy and environmentally friendly method for preparing stable, immobilized colloidal nano-particles in aqueous solutions using naturally occurring bio-materials such as fungi.
- Nano-particles are extremely important materials in different areas ranging from nano-technology, non-linear optics, diode lasers, smart sensors, markers in drugs, gene sequencing to catalysis. Nano-materials can be obtained by various chemical and physical methods. Some examples of physical methods are vapour deposition, lithographic processes and molecular beam epitaxy (MBE). Chemical methods include the popular borohydride and citrate reduction methods for the preparation of colloidal metal (like gold, silver etc.) particles. Reference may be made to D. A. Handley, Colloidal Gold: Principles, Methods and Applications; Hayat, M. A. Editor, Academic Press, San Diego, Calif. 1989; Vol.1, Chapter 2, wherein details of such chemical routes are given.
- Reduction of metal ions by radiolysis is also conventionally used for preparing nano-sized metal particles.
- the methods mentioned above suffer from drawbacks such as being environmentally hazardous (chemical methods) and result in the quick agglomeration of nano-particles leading to big particles for poor monodispersity.
- the main object of the invention is to provide an improved process for preparing immobilized nano-sized metal particles using an environment friendly biological method.
- Another object of the invention is to provide a process which uses naturally occurring fungi under aqueous medium.
- Another object of the invention is to provide the process for preparation of nano-sized metal particles, which are deposited on to the fungus cell wall.
- Another object of the invention is to provide a process where the formation of nano-particles occurs on the surface of biomass and not in the solution.
- the present invention provides an improved process for preparing immobilized nano-sized metal particles, which comprises treating wet fungal mycelia with a metal ion solution at temperature in the range of 15 to 40° C. for a period in the range of 2 to 120 hours, separating the biomass to obtain the immobilized nano-sized metal particles deposited on to the surface of the fungal cells.
- the wet fungal mycelia is obtained by growing the Verticillium (AAT-TS-4) in a culture medium for a period of 2 to 120 hours at temperature ranging between 15-40° C. under aseptic conditions, separating the biomass by centrifugation, washing several times with sterile water, and then incubating the whole reaction mixture at 15 to 40° C. and atmospheric pressure.
- the metal ion solution is obtained by dissolving metal salts of group IB-VIIIB metals in water.
- the metal is selected from the group consisting of Au, Ag, Pd, Pt, Ni, Rh and Ru.
- the metal salts are selected from the group consisting of halides, nitrates and carbonates.
- the metal ion solution is obtained by dissolving the acidic form of metals in water.
- the acidic form of the metal is selected from chloroauric acid and chloroplatinic acid.
- concentration of metal ions per gram of wet fungal mycelia is in the range of 10 to 200 mg metal ions per gram of wet fungal mycelia.
- concentration of metal ions per gram of wet fungal mycelia is in the range of 10 to 100 mg metal ions per gram of wet fungal mycelia.
- concentration of metal ions per gram of wet fungal mycelia is in the range of 25 to 100 mg metal ions per gram of wet fungal mycelia.
- ratio of water to wet fungal mycelia is 100:1 (w/w)
- the fungus Verticillium designated as AAT-TS-4 is taken as whole cell as wet solid mass.
- reaction of the fungus and a source of metal ions in solution is carried out in water.
- the incubation/reaction temperature is in the range of 15-40° C., preferably 23-33° C., most preferably 25-29° C.
- UV-vis spectra of the clear aqueous solution after reaction with the mycelial cells for 72 h showed the absence of the characteristic plasmon resonance band of gold ca 433 nm indicating the absence of gold in the solution.
- UV-vis spectra of the clear aqueous solution after reaction with the mycelial cells for 72 h showed the absence of the characteristic plasmon resonance band of gold ca 533 nm indicating the absence of gold in the solution.
- UV-vis spectra of the clear aqueous solutions after reaction with the mycelial cells for 72 h showed the absence of the characteristic plasmon resonance band of gold ca 533 nm indicating the absence of gold in the solution.
- the present invention provides a new process using biological method for the preparation of immobilized nano particles of metals obviating the drawbacks of the prior art methods.
- the process of the present invention describes a new biological method, instead of chemical or physical methods for preparing immobilized metal particles. This is the first time that fungi are used to efficiently prepare immobilized nano-particles of various metals ions from their aqueous solutions.
