本論文係利用射頻(Radio Frequency)濺鍍方式備製氮化鋁(Aluminum Nitride, AlN)薄膜於參考電極(Reference Electrode)/電解質(Electrolyte)/氮化鋁(AlN)薄膜/二氧化矽(SiO2)/矽晶片(p-type)/鋁(Al)結構中，並利用其具有類似MOS電容之特性，將其置於不同的酸鹼緩衝溶液(pH Buffer Solution)中偵測離子敏感度，並藉由量測電容-電壓的特性曲線來探討其感測膜表面電位(Surface Potential)之特性。同時亦將氮化鋁薄膜備製於雙層閘極結構之AlN/SiO2 Gate ISFET元件，進行元件之電流-電壓特性曲線之量測，以求出元件在待測溶液中起始電位(Threshold Voltage)的變化情形，進而計算其感測靈敏度。另外，對於元件存在的響應特性，諸如：溫度效應(Temperature Effect)、時漂(Drift)及遲滯(Hysteresis)等現象，亦將一併進行量測、分析與比較。
實驗結果顯示，以氮化鋁薄膜作為酸鹼離子感測層，在濃度為pH=1~11範圍，量測溫度為25℃，其感測度範圍分佈於50~58 mV/pH之間，時漂量與遲滯寬度則與氫離子濃度相關，其中時漂量隨著pH值的增加而增大，而遲滯量則與測量時間及測量路徑有關。當測量時間為960、1920、3840秒，經由pH=7®3®7®11®7的量測路徑所獲得之遲滯寬度分別為1.0、1.5、4.5 mV。另外，在溫度效應量測中，元件可操作於5~65 ℃的環境溫度範圍，且感測度與量測時的溫度有關，其感測度隨溫度變化之係數約為0.13 mV/pH℃。另外，可藉由恆壓恆流讀出電路量取AlN pH-ISFET元件的閘極輸出電位，對於線性度、穩定性與重現性之量測皆有良好的輸出表現，深具實用價值。

In this thesis, the aluminum nitride (AlN) thin film was selected as a sensing membrane for the H+ ion-sensitive field-effect transistor (ISFET). The AlN thin films were prepared by a rf sputtering technology on the reference electrode/electrolyte /AlN /SiO2/p-Si/Al structure. The capacitance-voltage (C-V) measurement was used to detect the H+ ion concentration and the C-V characteristic curves were obtained in the different pH buffer solutions. On the other hand, AlN thin films were also prepared on the double layer structure of AlN/SiO2 gate ISFET devices. After packaging, the current-voltage (I-V) measurement with a PID temperature controller was utilized to measure a series of the I-V characteristic curves. The threshold voltage can be obtained to evaluate the pH sensitivity in the different pH buffer solutions. Additionally, the effects of non-ideal factors, such as temperature effect, drift and hysteresis phenomenon on the characteristics of the ISFET are also measured, analyzed and compared with other sensing materials.
According to the experimental results, it can be found that the ISFET based on aluminum nitride thin film has a superior high pH sensitivity of approximately 50~58 mV/pH at 25℃. The drift and hysteresis are dependent on the H+ ion concentration in pH=1~11, in which the drift rate increases with the pH value increased and the hysteresis magnitude depends on the measuring time and route. It is found that the hysteresis widths measured in pH=7®3®7®11®7 cycle at 960s, 1920s and 3840s loop time are 1.0, 1.5 and 4.5 mV, respectively. When the temperature effect was considered, it was found that the ISFET could be operated at 5~65℃, in which, the pH sensitivity increased as the ambient temperature increased with the temperature coefficient of sensitivity of about 0.13 mV/pH℃. In addition, the output voltage of AlN pH-ISFET can be obtained by a constant current constant voltage (CCCV) read out circuit with a fairly linear response, stability and reproducibility in the pH measuring cycle. From the characteristics mentioned above, the AlN thin film can be as a sensing membrane for pH-ISFET applications.

