WO2014109722A1 - A method for production and coating of antibacterial copper (ii) oxide (cuo) nano-tube - Google Patents
A method for production and coating of antibacterial copper (ii) oxide (cuo) nano-tube Download PDFInfo
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- WO2014109722A1 WO2014109722A1 PCT/TR2013/000358 TR2013000358W WO2014109722A1 WO 2014109722 A1 WO2014109722 A1 WO 2014109722A1 TR 2013000358 W TR2013000358 W TR 2013000358W WO 2014109722 A1 WO2014109722 A1 WO 2014109722A1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/02—Oxides; Hydroxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/13—Nanotubes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
Definitions
- the present invention relates to production and coating of copper (II) oxide (CuO) nano-tubes which exhibit more anti-bacterial effect than conventional nano-particles since they have high purity and large surface area, and can be used as coating material in filters provided in device systems such as white goods, air conditioning, water treatment.
- Anti-bacterial systems are usually called as antimicrobial, anti-odor and disinfectant.
- CuO is an efficient catalyst which can convert hydrocarbons (microorganisms) into carbon dioxide and water.
- the invention is based on production of CuO nano-tubes with hydrothermal synthesis and following calcination processes and coating of nickel base filters with electrokinetic deposition method.
- the object of the present invention is to obtain and coat copper (IT) oxide (CuO) nano-tubes to materials used as anti-bacterial filters in many areas using a new production method and coating technique.
- IT copper
- CuO copper oxide
- Metal oxide nano-structures have found a quite common area of usage in information storage, photonics and anti-bacterial applications by stand out in recent years with their optical, chemical and physical properties differently from main material properties.
- Copper (II) oxide nanostructures are projected to be used as thermal conductivity enhancers in fluids, for reduction of NOx gases and diesel works, and also used in rocket fuels, gas sensors, magnetic memories, batteries, solar energy converters, semiconductors. Hollow nano-crystals are used as catalyst and drug delivery agents in use.
- Nano-sized CuO structures have been synthesized with various methods until today however few studies have been done about synthesis and use of CuO nano-tubes.
- Studies about calcination of Cu nano-wires in obtaining Copper (II) Oxide (CuO) nano-tubes (Bull. Korean Chem. Soc. Vol.29, No.12 (2008) 2525-2527), synthesis thereof by means of autoclave using CuCl as starting materials (Chem. Commun. 15 (2003) 1884-1885), synthesis of CuO nano-wire structured with hydrothermal method (Langmuir 21 (2005) 3746-3748) were published.
- a study about electrokinetic deposition for obtaining superconducting film is disclosed in the European patent document no.
- EP0425308A2 and coating single-walled carbon nano-tubes to a base material with electrokinetic deposition method is disclosed in the United States patent document no. US20110240480. Whereas CuO nano-tubes are obtained in two steps by synthesis and calcination of CuO+Cu 2 0 nano-wires in the present invention.
- Figure la provides flow diagram of production of CuO nano-tube.
- Figure lb is a flow diagram of process, method of synthesis of CuO+Cu 2 0 nano- wires.
- Figure lc is a flow diagram of method of coating nano-tubes to nickel base filter with electrokinetic deposition method.
- Figure 2 provides transmission electron microscope (TEM) view of CuO+Cu 2 0 nano- wires obtained by being kept at 100°C for 24 hours.
- TEM transmission electron microscope
- Figure 3 provides transmission electron microscope (TEM) view of CuO nano-tubes obtained by calcinating of CuO+Cu 2 0 nano-wires at 400°C for 5 hours.
- TEM transmission electron microscope
- Figure 4 provides XRD (X ray diffractometer) analysis results of CuO+Cu 2 0 nano- wires and CuO nano-tubes.
- Figure provides 100 times enlarged view of the nickel filter coated by CuO nano-tube at scanning electron microscobe (SEM).
- the inventive method is a method (1) enabling production of CuO nano-tubes, which have anti-bacterial property so as to be used for preventing bacterial and microbial growth in device systems such as air conditioning, water treatment, etc., with hydrothermal method + calcination; and application thereof to nickel base filters upon W
- the said process of coating to filter (30) comprises the following method steps: - stirring and preparing the solution comprising 20 g ethanol and 0,2 g CuO nano-tube in ball (approximately 20 zircon balls in 5 mm diameter) for 1 hour
- Copper (II) nitrate trihydrate (Cu(N0 3 ) 2 H 2 0), sodium hydroxide (NaOH), ethylenediamine (EDA) and hydrazine hydrate (N 2 H 4 .H 2 0) are used as starting materials.