- the immobilized nano-sized metal particles are stable.
- the method of the invention is simple and environmentally friendly.
- a single step method for obtaining immobilized nano-particles of metals [0049] A single step method for obtaining immobilized nano-particles of metals.
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- Zoology (AREA)
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- Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Biotechnology (AREA)
- Bioinformatics & Cheminformatics (AREA)
- General Health & Medical Sciences (AREA)
- Microbiology (AREA)
- Biochemistry (AREA)
- General Engineering & Computer Science (AREA)
- Mycology (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Botany (AREA)
- Medicinal Chemistry (AREA)
- Tropical Medicine & Parasitology (AREA)
- Virology (AREA)
- Biomedical Technology (AREA)
- Measuring Or Testing Involving Enzymes Or Micro-Organisms (AREA)
Abstract
The present invention provides a new process using biological method for the preparation of immobilized nano-particles of metals. Fungi are used to efficiently prepare immobilized nano-particles of various metals ions such as Au, Ag, Pd, Pt, Ni, Rh and Ru from their aqueous solutions.
Description
- The present invention relates to a process for preparing immobilized nano-sized metal particles. More particularly, the present invention relates to a new and improved process employing an efficient, easy and environmentally friendly method for preparing stable, immobilized colloidal nano-particles in aqueous solutions using naturally occurring bio-materials such as fungi.
- Nano-particles are extremely important materials in different areas ranging from nano-technology, non-linear optics, diode lasers, smart sensors, markers in drugs, gene sequencing to catalysis. Nano-materials can be obtained by various chemical and physical methods. Some examples of physical methods are vapour deposition, lithographic processes and molecular beam epitaxy (MBE). Chemical methods include the popular borohydride and citrate reduction methods for the preparation of colloidal metal (like gold, silver etc.) particles. Reference may be made to D. A. Handley, Colloidal Gold: Principles, Methods and Applications; Hayat, M. A. Editor, Academic Press, San Diego, Calif. 1989; Vol.1, Chapter 2, wherein details of such chemical routes are given. Reduction of metal ions by radiolysis is also conventionally used for preparing nano-sized metal particles. However, the methods mentioned above suffer from drawbacks such as being environmentally hazardous (chemical methods) and result in the quick agglomeration of nano-particles leading to big particles for poor monodispersity.
- Although specific capping agents are used in some of the abovementioned methods to restrict the size of the colloidal metal particles and to stabilize the particle size distribution, this makes the whole system quite complicated and user unfriendly. Another disadvantage, particularly of the radiolysis method, is that it is quite complicated and gamma ray sources are not readily available.
- The main object of the invention is to provide an improved process for preparing immobilized nano-sized metal particles using an environment friendly biological method.
- Another object of the invention is to provide a process which uses naturally occurring fungi under aqueous medium.
- Another object of the invention is to provide the process for preparation of nano-sized metal particles, which are deposited on to the fungus cell wall.
- Another object of the invention is to provide a process where the formation of nano-particles occurs on the surface of biomass and not in the solution.
- Accordingly the present invention provides an improved process for preparing immobilized nano-sized metal particles, which comprises treating wet fungal mycelia with a metal ion solution at temperature in the range of 15 to 40° C. for a period in the range of 2 to 120 hours, separating the biomass to obtain the immobilized nano-sized metal particles deposited on to the surface of the fungal cells.
- In an embodiment of the present invention the wet fungal mycelia is obtained by growing the Verticillium (AAT-TS-4) in a culture medium for a period of 2 to 120 hours at temperature ranging between 15-40° C. under aseptic conditions, separating the biomass by centrifugation, washing several times with sterile water, and then incubating the whole reaction mixture at 15 to 40° C. and atmospheric pressure.
- In another embodiment the metal ion solution is obtained by dissolving metal salts of group IB-VIIIB metals in water.
- In a further embodiment of the invention, the metal is selected from the group consisting of Au, Ag, Pd, Pt, Ni, Rh and Ru.
- In a further embodiment of the invention, the metal salts are selected from the group consisting of halides, nitrates and carbonates.
- In another embodiment the metal ion solution is obtained by dissolving the acidic form of metals in water.
- In a further embodiment of the invention, the acidic form of the metal is selected from chloroauric acid and chloroplatinic acid.
