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Synthesis of metal oxide nanostructures, their characterization and chemical sensing applications
Linköping University, Department of Science and Technology, Physics and Electronics. Linköping University, The Institute of Technology.
2014 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

The existence of nanomaterials is a revolutionizing step towards the fabrication of nanodevices and it enhances the enthusiasm of the researchers for the development of new devices with improved performance relative to that of bulk material based devices. Among the nanomaterials, the metal oxide nanostructures have drawn the attention of scientific community in the development of different biochemical and biomedical nanodevices in the recent time. Today, the nanotechnology based applications of several materials particularly biosensing, molecular imaging, biological separation, biomarkers and photodynamic therapy have given wide spectrum of the fabrication of novel and sensitive nanodevices. The attraction of nanomaterials based devices is hidden in the fact of their desirable and unique properties such as high surface to volume ratio, biocompatibility, fast electron transfer rate, and nontoxic in many cases. The biocompatibility is the most favourable property of several nanomaterials such as ZnO, TiO2 etc. which provide the solid platform for the synthesis of nanomedicine. In the sensor technology, the uses of nanomaterials have shown the drastic and bombastic realization of high sensitivity for a particular sensor and the possible detection of specific analytes from their small volumes. The metal oxide nanostructures show a fast electron communication, and high degree of adsorption of biosensitive material which further enhances the sensitivity of nanosensor device. The metal oxides nanostructures  exhibit tuneable size; morphology based chemical and physical properties which are easily to combine with biosensitive material in the fabrication of sensitive chemical and biosensors. The metal oxide nanostructures experienced attractive surface chemistry, high surface  to volume ratio, valuable thermal and electrical properties, therefore the development of nanosensors is accompanied by high sensitivity, low limit of detection and a fast response time.

In this dissertation, several metal oxide nanostructures have been presented such as ZnO, CuO, NiO, Co3O4, Fe2O3, Mn3O4, NiCo2O4 and TiO2. By exploiting the favourable properties of these metal oxides for the sensing, thus have been used potentially in the fabrication of chemical nanosensors.

Place, publisher, year, edition, pages
Linköping: Linköping University Electronic Press, 2014. , 56 p.
Series
Linköping Studies in Science and Technology. Dissertations, ISSN 0345-7524 ; 1577
Keyword [en]
Hydrothermal method, seed layer, ZnO nanorods, ZnO nanotubes, immunosensor, iron ferrite, glucose sensor, well aligned ZnO nanorods, CuO nanoleaves, CuO nanosheets, CuO bundle of nanowires
National Category
Natural Sciences
Identifiers
URN: urn:nbn:se:liu:diva-104422ISBN: 978-91-7519-394-6 (print)OAI: oai:DiVA.org:liu-104422DiVA: diva2:696983
Public defence
2014-03-20, K 3, Kåkenhus, Campus Norrköping, Linköpings universitet, Norrköping, 10:00 (English)
Opponent
Supervisors
Available from: 2014-02-17 Created: 2014-02-17 Last updated: 2014-02-17Bibliographically approved
List of papers
1. Hydrothermal Growth of Vertically Aligned ZnO Nanorods Using a Biocomposite Seed Layer of ZnO Nanoparticles
Open this publication in new window or tab >>Hydrothermal Growth of Vertically Aligned ZnO Nanorods Using a Biocomposite Seed Layer of ZnO Nanoparticles
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2013 (English)In: Materials, ISSN 1996-1944, E-ISSN 1996-1944, Vol. 6, no 8, 3584-3597 p.Article in journal (Refereed) Published
Abstract [en]

Well aligned ZnO nanorods have been prepared by a low temperature aqueous chemical growth method, using a biocomposite seed layer of ZnO nanoparticles prepared in starch and cellulose bio polymers. The effect of different concentrations of biocomposite seed layer on the alignment of ZnO nanorods has been investigated. ZnO nanorods grown on a gold-coated glass substrate have been characterized by X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM) techniques. These techniques have shown that the ZnO nanorods are well aligned and perpendicular to the substrate, and grown with a high density and uniformity on the substrate. Moreover, ZnO nanorods can be grown with an orientation along the c-axis of the substrate and exhibit a wurtzite crystal structure with a dominant (002) peak in an XRD spectrum and possessed a high crystal quality. A photoluminescence (PL) spectroscopy study of the ZnO nanorods has revealed a conventional near band edge ultraviolet emission, along with emission in the visible part of the electromagnetic spectrum due to defect emission. This study provides an alternative method for the fabrication of well aligned ZnO nanorods. This method can be helpful in improving the performance of devices where alignment plays a significant role.

