HANOL UNIVERSITY OF SCIENCE AND TECHNOLOGY MASTER THESIS In situ growth of Ni(OH); nanostructures on substate for glucose measurement VU THỊ OANH Oanh. VT 202682Mi@sis hust.cduvn Major of Matcrials Science Supersivnr: Dr. Chu Thi Xuan —————— Signature of Supervisor Tnstitute Tuternational Training Tuslilute for Materials Science (ITIMS HANOI, 05/2022 SOCIALIST REPUBLIC OF VIETNAM Independence — Freedom - Happiness CONFIRMATION OF MASTER’S THESIS ADJUSTMENT Full name of author: Vu Thi Oanh Thesis topic: In situ growth of Ni(OH), nanostructures on substate for glucose measurement Major: Materials Science Student ID: 20202682M The author, the supervisor, and the Commuttce confirmed that the author has adjusted and implemented the thesis aecording to the report of the Committee on May 19", 2022 with the following contents The thesis has been corrected for typographical errors and printing according to the opinions of the committees members, Tune 242022 Supervisor Author Vu Thi Oanh COMMITTEE'S CHAIRMAN Assoc. Nguyen Van Quy THESIS TOPIC In situ growth of Ni(OH); nanostructures on substrate for glucose measurement Abstract Glucose sensor has attracted the attention of academic and industrial restarchers because of its broad applications in diabetes management, food quality control and bioprosess inspection.
Compared with enzymatic glucose sensors, non-enzymatic glucose sensors are more relevant because of their stable, sensitive, and low-cusl process. The simple and low- ast synthesis of advanced nanomaterials for non-enzymalic glucose sensor is vital in practical application. Here, we introduce a facile chemical method for the synthesis of nickel(1l) hhydroxide nanostructures on porous nickcl foam (NF) for electrochemical glucose sensor. The properties of the synthesized malorial were characlerised by fieldemission scanning electron microscopy, energy-dispersive X-ray spectroscopy, high-resolution transmission electron microscopy, selected area elootro diffraction, and Raman speolroscopy.
The fabricated materials were apphed for glucose concentraliou measurement m 0.1 M NaOH by cyclic voltammetry and chronoamperemetry. The Ni(OH),/NF sensor is stable and has excellent scnsitivity with low detection limit based on the signal-to-noise ratio of 3 and high sclectivity for glucose detection im the presence of common interfering species. The Ni(OH),/Ni electrode was successfully tested in measuring glucose concentration in real serum samples. The fabricated Ni(OM),/NF electrode can be used as « low-cost, sensitive, slable and selective platform for non-enzymatic glucose sensor.
LIST OF TABLES ‘Table 1.1: Unit cell parameters for the two fundamental phases of Ni(OH),.2: X-ray diffraction parameters of J-Ni(OH)z. Diffraction angles are listed for CuKa (A 1.3: X-ray diffraction parameters of a-Ni(OA)2 calculated using the unil cell shown in figure 1. Diffraction angles are listed for Cu Ka.542 A) and Co Kq (A = 1.1: Comparison of the performance of thee synthesized NHOH)/NE and other nickel-based materials for non-cnzymatic gÏueose seItsors.2: Measurement of glucose concentration of real human blood serum samples. : Tơ compare the glucose elecbochemivel sensing of the fabricated sensors with other nickel-based sensars - MT INTRODUCTION.1 Overview of glucose, blood sugar, and diabetes mellitus.2 ÏU€OSE S€ISOTS,.2 Introduction of electrochemical glucose seDSOT.
2 13 Nickel(T) hydroxide nanostructures 8 1.1 Electrochemical behaviours of Ni(OH), toward glucose in alkaline 9 1.2 Structure and characteristics of Ni(O1D), nanostructures .3 Methods to synthesis of Ni(OLD), nanostructures. EXPERIMENTS AND METHODS.1 Chemical and wpparalus.2 Ni(OH), nanostructures fabrication - - 22 2.3 Characterization of the morphologies and composition of the synthesized 16 ố kmniearo.22) 2341 1 Scanning Dlectron Microsope (SIM). 3 lransmission Electron Microscopy (TEM). Characterivation of ch Irochemical properties of the synthesized materials - - - - - 29 2.
RESULTS AND DISCUSSTION. Morphologies and structural characteristics of the synthesized materials33 3. FESEM imagss of the synthesized materialls.2 HRTEM images of the synthesized materials.3 Coiponent ofthe synthesized materials.2 Cyclic vollammetry measurement of Lie synthesized materials in alkaline medium. Influence of reaction time on the electrochemical properties of the synthesized materils.