- 10 M (2,416 g) Cu(N0 3 ) 2 .3H 2 0 is added to 10 M (28 g) NaOH solution and stirred in a magnetic stirrer.
- the CuO nano-tubes synthesized are coated to nickel base filters with electrophoretic deposition method, by preparing colloidal solutions.
- the colloidal solution is prepared.
- the solution comprising 20 g ethanol and 0,2 g CuO nano-tube is stirred and prepared in ball (approximately 20 zircon balls in 5 mm diameter) for 1 hour.
- the nickel base filter connected to (+) load of the voltmeter device is coated at 29,9 V value for 3 minutes. SEM image of the nickel base filter coated by CuO nano-tubes is given in Figure 5.
- Staphylococcus aureus used for anti-bacterial test lead to many infections in humans. They are very common in nature because they are resistant to ambient conditions. Naturally, they intensively exist in nasal and throat cavity, human and animal excrements, abscessed wounds and acnes on the skin at most. Also, they intensively exist in foodstuffs and food premises, manual food preparers, hospital staff and hospital environments. Effect of CuO nano-tubes, which are produced in the invention, on S. Aureus type bacteria in dark medium are given in the Table 1.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Inorganic Chemistry (AREA)
- Composite Materials (AREA)
- Catalysts (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The present invention relates to production and coating of copper (II) oxide (CuO) nano-tubes which exhibit more antibacterial effect than conventional nano-particles since they have high purity and large surface area, and can be used as coating material in filters provided in device systems such as white goods, air conditioning, water treatment by means of a new method (1).
Description
DESCRIPTION
A METHOD FOR PRODUCTION AND COATING OF ANTIBACTERIAL COPPER (II) OXIDE (CuO) NANO-TUBE
Technical Field
The present invention relates to production and coating of copper (II) oxide (CuO) nano-tubes which exhibit more anti-bacterial effect than conventional nano-particles since they have high purity and large surface area, and can be used as coating material in filters provided in device systems such as white goods, air conditioning, water treatment. Anti-bacterial systems are usually called as antimicrobial, anti-odor and disinfectant. Whereas CuO is an efficient catalyst which can convert hydrocarbons (microorganisms) into carbon dioxide and water. The invention is based on production of CuO nano-tubes with hydrothermal synthesis and following calcination processes and coating of nickel base filters with electrokinetic deposition method.
Object of the Invention
The object of the present invention is to obtain and coat copper (IT) oxide (CuO) nano-tubes to materials used as anti-bacterial filters in many areas using a new production method and coating technique.
Prior Art of the Invention
The fact that their surface-to-volume ratio is high and they have superior chemical and physical properties are the main properties increasing the significance of nano- sized materials. Metal oxide nano-structures have found a quite common area of
usage in information storage, photonics and anti-bacterial applications by stand out in recent years with their optical, chemical and physical properties differently from main material properties. Copper (II) oxide nanostructures are projected to be used as thermal conductivity enhancers in fluids, for reduction of NOx gases and diesel works, and also used in rocket fuels, gas sensors, magnetic memories, batteries, solar energy converters, semiconductors. Hollow nano-crystals are used as catalyst and drug delivery agents in use.
Chemical systems which comprise halogen ions in order to control harmful microorganisms and have very complicated mixtures such as detergent have been used for a long period of time. These systems are harmful to human body and irritate skin and their effects last a short time. People get sick upon being exposed to various bacteria and viruses in collectively used spaces and spread these diseases. Two ways are followed so as to struggle with bacteria on-site. First method is to prevent and control bacterial growth by enabling certain ions and/or oxides having anti-bacterial effect to be present in the medium and another method is to dispose growing bacteria via photocatalytic effect. As is known, some metal ions enter bacteria metabolisms and inactivate their enzymes. There have been environmental improvements promising various solutions such as disinfection of air and water by semi-conductor and/or photocatalytic materials because complete disinfection is possible by less chemical at room temperature.
Nano-sized CuO structures have been synthesized with various methods until today however few studies have been done about synthesis and use of CuO nano-tubes. Studies about calcination of Cu nano-wires in obtaining Copper (II) Oxide (CuO) nano-tubes (Bull. Korean Chem. Soc. Vol.29, No.12 (2008) 2525-2527), synthesis thereof by means of autoclave using CuCl as starting materials (Chem. Commun. 15 (2003) 1884-1885), synthesis of CuO nano-wire structured with hydrothermal method (Langmuir 21 (2005) 3746-3748) were published. A study about electrokinetic
deposition for obtaining superconducting film is disclosed in the European patent document no. EP0425308A2 and coating single-walled carbon nano-tubes to a base material with electrokinetic deposition method is disclosed in the United States patent document no. US20110240480. Whereas CuO nano-tubes are obtained in two steps by synthesis and calcination of CuO+Cu20 nano-wires in the present invention.