Place, publisher, year, edition, pages
MDPI, 2013
Keyword
biocomposite seed layer; ZnO nanorods; hydrothermal growth method; starch; cellulose
National Category
Engineering and Technology
Identifiers
urn:nbn:se:liu:diva-103818 (URN)10.3390/ma6083584 (DOI)000330293100034 ()
Available from: 2014-01-28 Created: 2014-01-28 Last updated: 2017-12-06Bibliographically approved
2. Fabrication of Well-Aligned ZnO Nanorods Using a Composite Seed Layer of ZnO Nanoparticles and Chitosan Polymer
Open this publication in new window or tab >>Fabrication of Well-Aligned ZnO Nanorods Using a Composite Seed Layer of ZnO Nanoparticles and Chitosan Polymer
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2013 (English)In: Materials, ISSN 1996-1944, E-ISSN 1996-1944, Vol. 6, no 10, 4361-4374 p.Article in journal (Refereed) Published
Abstract [en]

In this study, by taking the advantage of both inorganic ZnO nanoparticles and the organic material chitosan as a composite seed layer, we have fabricated well-aligned ZnO nanorods on a gold-coated glass substrate using the hydrothermal growth method. The ZnO nanoparticles were characterized by the Raman spectroscopic techniques, which showed the nanocrystalline phase of the ZnO nanoparticles. Different composites of ZnO nanoparticles and chitosan were prepared and used as a seed layer for the fabrication of well-aligned ZnO nanorods. Field emission scanning electron microscopy, energy dispersive X-ray, high-resolution transmission electron microscopy, X-ray diffraction, and infrared reflection absorption spectroscopic techniques were utilized for the structural characterization of the ZnO nanoparticles/chitosan seed layer-coated ZnO nanorods on a gold-coated glass substrate. This study has shown that the ZnO nanorods are well-aligned, uniform, and dense, exhibit the wurtzite hexagonal structure, and are perpendicularly oriented to the substrate. Moreover, the ZnO nanorods are only composed of Zn and O atoms. An optical study was also carried out for the ZnO nanoparticles/chitosan seed layer-coated ZnO nanorods, and the obtained results have shown that the fabricated ZnO nanorods exhibit good crystal quality. This study has provided a cheap fabrication method for the controlled morphology and good alignment of ZnO nanorods, which is of high demand for enhancing the working performance of optoelectronic devices.

Place, publisher, year, edition, pages
MDPI, 2013
Keyword
ZnO nanoparticles; chitosan; ZnO nanorods; well-aligned; low-temperature growth
National Category
Engineering and Technology
Identifiers
urn:nbn:se:liu:diva-104420 (URN)10.3390/ma6104361 (DOI)000330295600005 ()
Available from: 2014-02-17 Created: 2014-02-17 Last updated: 2017-12-06Bibliographically approved
3. Well aligned ZnO nanorods growth on the gold coated glass substrate by aqueous chemical growth method using seed layer of Fe3O4 and Co3O4 nanoparticles
Open this publication in new window or tab >>Well aligned ZnO nanorods growth on the gold coated glass substrate by aqueous chemical growth method using seed layer of Fe3O4 and Co3O4 nanoparticles
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2013 (English)In: Journal of Crystal Growth, ISSN 0022-0248, E-ISSN 1873-5002, Vol. 368, 39-46 p.Article in journal (Refereed) Published
Abstract [en]