- In another embodiment of the invention concentration of metal ions per gram of wet fungal mycelia is in the range of 10 to 200 mg metal ions per gram of wet fungal mycelia.
- In another embodiment of the invention concentration of metal ions per gram of wet fungal mycelia is in the range of 10 to 100 mg metal ions per gram of wet fungal mycelia.
- In another embodiment of the invention concentration of metal ions per gram of wet fungal mycelia is in the range of 25 to 100 mg metal ions per gram of wet fungal mycelia.
- In yet another embodiment of the invention ratio of water to wet fungal mycelia is 100:1 (w/w) In another embodiment of the invention the fungus Verticillium designated as AAT-TS-4 is taken as whole cell as wet solid mass.
- In another embodiment of the invention, reaction of the fungus and a source of metal ions in solution is carried out in water.
- In another embodiment of the invention the incubation/reaction temperature is in the range of 15-40° C., preferably 23-33° C., most preferably 25-29° C.
- The process for the present invention is described herein below with examples that are illustrative and should not be construed to limit the scope of the present invention.
- In this experiment, 10 g of wet fungal mycelia (Verticillium AAT-TS-4), grown in a culture medium, separated from medium by centrifugation, washed several times with water through centrifugation, was taken in a autoclaved conical flask and then 100 ml solution of 100 mg of HAuCl 4 in water was added.
- The conical flask was then plugged with cotton and incubated at 27° C. Samples were collected periodically by filtration of solution containing the fungus inside the inoculation chamber under laminar flow condition. Bio-transformation was routinely monitored by visual inspection of the biomass as well as measurement of UV-vis spectra from the fungal cells.
- Films of the fungal cells (both before and after exposure to Au + ions for 72 h) for UV-vis spectroscopy and scanning electron microscopy (SEM) studies were prepared by solution casting fungal cells onto Si (111) wafers and thoroughly drying film in flowing N2. UV-vis spectroscopy measurement of films were made on a Shimadzu dual-beam spectrophotometer (model UV-1601PC) operating the reflection mode at a resolution of 2 run.
- These data confirm the presence of gold nano-particles on to the surface of the biomaterial. UV-vis spectra of the clear aqueous solution after reaction with the mycelial cells for 72 h showed the absence of the characteristic plasmon resonance band of gold ca 433 nm indicating the absence of gold in the solution.
- In this experiment, 10 g of wet fungal mycelia (Verticillium), grown in a culture medium, separated from medium by centrifugation, washed several times with water through centrifugation, was taken in an autoclaved conical flask and then a solution containing 25 mg of HAuCl 4 in 100 ml water was added.
- The conical flask was then plugged with cotton and incubated at 27° C. Samples were collected periodically by filtration of solution containing the fungus inside the inoculation chamber under laminar flow condition. Bio-transformation was routinely monitored by visual inspection of the biomass as well as measurement of the UV-vis spectra from the fungal cells.
- Films of the fungal cells (both before and after exposure to Au + ions for 72 h) for UV-vis spectroscopy and scanning electron microscopy (SEM) studies were prepared by solution casting the fungal cells onto Si (111) wafers and thoroughly drying the film in flowing N2. UV-vis spectroscopy measurements of the films were made on a Shimadzu dual-beam spectrophotometer (model UV-1601PC) operating in reflection mode at a resolution of 2 nm.
- These data confirm the presence of gold nanoparticles on the surface of the biomaterial. UV-vis spectra of the clear aqueous solution after reaction with the mycelial cells for 72 h showed the absence of the characteristic plasmon resonance band of gold ca 533 nm indicating the absence of gold in the solution.
- In this experiment, 10 g of wet fungal mycelia (Verticillium), grown in a culture medium, separated from medium by centrifugation, washed several times with water through centrifugation, was taken in an autoclaved conical flask and then 250 mg of HAuCl 4 in 100 ml water was added.
- The conical flask was then plugged with cotton and incubated at 27° C. Samples were collected periodically by filtration of solution containing the fungus inside the inoculation chamber under laminar flow condition. Bio-transformation was routinely monitored by visual inspection of the biomass as well as measurement of the UV-vis spectra form the fungal cells.