HH tá re —- ABBREVIATIONS No. Abbreviations and symbols Meaning 1 SEM Scanning Electron Microscope 2 FESEM Field-emission scanning electran microscopy 3 TEM Triton Thay 4 HRTEM High resolution transmission electron microscopy 5 SARD Selecind area elociron 6 EDS/EDX Bnergy-disparsive spectroscopy X-ray 7 cv Cyclic voltammetry 8 CA Chroncamperometry 9 NE Mickel foam. 10 LOD Limit of detection 11 HMTA Hexamethylenetclramine 12 AA L-ascorbic acid 13 DA Dopamine 14 CA Citric acid monchydrato 15 DL Deionized water 16 RE Relerence electrode 17 CE Counter electrode 18 WE Working electrode LIST OF FIGURES igure 1.1: Structural chemical formulas of glucose (Ð-glucose) [25].2: Schematic representation of a biosensor [32] .3: Schematic drawing of the first-generation glucose sensor [17].4: Schematic drawing of the second-generation glucose sensor [47].5: Schematic representation of a third-generation biosensor [47] 7 Figure 1.6: A general scheme of the chemical and electrochemical processes that occur at a nickel hydroxide battery eleelrode.7: Mechanism o£ oxidation-redution electrochemical reaction between Ni(OH); and glucose in alkaline medium.8: A non-cnzymatic glucose sensor based on NIOH), hanoplatelet based on GCE and ECF [55].9: The crystal structure oŸ B-Ni(OH); (591 - - 10 Figure 1.10: The idealized eryslal siruclure o[a-Ni(ORD; - xH¿O |57]. "1 Figure 141: X-ray diffraction patlems of Ni(OH), fikns ơn Ni substrates collected using a Cu Ka X-ray source [57].12: Raman spectra of (a) BNi(OH),, (b) -NIOH), a and (¢) witrale- intercalated o-Ni(OH): [57].13: Six methods to prepareve ÀXI(OLD; [51 l6 igure 1.14: 1'xamples of Ni(OH); prepared by different methods [57).1: Images of the commercial nickel foam, Figure 2.2: Experiment procedure for fabrication of materials.3: SEM procedure [61] Figure 2.4: Field-emission scanning electron microscopy (FESEM) with energy- dispersive X-ray spectroscopy (Hitachi S-4800} 24 Figure 2.5: Classification of TEM [62].6: Working prineiple of LÉM ]62|.7; Renishaw Invia Raman Microscope.9: a) Potential step, b) the decrease of concentration of electrochemical substanoe, e} relationship betwrccn current and thue |63|.10; Autolab electrochemical workstation (PGSTAT302N, Netherlands).41; Scheme for electrochemical measurement diagram 32 Figure 3.1: FESEM images of (a) the bare NF and (b-d) the Ni(OH),/NF electrodes.2: Higher “magnifiation of FESEM images of the Ni(OH)2/NF electrodes with different reaction tine.
„34 Abstract Glucose sensor has attracted the attention of academic and industrial restarchers because of its broad applications in diabetes management, food quality control and bioprosess inspection. Compared with enzymatic glucose sensors, non-enzymatic glucose sensors are more relevant because of their stable, sensitive, and low-cusl process. The simple and low- ast synthesis of advanced nanomaterials for non-enzymalic glucose sensor is vital in practical application. Here, we introduce a facile chemical method for the synthesis of nickel(1l) hhydroxide nanostructures on porous nickcl foam (NF) for electrochemical glucose sensor.
The properties of the synthesized malorial were characlerised by fieldemission scanning electron microscopy, energy-dispersive X-ray spectroscopy, high-resolution transmission electron microscopy, selected area elootro diffraction, and Raman speolroscopy. The fabricated materials were apphed for glucose concentraliou measurement m 0.1 M NaOH by cyclic voltammetry and chronoamperemetry. The Ni(OH),/NF sensor is stable and has excellent scnsitivity with low detection limit based on the signal-to-noise ratio of 3 and high sclectivity for glucose detection im the presence of common interfering species. The Ni(OH),/Ni electrode was successfully tested in measuring glucose concentration in real serum samples.
The fabricated Ni(OM),/NF electrode can be used as « low-cost, sensitive, slable and selective platform for non-enzymatic glucose sensor. LIST OF TABLES ‘Table 1.1: Unit cell parameters for the two fundamental phases of Ni(OH),.2: X-ray diffraction parameters of J-Ni(OH)z. Diffraction angles are listed for CuKa (A 1.3: X-ray diffraction parameters of a-Ni(OA)2 calculated using the unil cell shown in figure 1. Diffraction angles are listed for Cu Ka.542 A) and Co Kq (A = 1.1: Comparison of the performance of thee synthesized NHOH)/NE and other nickel-based materials for non-cnzymatic gÏueose seItsors.2: Measurement of glucose concentration of real human blood serum samples.
: Tơ compare the glucose elecbochemivel sensing of the fabricated sensors with other nickel-based sensars - MT INTRODUCTION.1 Overview of glucose, blood sugar, and diabetes mellitus.2 ÏU€OSE S€ISOTS,.2 Introduction of electrochemical glucose seDSOT. 2 13 Nickel(T) hydroxide nanostructures 8 1.1 Electrochemical behaviours of Ni(OH), toward glucose in alkaline 9 1.2 Structure and characteristics of Ni(O1D), nanostructures .3 Methods to synthesis of Ni(OLD), nanostructures. EXPERIMENTS AND METHODS.1 Chemical and wpparalus.2 Ni(OH), nanostructures fabrication - - 22 2.3 Characterization of the morphologies and composition of the synthesized 16 ố kmniearo.22) 2341 1 Scanning Dlectron Microsope (SIM). 3 lransmission Electron Microscopy (TEM).