Short Description of the Figures
Figure la provides flow diagram of production of CuO nano-tube.
Figure lb is a flow diagram of process, method of synthesis of CuO+Cu20 nano- wires.
Figure lc is a flow diagram of method of coating nano-tubes to nickel base filter with electrokinetic deposition method.
Figure 2 provides transmission electron microscope (TEM) view of CuO+Cu20 nano- wires obtained by being kept at 100°C for 24 hours.
Figure 3 provides transmission electron microscope (TEM) view of CuO nano-tubes obtained by calcinating of CuO+Cu20 nano-wires at 400°C for 5 hours.
Figure 4 provides XRD (X ray diffractometer) analysis results of CuO+Cu20 nano- wires and CuO nano-tubes.
Figure provides 100 times enlarged view of the nickel filter coated by CuO nano-tube at scanning electron microscobe (SEM).
Detailed Description of the Invention
The inventive method is a method (1) enabling production of CuO nano-tubes, which have anti-bacterial property so as to be used for preventing bacterial and microbial growth in device systems such as air conditioning, water treatment, etc., with hydrothermal method + calcination; and application thereof to nickel base filters upon
W
being coated with electrokinetic deposition method; and it comprises the following method steps:
- Synthesizing CuO+Cu20 nano-wires with hydrothermal method (10),
- Obtaining CuO nano-tubes with heat treatment of the nano-wires synthesized (20),
- Coating the CuO nano-tubes obtained to nickel base filters with electrokinetic deposition method (30).
In the invention, the process of synthesizing CuO+Cu20 nano-wires (10) is carried out by the following method steps:
- 10 M (2,416 g) Cu(N03)2.3H20 is added to 10 M (28 g) NaOH solution and stirred in a magnetic stirrer (101),
- After the Cu(N03)2.3H20 is completely dissolved, 20 ml EDA (ethylenediamine) and 10 ml (3,5 ml hydrazine hydrate + 6,5 ml distilled water) are added, respectively, to it and stirred in a magnetic stirrer for 2 hours (102),
- The solution prepared is kept in a stainless steel autoclave within a teflon coated container at 100°C for 24 hours (103),
- After the autoclave reaches the room temperature, it is washed with ethanol by means of centrifuge for 3 times and dried (104).
By calcinating the nano-wires which have been prepared by carrying out the method steps of no. 10, the process of "obtaining CuO nano-tubes" (20) is completed.
Then, the CuO nano-tubes prepared according to the method step no. 20 are coated to the filter (30). The said process of coating to filter (30) comprises the following method steps:
- stirring and preparing the solution comprising 20 g ethanol and 0,2 g CuO nano-tube in ball (approximately 20 zircon balls in 5 mm diameter) for 1 hour
(301) ,
- adding the 10 M NaOH into the colloidal solution prepared until it is pH = 9
(302) ,
- plunging the nickel base filters connected to (+) load of the voltmeter device and the metallic plate connected to (-) load thereof, into the colloidal solution prepared and coating them by being kept at 29.9 V value for 3 minutes (303).
Synthesis of Cuo Nano-Tubes (20)
Copper (II) nitrate trihydrate (Cu(N03)2 H20), sodium hydroxide (NaOH), ethylenediamine (EDA) and hydrazine hydrate (N2H4.H20) are used as starting materials. In order to synthesize copper oxide nano-tubes with hydrothermal method, 10 M (2,416 g) Cu(N03)2.3H20 is added to 10 M (28 g) NaOH solution and stirred in a magnetic stirrer. Then, by adding 20 ml EDA and 10 ml (3,5 ml hydrazine hydrate + 6,5 ml distilled water) to blue-coloured mixture, respectively, it is stirred in a magnetic stirrer for 2 hours. 40 ml is taken from the solution obtained after the stirring, put into stainless steel autoclave with 50 ml capacity and kept under hydrothermal conditions 100°C for 24 hours. The solution cooled to room temperature is washed by distilled water 3 times by being centrifuged and dried. The nano-wire structures (Figure 2) obtained are calcinated at 400°C for 5 hours after the hydrothermal process. Following the calcination process performed, multi-walled CuO nano-tubes with 2-3 nm inner diameters and 7 nm outside diameters are obtained. The flow diagram is given in Figure 1. The TEM image taken from the CuO nano-tube section obtained is given in Figure 3. Because the surface area has increased from particle state by 8-fold, the CuO nano-tubes which can be used at smaller amounts can be synthesized at two steps, namely 100-400 °C, and with hydrothermal method at low temperatures. Analysis result of the X ray diffractometer
indicating that the CuO nano-wires and nano-tubes synthesized are at high purity, is given in Figure 4.