- Films of fungal cells (both before and after exposure to Au + ions for 72 h) for UV-vis spectroscopy and scanning electron microscopy (SEM) studies were prepared by solution casting fungal cells onto Si (111) wafers and thoroughly drying the film in flowing N2. UV-vis spectroscopy measurements of the films were made on a Shimadzu dual-beam spectrophotometer (model UV-1601IPC) operating in reflection mode at a resolution of 2 nm.
- These data confirm the presence of gold nano-practicles on the surface of the biomaterial. UV-vis spectra of the clear aqueous solutions after reaction with the mycelial cells for 72 h showed the absence of the characteristic plasmon resonance band of gold ca 533 nm indicating the absence of gold in the solution.
- In this experiment, 10 g of wet fungus (Verticillium) grown in a culture medium, separated from medium by centrifugation, washed several times with water through centrifugation, was taken in an autoclaved conical flask and then 125 mg AgNO 3 in 100 water was added.
- The conical flask was then plugged with cotton and incubated at 27° C. Samples were collected periodically by filtration of solution containing the fungus inside the inoculation chamber under laminar flow condition. Presence of nano sized Ag particles deposited on to the fungal cells was confirmed by evolution of plasmon resonance band around 400 nm. The brown coloration is a clear indication of formation of silver nano-clusters. The range of the silver nano-particles size was found to be 5-80 nm.
- In this experiment, 10 g of wet fungal mycelia (Verticillium), grown in a culture medium, separated from medium by centrifugation, washed several times with water through centrifugation, was taken in a autoclaved conical flask and then 50 mg AgNO 3 in 100 ml water was added.
- The conical flask was then plugged with cotton and incubated at 37° C. Samples were collected periodically by filtration of solution containing the fungus inside the inoculation chamber under laminar flow condition. Samples were collected between 1 and 86 th and each sample was characterized by UV-vis spectroscopy fluorescence spectroscopy, TEM analysis. Evolution of plasmon resonance band around 400 nm and the brown coloration is a clear indication of formation of silver nanoclusters. The range of the silver nanoparticles size was found to be ca. 50 nm.
- In this experiment, 10 g of wet fungal mycelia (Verticillium) grown, in a culture medium, separated from medium by centrifugation, washed several times with water through centrifugation, was taken in an autoclaved conical flask and then 100 ml solution containing 100 mg Ni(NO 3)2 (nickel nitrate) was added. The conical flask was then plugged with cotton and incubated at 22° C. Samples were collected periodically by filtration of solution containing the fungus inside the inoculation chamber under lamiar flow condition. Samples were collected at 86 h and characterized by UV-vis spectroscopy, TEM analysis and by fluorescence spectroscopy. Evolution of plasmon resonance band around 415 nm is clear indication of formation of Ni-nano-clusters in solution. Sizes of the nano-clusters were determined by TEM analysis and found to be 100 nm.
- In this experiment, 10 g of wet fungal mycelia (Verticillium) grown in a culture medium, separated from medium by centrifugation, washed several times with water through centrifugation, was taken in an autoclaved conical flask and then 25 mg NiSO 4 in 100 ml water was added.
- The conical flask was then plugged with cotton and incubated at 25° C. Samples were collected periodically by filtration of solution containing the fungus inside the inoculation chamber under laminar flow condition. The samples were collected between 1 and 96 h and each stage was characterized by UV-vis spectroscopy fluorescence spectroscopy, TEM analysis. The brown coloration of the fungal mycelial biomass, evolution of the plasmon resonance band around 415 nm and TEM analysis indicated the formation of nickel nanoclusters, deposited on to the fungal cell, in the range of 50-100 nm. No evidence of the presence of Ni in the solution was observed.
- In this experiment, 10 g of wet fungal mycelia (Verticillium), grown in a culture medium, separated from medium by centrifugation, washed severed times with water through centrifugation, was taken in an autoclaved conical flask and then 100 ml aqueous solution containing 125 mg of H 2PtCl6 (chloroplatinic acid) in water were added.
- The conical flask was then plugged with cotton and incubated at 33° C. Samples were collected periodically by filtration of solution containing the fungus inside the inoculation chamber under laminar flow condition. Samples were collected between 1 and 96 h and the sample were characterized by UV-vis spectroscopy, fluorescence spectroscopy, TEM analysis. The evolution of the plasmon resonance band at 215 nm is a clear indication of the formation of Pt-nano-particles deposited on to fungal cell. The samples were further characterized by TEM analysis and the particle size was found to be in the range of 30-50 nm. No evidence could be obtained for the presence of Pt. in solution after the reaction.