In this study, Fe3O4 and Co3O4 nanoparticles were prepared by co-precipitation method and sol-gel method respectively. The synthesised nanoparticles were characterised by X-ray diffraction [XRD] and Raman spectroscopy techniques. The obtained results have shown the nanocrystalline phase of obtained Fe3O4 and Co3O4 nanoparticles. Furthermore, the Fe3O4 and Co3O4 nanoparticles were used as seed layer for the fabrication of well-aligned ZnO nanorods on the gold coated glass substrate by aqueous chemical growth method. Scanning electron microscopy (SEM), high resolution transmission electron microscopy [HRTEM], as well as XRD and energy dispersive X-ray techniques were used for the structural characterisation of synthesised ZnO nanorods. This study has explored highly dense, uniform, well-aligned growth pattern along 0001 direction and good crystal quality of the prepared ZnO nanorods. ZnO nanorods are only composed of Zn and O atoms. Moreover, X-ray photoelectron spectroscopy was used for the chemical analysis of fabricated ZnO nanorods. In addition, the structural characterisation and the chemical composition study and the optical investigation were carried out for the fabricated ZnO nanorods and the photoluminescence [PL] spectrum have shown strong ultraviolet (UV) peak at 381 nm for Fe3O4 nanoparticles seeded ZnO nanorods and the PL spectrum for ZnO nanorods grown with the seed layer of Co3O4 nanoparticles has shown a UV peak at 382 nm. The green emission and orange/red peaks were also observed for ZnO nanorods grown with both the seed layers. This study has indicated the fabrication of well aligned ZnO nanorods using the one inorganic nanomaterial on other inorganic nanomaterial due to their similar chemistry.

Place, publisher, year, edition, pages
Elsevier, 2013
Keyword
Characterisation, Crystal structure, Hydrothermal crystal growth, Seed crystals, Nanomaterials, Oxides, Semiconducting II-VI materials
National Category
Engineering and Technology
Identifiers
urn:nbn:se:liu:diva-90667 (URN)10.1016/j.jcrysgro.2013.01.009 (DOI)000315574700007 ()
Note

Funding Agencies|King Saud University|RGP-VPP-023|

Available from: 2013-04-03 Created: 2013-04-03 Last updated: 2017-12-06
4. Development of a disposable potentiometric antibody immobilized ZnO nanotubes based sensor for the detection of C-reactive protein
Open this publication in new window or tab >>Development of a disposable potentiometric antibody immobilized ZnO nanotubes based sensor for the detection of C-reactive protein
2012 (English)In: Sensors and actuators. B, Chemical, ISSN 0925-4005, E-ISSN 1873-3077, Vol. 166, 809-814 p.Article in journal (Refereed) Published
Abstract [en]

In this paper, the fabrication of ZnO nanotubes was carried out through chemical etching of ZnO nanorods on the gold coated glass substrates. The monoclonal anti-C-reactive protein clone CRP-8 (mouse IgG1 isotype) with glutaraldehyde was immobilized on these ZnO nanotubes using simple physical adsorption method. The novelty of the present ZnO nanotubes based research is the generation of electromotive force (EMF) in the environment of rapid formation of complex between immobilized antibodies with CRP on the surface of ZnO nanotubes. The electrochemical response of the proposed C-reactive protein (CRP) of human plasma biosensor was measured using potentiometric technique. The antibody immobilized ZnO nanotubes based sensor electrode detected the concentration range of CRP from 1.0 x 10(-5) mg/L to 1.0 x 100 mg/L with an acceptable sensitivity of 13.17 +/- 0.42 mV/decade. This unusual behavior of the proposed ZnO nanotubes based sensor in no particular electrolytic atmosphere is opening a new way for the detection of proteins at the nanolevel. The response of CRP sensor was highly linear and stable for above detected concentrations. The time response of antibody immobilized ZnO nanotubes based sensor was observed less than 10 s with good selectivity, reproducibility, repeatability and stability. The life time of sensor was not more than three days after use, so it can be used as disposable sensor.

Place, publisher, year, edition, pages
Elsevier, 2012
Keyword
ZnO nanotubes; Monoclonal anti-C-reactive protein clone; CRP-8; Potentiometric technique; C-reactive protein; Glutaraldehyde; Electrochemical response
National Category
Engineering and Technology
Identifiers
urn:nbn:se:liu:diva-79821 (URN)10.1016/j.snb.2012.03.083 (DOI)000305356900111 ()
Available from: 2012-08-14 Created: 2012-08-14 Last updated: 2017-12-07
5. The synthesis of CuO nanoleaves, structural characterization, and their glucose sensing application
Open this publication in new window or tab >>The synthesis of CuO nanoleaves, structural characterization, and their glucose sensing application
2013 (English)In: Applied Physics Letters, ISSN 0003-6951, E-ISSN 1077-3118, Vol. 102, no 10Article in journal (Refereed) Published
Abstract [en]