Coating the Nickel Base Filter By Cuo Nano-Tubes (30)
The CuO nano-tubes synthesized are coated to nickel base filters with electrophoretic deposition method, by preparing colloidal solutions. Firstly, the colloidal solution is prepared. For this, the solution comprising 20 g ethanol and 0,2 g CuO nano-tube is stirred and prepared in ball (approximately 20 zircon balls in 5 mm diameter) for 1 hour. Because colloidal solution obtained has pH value of 7, the particles are neutral. Therefore, 10 M NaOH is added to the solution until it is pH = 9. The nickel base filter connected to (+) load of the voltmeter device is coated at 29,9 V value for 3 minutes. SEM image of the nickel base filter coated by CuO nano-tubes is given in Figure 5.
Bacteria called as Staphylococcus aureus used for anti-bacterial test lead to many infections in humans. They are very common in nature because they are resistant to ambient conditions. Naturally, they intensively exist in nasal and throat cavity, human and animal excrements, abscessed wounds and acnes on the skin at most. Also, they intensively exist in foodstuffs and food premises, manual food preparers, hospital staff and hospital environments. Effect of CuO nano-tubes, which are produced in the invention, on S. Aureus type bacteria in dark medium are given in the Table 1.
Table 1. Effect of CuO nano-tubes on S. Aureus type bacteria in dark medium
Bacteria
55,2% of bacteria present in dark medium comprising 1000 μ§/ηύ CuO nano-tube were observed to disappear.
Claims
1. A method (1) enabling production of CuO nano-tubes, which have anti-bacterial property so as to be used for preventing bacterial and microbial growth in device systems such as air conditioning, water treatment, etc., with hydrothermal method + calcination and application thereof to nickel base filters upon being coated with electrokinetic deposition method; characterized in that it comprises the process steps of:
- Synthesizing CuO+Cu20 nano-wires with hydrothermal method (10),
- Obtaining CuO nano-tubes with heat treatment of the nano-wires synthesized (20),
- Coating the CuO nano-tubes obtained to nickel base filters with electrokinetic deposition method (30).
2. A method (1) according to Claim 1, wherein the process of synthesizing CuO+Cu20 nano-wires (10) is characterized by the following steps of:
- 10 M (2,416 g) Cu(N03)2.3H20 is added to 10 M (28 g) NaOH solution and stirred in a magnetic stirrer (101),
- After the Cu( 03)2.3H20 is completely dissolved, 20 ml EDA (ethylenediamine) and 10 ml (3,5 ml hydrazine hydrate + 6,5 ml distilled water) are added, respectively, to it and stirred in a magnetic stirrer for 2 hours (102),
- The solution prepared is kept in a stainless steel autoclave within a teflon coated container at 100°C for 24 hours (103),
After the autoclave reaches the room temperature, it is washed with ethanol by means of centrifuge for 3 times and dried (104).
3. A method for obtaining CuO nano-tubes with heat treatment of the nano-wires according to Claim 1, characterized in that the nano-wires synthesized according to Claim 2 are calcinated at 400°C for 5 hours (20).