- It is therefore clear that the present invention provides a new process using biological method for the preparation of immobilized nano particles of metals obviating the drawbacks of the prior art methods. The process of the present invention describes a new biological method, instead of chemical or physical methods for preparing immobilized metal particles. This is the first time that fungi are used to efficiently prepare immobilized nano-particles of various metals ions from their aqueous solutions.
- Justification and Advantages of the Present Invention
- The use of naturally occurring fungi under aqueous medium.
- The immobilized nano-sized metal particles are stable.
- The method of the invention is simple and environmentally friendly.
- The formation of nano-particles occurs on the surface, therefore immobilizing them and the metal nano-particles are not released in to the solution.
- A single step method for obtaining immobilized nano-particles of metals.
Claims (16)
1. A process for preparing immobilized nano-sized metal particles comprising treating wet fungal mycelia with a metal ion solution at temperature in the range of 15 to 40° C. for a period in the range of 2 to 120 hours, separating the biomass to obtain the immobilized nano-sized metal particles deposited on to the surface of the fungal cells.
2. A process as claimed in claim 1 wherein the wet fungal mycelia is obtained by growing the Verticillium (AAT-TS-4) in a culture medium for a period of 2 to 120 hours at temperature ranging between 15-40° C. under aseptic conditions, separating the biomass by centrifugation, washing several times with sterile water, and then incubating the whole reaction mixture at 15 to 40° C. and atmospheric pressure.
3. A process as claimed in claim 1 wherein the metal ion solution is obtained by dissolving metal salts of group IB-VIIIB metals in water
4. A process as claimed in claim 3 wherein the metal is selected from the group consisting of Au, Ag, Pd, Pt, Ni, Rh and Ru.
5. A process as claimed in claim 3 wherein the metal salts are selected from the group consisting of halides, nitrates and carbonates.
6. A process as claimed in claim 1 wherein the metal ion solution is obtained by dissolving the acidic form of metals in water.
7. A process as claimed in claim 6 wherein the acidic form of the metal is selected from chloroauric acid and chloroplatinic acid.
8. A process as claimed in claim 1 wherein the concentration of metal ions per gram of wet fungal mycelia is in the range of 10 to 200 mg metal ions per gram of wet fungal mycelia.
9. A process as claimed in claim 8 wherein the concentration of metal ions per gram of wet fungal mycelia is in the range of 10 to 100 mg metal ions per gram of wet fungal mycelia.
10. A process as claimed in claim 8 wherein the concentration of metal ions per gram of wet fungal mycelia is in the range of 25 to 100 mg metal ions per gram of wet fungal mycelia.
11. A process as claimed in claim 1 wherein the ratio of water to wet fungal mycelia is 100:1 (w/w).
12. A process as claimed in claim 1 wherein the fungus Verticillium AAT-TS-4 is taken as whole cell as wet solid mass.
13. A process as claimed in claim 1 wherein the reaction of the fungus and metal ion source in solution is carried out in water.