Characterivation of ch Irochemical properties of the synthesized materials - - - - - 29 2. RESULTS AND DISCUSSTION. Morphologies and structural characteristics of the synthesized materials33 3. FESEM imagss of the synthesized materialls.2 HRTEM images of the synthesized materials.3 Coiponent ofthe synthesized materials.2 Cyclic vollammetry measurement of Lie synthesized materials in alkaline medium.
Influence of reaction time on the electrochemical properties of the synthesized materils. HH tá re —- Acknowledgement To complete this thesis, I would like to strongly express deep gratitude to my supervisor, Dr. Chu ‘rhi Xuan, who directly instructed me as well as helped me writs this thesis, I would Like to sincerely thank all professors, lecturers, and employees at TTTMS for their kindness to support me during a period T have already studied and worked there. I sincerely thank my groupmates in Nanosensors Laboratory and many others who supported me in doing experiments and research.
‘They are my good mentors and good friends who T am really appreciated T would dike to thank “The Domestic Mastcr/PhD. Scholarship Programme” of Vingroup Tanovation Foundalion (VINTF), Vingroup Big Data Anstitute (VINBIGDATA), code VINI’.33 for supporting my master's course. J also thank the project grant number B2022-BKA-25 CTVL Finally, | want to wamnly thank my family who always encourages me †o follow my research career Master student (Sign and write (ull name) Vu Thi Oanh LIST OF FIGURES igure 1.1: Structural chemical formulas of glucose (Ð-glucose) [25].2: Schematic representation of a biosensor [32] .3: Schematic drawing of the first-generation glucose sensor [17].4: Schematic drawing of the second-generation glucose sensor [47].5: Schematic representation of a third-generation biosensor [47] 7 Figure 1.6: A general scheme of the chemical and electrochemical processes that occur at a nickel hydroxide battery eleelrode.7: Mechanism o£ oxidation-redution electrochemical reaction between Ni(OH); and glucose in alkaline medium.8: A non-cnzymatic glucose sensor based on NIOH), hanoplatelet based on GCE and ECF [55].9: The crystal structure oŸ B-Ni(OH); (591 - - 10 Figure 1.10: The idealized eryslal siruclure o[a-Ni(ORD; - xH¿O |57]. "1 Figure 141: X-ray diffraction patlems of Ni(OH), fikns ơn Ni substrates collected using a Cu Ka X-ray source [57].12: Raman spectra of (a) BNi(OH),, (b) -NIOH), a and (¢) witrale- intercalated o-Ni(OH): [57].13: Six methods to prepareve ÀXI(OLD; [51 l6 igure 1.14: 1'xamples of Ni(OH); prepared by different methods [57).1: Images of the commercial nickel foam, Figure 2.2: Experiment procedure for fabrication of materials.3: SEM procedure [61] Figure 2.4: Field-emission scanning electron microscopy (FESEM) with energy- dispersive X-ray spectroscopy (Hitachi S-4800} 24 Figure 2.5: Classification of TEM [62].6: Working prineiple of LÉM ]62|.7; Renishaw Invia Raman Microscope.9: a) Potential step, b) the decrease of concentration of electrochemical substanoe, e} relationship betwrccn current and thue |63|.10; Autolab electrochemical workstation (PGSTAT302N, Netherlands).41; Scheme for electrochemical measurement diagram 32 Figure 3.1: FESEM images of (a) the bare NF and (b-d) the Ni(OH),/NF electrodes.2: Higher “magnifiation of FESEM images of the Ni(OH)2/NF electrodes with different reaction tine.
„34 Abstract Glucose sensor has attracted the attention of academic and industrial restarchers because of its broad applications in diabetes management, food quality control and bioprosess inspection. Compared with enzymatic glucose sensors, non-enzymatic glucose sensors are more relevant because of their stable, sensitive, and low-cusl process. The simple and low- ast synthesis of advanced nanomaterials for non-enzymalic glucose sensor is vital in practical application. Here, we introduce a facile chemical method for the synthesis of nickel(1l) hhydroxide nanostructures on porous nickcl foam (NF) for electrochemical glucose sensor.
The properties of the synthesized malorial were characlerised by fieldemission scanning electron microscopy, energy-dispersive X-ray spectroscopy, high-resolution transmission electron microscopy, selected area elootro diffraction, and Raman speolroscopy. The fabricated materials were apphed for glucose concentraliou measurement m 0.1 M NaOH by cyclic voltammetry and chronoamperemetry. The Ni(OH),/NF sensor is stable and has excellent scnsitivity with low detection limit based on the signal-to-noise ratio of 3 and high sclectivity for glucose detection im the presence of common interfering species.