4. A method (1) according to Claim 1, which is a process of coating the CuO nano- tubes prepared according to Claim 3 to the filter (30) characterized by the following steps:
- stirring and preparing the solution comprising 20 g ethanol and 0,2 g CuO nano-tube in ball (approximately 20 zircon balls in 5 mm diameter) for 1 hour
(301) ,
- adding the 10 M NaOH into the colloidal solution prepared until it is pH = 9
(302) ,
- plunging the nickel base filters connected to (+) load of the voltmeter device and the metallic plate connected to (-) load thereof, into the colloidal solution prepared and coating them by being kept at 29.9 V value for 3 minutes.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP13829049.9A EP2791059A1 (en) | 2013-01-14 | 2013-12-04 | A method for production and coating of antibacterial copper (ii) oxide (cuo) nano-tube |
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| TR2013/00477 | 2013-01-14 |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104445359A (en) * | 2014-11-17 | 2015-03-25 | 河南大学 | Method for preparing cuprous oxide nano-structure on surface of phosphor bronze |
| CN105084409A (en) * | 2015-08-13 | 2015-11-25 | 南阳师范学院 | Method for synthesizing (200) crystal face exposed monodisperse CuO nanosheet |
| WO2017138890A1 (en) | 2016-02-12 | 2017-08-17 | Agency For Science, Technology And Research | Anti-bacterial patterned surfaces and methods of making the same |
| CN109110797A (en) * | 2018-09-20 | 2019-01-01 | 西安凯立新材料股份有限公司 | A kind of preparation method of sector multi-layer cupric oxide powder |
| TWI650436B (en) * | 2017-05-17 | 2019-02-11 | 林宗新 | Antibacterial copper coating film and preparation method thereof |
| CN109956493A (en) * | 2019-04-18 | 2019-07-02 | 上海电力学院 | A kind of preparation method of cerium or/and zinc doping cuprous nano material |
| EP3515193A4 (en) * | 2016-09-20 | 2019-07-31 | Agency for Science, Technology and Research | Cell rupture-based antimicrobial surfaces coated with metal oxide nano-arrays |
| CN110577234A (en) * | 2018-11-07 | 2019-12-17 | 江西省科学院能源研究所 | Preparation method of nano cuprous oxide |
| CN111252800A (en) * | 2020-01-21 | 2020-06-09 | 上海电力大学 | Preparation method of nano cuprous oxide photoelectric material |
| CN115233199A (en) * | 2022-08-03 | 2022-10-25 | 青岛特览新材料有限公司 | Stainless steel composite material, preparation method and application |
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| US20110240480A1 (en) | 2007-06-20 | 2011-10-06 | New Jersey Institute Of Technology | Nanotube Device and Method of Fabrication |
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2013
- 2013-12-04 EP EP13829049.9A patent/EP2791059A1/en not_active Withdrawn
- 2013-12-04 WO PCT/TR2013/000358 patent/WO2014109722A1/en active Application Filing
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104445359A (en) * | 2014-11-17 | 2015-03-25 | 河南大学 | Method for preparing cuprous oxide nano-structure on surface of phosphor bronze |
| CN105084409A (en) * | 2015-08-13 | 2015-11-25 | 南阳师范学院 | Method for synthesizing (200) crystal face exposed monodisperse CuO nanosheet |
| EP3413710A4 (en) * | 2016-02-12 | 2020-01-22 | Agency for Science, Technology and Research | Anti-bacterial patterned surfaces and methods of making the same |
| WO2017138890A1 (en) | 2016-02-12 | 2017-08-17 | Agency For Science, Technology And Research | Anti-bacterial patterned surfaces and methods of making the same |
| CN108777957A (en) * | 2016-02-12 | 2018-11-09 | 新加坡科技研究局 | Antibacterial patterned surface and its manufacturing method |
| EP3704941A1 (en) * | 2016-02-12 | 2020-09-09 | Agency for Science, Technology and Research | Anti-bacterial patterned surfaces and methods of making the same |
| US11154054B2 (en) | 2016-09-20 | 2021-10-26 | Agency For Science, Technology And Research | Cell rupture-based antimicrobial surfaces coated with metal oxide nano-arrays |
| EP3515193A4 (en) * | 2016-09-20 | 2019-07-31 | Agency for Science, Technology and Research | Cell rupture-based antimicrobial surfaces coated with metal oxide nano-arrays |
| TWI650436B (en) * | 2017-05-17 | 2019-02-11 | 林宗新 | Antibacterial copper coating film and preparation method thereof |
| CN109110797A (en) * | 2018-09-20 | 2019-01-01 | 西安凯立新材料股份有限公司 | A kind of preparation method of sector multi-layer cupric oxide powder |
| CN109110797B (en) * | 2018-09-20 | 2020-09-01 | 西安凯立新材料股份有限公司 | Preparation method of sector multi-layer copper oxide powder |
| CN110577234A (en) * | 2018-11-07 | 2019-12-17 | 江西省科学院能源研究所 | Preparation method of nano cuprous oxide |
| CN109956493B (en) * | 2019-04-18 | 2021-09-07 | 上海电力学院 | Preparation method of cerium or/and zinc doped cuprous oxide nano material |
| CN109956493A (en) * | 2019-04-18 | 2019-07-02 | 上海电力学院 | A kind of preparation method of cerium or/and zinc doping cuprous nano material |
| CN111252800A (en) * | 2020-01-21 | 2020-06-09 | 上海电力大学 | Preparation method of nano cuprous oxide photoelectric material |
| CN115233199A (en) * | 2022-08-03 | 2022-10-25 | 青岛特览新材料有限公司 | Stainless steel composite material, preparation method and application |
| CN115233199B (en) * | 2022-08-03 | 2023-12-22 | 青岛特览新材料有限公司 | Stainless steel composite material, preparation method and application |
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|---|---|
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