The present study describes the synthesis of well aligned and highly dense polyethylene glycol template assisted cupric oxide (CuO) nanoleaves on the gold coated glass substrate by hydrothermal growth method. The structural study based investigations of CuO nanoleaves were performed by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), energy dispersive X-ray (EDX), infrared reflection-absorption spectroscopy (IRAS), and high resolution transmission electron microscopy (HRTEM). The glucose sensor based on the glucose oxidase immobilized CuO nanoleaves electrode detected the wide range of glucose concentrations with good linearity and exhibited high sensitivity of 61.9+/-2.0 mV/decade. The linear detection range was observed from 1.0 x 10(-5) to 2.0 x 10(-2) M with detection limit of 5.0 x 10(-6) M and a fast response time of less than 5 s was also observed. The glucose sensor electrode possesses good anti-interference ability, stability, repeatability, and reproducibility.

Place, publisher, year, edition, pages
American Institute of Physics (AIP), 2013
National Category
Engineering and Technology
Identifiers
urn:nbn:se:liu:diva-91547 (URN)10.1063/1.4795135 (DOI)000316501200089 ()
Available from: 2013-04-26 Created: 2013-04-26 Last updated: 2017-12-06
6. Low temperature synthesis of seed mediated CuO bundle of nanowires, their structural characterisation and cholesterol detection
Open this publication in new window or tab >>Low temperature synthesis of seed mediated CuO bundle of nanowires, their structural characterisation and cholesterol detection
2013 (English)In: Materials science & engineering. C, biomimetic materials, sensors and systems, ISSN 0928-4931, E-ISSN 1873-0191, Vol. 33, no 7, 3889-3898 p.Article in journal (Refereed) Published
Abstract [en]

In this study, we have successfully synthesised CuO bundle of nanowires using simple, cheap and low temperature hydrothermal growth method. The growth parameters such as precursor concentration and time for duration of growth were optimised. The field emission scanning electron microscopy (FESEM) has demonstrated that the CuO bundles of nanowires are highly dense, uniform and perpendicularly oriented to the substrate. The high resolution transmission electron microscopy (HRTEM) has demonstrated that the CuO nanostructures consist of bundle of nanowires and their growth pattern is along the [010] direction. The X-ray diffraction (XRD) technique described that CuO bundle of nanowires possess the monoclinic crystal phase. The surface and chemical composition analyses were carried out with X-ray photoelectron spectroscopy (XPS) technique and the obtained results suggested the pure crystal state of CuO nanostructures. In addition, the CuO nanowires were used for the cholesterol sensing application by immobilising the cholesterol oxidase through electrostatic attraction. The infrared reflection absorption spectroscopy study has also revealed that CuO nanostructures are consisting of only Cu-O bonding and has also shown the possible interaction of cholesterol oxidase with the sharp edge surface of CuO bundle of nanowires. The proposed cholesterol sensor has demonstrated the wide range of detection of cholesterol with good sensitivity of 33.88 +/- 0.96 mV/decade. Moreover, the CuO bundle of nanowires based sensor electrode has revealed good repeatability, reproducibility, stability, selectivity and a fast response time of less than 10 s. The cholesterol sensor based on the immobilised cholesterol oxidase has good potential applicability for the determination of cholesterol from the human serum and other biological samples.

Place, publisher, year, edition, pages
Elsevier, 2013
Keyword
CuO bundle of nanowires, Hydrothermal method, Seed layer, IRAS, Potentiometric technique, Cholesterol sensor
National Category
Engineering and Technology
Identifiers
urn:nbn:se:liu:diva-100485 (URN)10.1016/j.msec.2013.05.029 (DOI)000325445700042 ()
Available from: 2013-11-08 Created: 2013-11-08 Last updated: 2017-12-06
7. Synthesis of Novel CuO Nanosheets and Their Non-Enzymatic Glucose Sensing Applications
Open this publication in new window or tab >>Synthesis of Novel CuO Nanosheets and Their Non-Enzymatic Glucose Sensing Applications
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2013 (English)In: Sensors, ISSN 1424-8220, E-ISSN 1424-8220, Vol. 13, no 6, 7926-7938 p.Article in journal (Refereed) Published
Abstract [en]