14. A process as claimed in claim 1 wherein the incubation/reaction temperature is in the range of 15-40° C.
15. A process as claimed in claim 14 wherein the incubation/reaction temperature is in the range of 23-33° C.
16. A process as claimed in claim 14 wherein the incubation/reaction temperature is in the range of 25-29° C.
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US10/032,206 US20030116501A1 (en) | 2001-12-21 | 2001-12-21 | Process for preparing immobilized nano-sized metal particles |
| US10/869,548 US20040229328A1 (en) | 2001-12-21 | 2004-06-15 | Process for immobilized nano-sized metal particles |
| US11/157,247 US20050239183A1 (en) | 2001-12-21 | 2005-06-20 | Process for immobilized nano-sized metal particles |
| US12/129,451 US7759098B2 (en) | 2001-12-21 | 2008-05-29 | Process for immobilized nano-sized metal particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US10/032,206 US20030116501A1 (en) | 2001-12-21 | 2001-12-21 | Process for preparing immobilized nano-sized metal particles |
Related Child Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US10/869,548 Continuation US20040229328A1 (en) | 2001-12-21 | 2004-06-15 | Process for immobilized nano-sized metal particles |
| US11/157,247 Continuation US20050239183A1 (en) | 2001-12-21 | 2005-06-20 | Process for immobilized nano-sized metal particles |
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| Publication Number | Publication Date |
|---|---|
| US20030116501A1 true US20030116501A1 (en) | 2003-06-26 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US10/032,206 Abandoned US20030116501A1 (en) | 2001-12-21 | 2001-12-21 | Process for preparing immobilized nano-sized metal particles |
| US10/869,548 Abandoned US20040229328A1 (en) | 2001-12-21 | 2004-06-15 | Process for immobilized nano-sized metal particles |
| US11/157,247 Abandoned US20050239183A1 (en) | 2001-12-21 | 2005-06-20 | Process for immobilized nano-sized metal particles |
| US12/129,451 Expired - Fee Related US7759098B2 (en) | 2001-12-21 | 2008-05-29 | Process for immobilized nano-sized metal particles |
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| Application Number | Title | Priority Date | Filing Date |
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| US10/869,548 Abandoned US20040229328A1 (en) | 2001-12-21 | 2004-06-15 | Process for immobilized nano-sized metal particles |
| US11/157,247 Abandoned US20050239183A1 (en) | 2001-12-21 | 2005-06-20 | Process for immobilized nano-sized metal particles |
| US12/129,451 Expired - Fee Related US7759098B2 (en) | 2001-12-21 | 2008-05-29 | Process for immobilized nano-sized metal particles |
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| US (4) | US20030116501A1 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060172015A1 (en) * | 2004-12-31 | 2006-08-03 | Development Center For Biotechnology | Methods and pharmaceutical compositions for inhibiting metastasis of malignant tumors and growth of leukemic cells |
| CN104450564A (en) * | 2014-11-14 | 2015-03-25 | 东北林业大学 | Sulfate reducing bacterium capable of being used for preparing Ag/AgCl nano particles |
| KR101517665B1 (en) | 2013-02-05 | 2015-05-11 | 영남대학교 산학협력단 | Preparation method of nanoparticle using Flammulina velutipes |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2462227B1 (en) * | 2009-08-04 | 2014-12-03 | Council of Scientific & Industrial Research | Dna loaded supported gold nanoparticles, process for the preparation and use thereof |
| CN104673679B (en) * | 2015-01-15 | 2017-07-21 | 大连理工大学 | A Malia mold and its application in the synthesis of gold nanomaterials |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| NZ516848A (en) * | 1997-06-20 | 2004-03-26 | Ciphergen Biosystems Inc | Retentate chromatography apparatus with applications in biology and medicine |
| US6537344B2 (en) * | 2001-03-20 | 2003-03-25 | Council Of Scientific & Industrial Research | Process for the preparation of a nanosized colloidal metal particle |
| US7276283B2 (en) * | 2004-03-24 | 2007-10-02 | Wisconsin Alumni Research Foundation | Plasma-enhanced functionalization of carbon-containing substrates |
-
2001
- 2001-12-21 US US10/032,206 patent/US20030116501A1/en not_active Abandoned
-
2004
- 2004-06-15 US US10/869,548 patent/US20040229328A1/en not_active Abandoned
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2005
- 2005-06-20 US US11/157,247 patent/US20050239183A1/en not_active Abandoned
-
2008
- 2008-05-29 US US12/129,451 patent/US7759098B2/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060172015A1 (en) * | 2004-12-31 | 2006-08-03 | Development Center For Biotechnology | Methods and pharmaceutical compositions for inhibiting metastasis of malignant tumors and growth of leukemic cells |
| KR101517665B1 (en) | 2013-02-05 | 2015-05-11 | 영남대학교 산학협력단 | Preparation method of nanoparticle using Flammulina velutipes |
| CN104450564A (en) * | 2014-11-14 | 2015-03-25 | 东北林业大学 | Sulfate reducing bacterium capable of being used for preparing Ag/AgCl nano particles |
Also Published As
| Publication number | Publication date |
|---|---|
| US20080227167A1 (en) | 2008-09-18 |
| US20050239183A1 (en) | 2005-10-27 |
| US7759098B2 (en) | 2010-07-20 |
| US20040229328A1 (en) | 2004-11-18 |
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