Abstract: In this study, we have developed a sensitive and selective glucose sensor using novel CuO nanosheets which were grown on a gold coated glass substrate by a low temperature growth method. X-ray differaction (XRD) and scanning electron microscopy (SEM) techniques were used for the structural characterization of CuO nanostructures. CuO nanosheets are highly dense, uniform, and exhibited good crystalline array structure. X-ray photoelectron spectroscopy (XPS) technique was applied for the study of chemical composition of CuO nanosheets and the obtained information demonstrated pure phase CuO nanosheets. The novel CuO nanosheets were employed for the development of a sensitive and selective non-enzymatic glucose sensor. The measured sensitivity and a correlation coefficient are in order 5.20 × 102 µA/mMcm2 and 0.998, respectively. The proposed sensor is associated with several advantages such as low cost, simplicity, high stability, reproducibility and selectivity for the quick detection of glucose.

Place, publisher, year, edition, pages
Basel, Switzerland: MDPI, 2013
Keyword
CuO nanosheets; hydrothermal growth method; non-enzymatic glucose sensor; selectivity; reproducibility
National Category
Engineering and Technology
Identifiers
urn:nbn:se:liu:diva-96478 (URN)10.3390/s130607926 (DOI)000320767600059 ()
Available from: 2013-08-23 Created: 2013-08-20 Last updated: 2017-12-06Bibliographically approved
8. Potentiometric glucose sensor based on the glucose oxidase immobilized iron ferrite magnetic particle/chitosan composite modified gold coated glass electrode
Open this publication in new window or tab >>Potentiometric glucose sensor based on the glucose oxidase immobilized iron ferrite magnetic particle/chitosan composite modified gold coated glass electrode
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2012 (English)In: Sensors and actuators. B, Chemical, ISSN 0925-4005, E-ISSN 1873-3077, Vol. 173, 698-703 p.Article in journal (Refereed) Published
Abstract [en]

A potentiometric glucose sensor based on the glucose oxidase immobilized on iron ferrite (Fe3O4) nanoparticles/chitosan composite modified gold coated glass substrate was fabricated. The electrode has advantages of both the inorganic Fe3O4 magnetic nanoparticles and the organic substance chitosan. The freshly prepared iron ferrite magnetic nanoparticles were characterized by X-ray diffraction (xRD) and transmission electron microscopy (TEM) technique was used for the analysis of dispersed iron ferrite magnetic nanoparticles in the mixture of glucose oxidase and chitosan. The electrostatic interaction of Fe3O4 nanoparticles with chitosan and the glucose oxidase molecules was investigated by the infra-red reflection absorption spectroscopy (IRAS) study. The glucose oxidase enzyme was immobilized on the surface of iron ferrite/chitosan composite without the use of Nafion or cross linker molecules. The fabricated glucose sensor has shown acceptable potentiometric response for the wide range of glucose concentrations from 1.0 x 10(-6) to 3.0 x 10(-2) M. The sensor electrode showed a sensitivity of 27.3 +/- 0.8 mV/decade and also fast response time of 7.0s. Moreover, the present glucose sensor has demonstrated good reproducibility, repeatability, selectivity and the storage stability. All the obtained results indicated that the glucose sensor based on the glucose oxidase immobilized iron ferrite/chitosan composite modified gold coated glass electrode can be used for the monitoring of glucose concentrations in human serum, drugs and may be applicable to detect glucose in the presence of other analytes.

Place, publisher, year, edition, pages
Elsevier, 2012
Keyword
Iron ferrite, Magnetic nanoparticles, Potentiometric, Immobilization, Glucose oxidase, IR study
National Category
Engineering and Technology
Identifiers
urn:nbn:se:liu:diva-86659 (URN)10.1016/j.snb.2012.07.074 (DOI)000311248100098 ()
Note

Funding Agencies|Scientific Research at King Saud University|RGP-VPP-023|

Available from: 2012-12-20 Created: 2012-12-20 Last updated: 2017-12-06

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