Contents

Page
Chapter 1. Introduction…………………………………………………………………… 1
Chapter 2. Theory Description and Simulation……..…………………………………… 5
2.1. Introduction………………………………………………………………………….5
2.2. Site-Binding Model…………………………………………………………………. 5
2.3. EIS Structure……………………………………………………………………… 9
2.4. pH-ISFET Operation Mechanism…………………………………………………. 10
2.5. Simulation…………………………………………………………………………. 12
Chapter 3. Experiment…..……..………………………………………………………… 18
3.1. Introduction……………………………………………………………………….. 18
3.2. AlN Thin Films Preparation………………………………………………………. 18
3.3. EIS and MIS Structures Preparation……………………………………………… 19
3.4. pH-ISFET Fabrication……………………………………………………………. 19
3.5. Packaging Processes………………………………………………………………. 20
3.6. X-Ray Diffraction Analysis………………………………………………………. 21
3.7. Scanning Electron Microscope (SEM) Analysis…………………………………. 21
3.8. Capacitance-Voltage (C-V) Measurement Set-Up………………………………… 22
3.9. Current-Voltage (I-V) Measurement Set-Up………………………………………. 22
3.10. Drift and Hysteresis Measurement Set-Up………………………………………. 23
3.11. Light Exposure Measurement Set-Up……………………………………………. 24
3.12. Effects of Annealing Treatment on ISFET………………………………………. 25
Chapter 4. Results and Discussion..……………………………………………………… 26
4.1. Introduction……………………………………………………………………….. 26
4.2. Surface Structure Analysis………………………………………………………… 27
4.3. Capacitance Voltage Characteristics………………………………………………. 28
4.3.1. MIS Structure………………………………………………………………….. 28
4.3.2. EIS Structure…………………………………………………………………… 28
4.3.3. Permittivity Estimation………………………………………………………. 30
4.4. ISFET Characteristics…………………………………………………………….. 30
4.4.1. pH Sensitivity…………………………………………………………………… 31
4.4.2. Extraction of the Surface Potential and pHpzc (Point of Zero Charge)………… 33
4.4.3. Time Dependence of pH Response……………………………………………. 35
4.4.4. Reproducibility and Stability……………………………………………………. 36
4.4.5. Drift and Hysteresis Phenomenon……………………………………………. 36
4.5. Temperature and Photoelectric Characteristics…………………………………… 40
4.5.1. Temperature Characteristics of pH-ISFET……………………………………. 40
4.5.1.1. Temperature coefficients of the reference electrode (T.C.R) …………….. 41
4.5.1.2. Test solutions (T.C.S)…………………………………….……………….. 41
4.5.1.3. pH sensing film/electrolyte interface (T.C.I)…………….……………….. 42
4.5.1.4. Field-effect transistor (T.C.F)………………………….………………….. 42
4.5.1.5. Temperature coefficients of the ISFET device (T.C.T)…..……………….. 43
4.5.1.6. Extraction of temperature coefficients of AlN pH-ISFET……………….. 44
4.5.2. Light Induced Behaviour…………………………………………………….. 45
4.6. Annealing Treatment Analysis…………………………………………………….. 47
4.7. Comparison with Other Sensing Materials……….……………………………….. 49
4.8. Measurement System of a Read Out Circuit…………………………………… 51
4.8.1. Experiment and Measurement………………………………………………. 51
4.8.2. Results and Discussion……………………………………….……………… 52
Chapter 5. Conclusion…………………………………………………………………… 53
References…………………………………………………………………………………… 56


List of Figures

Page
Fig. 1-1 Schematic cross-section of an ISFET structure………………………………… 66
Fig. 2-1 Schematic representation of the site-binding model……………………………. 67
Fig. 2-2 Basic and multi-phase diagram of EIS structure……………………………….. 67
Fig. 2-3 Typical C-V curves for the electrolyte-SiO2-Si EIS structure. Oxide thickness is 560 Å on a 〈100〉10 Ω-cm p-type substrate. Curve: 1, pH 4.4; 2, pH 6.0; 3, pH 7.2; 4, pH 8.3; 5, pH 9.9; 6, pH 11.2. (Adapted from Luc Bousse [21] ).…………………………………………………………………………… 68
Fig. 2-4 Relationship between pKa, pKb and sensitivity……………………….………… 69
Fig. 2-5 Surface potential curves with different Ns……………………….……………… 69
Fig. 2-6 Surface potential curves with different Kb/Ka ratios…………….……………… 70
Fig. 2-7 Surface potential curves with constant Ka and variable of Kb…….…………….. 70
Fig. 2-8 Simulation of the C-V curves for the EIS structure…………….………………. 71
Fig. 2-9 Simulation of the IDS-VDS curves of the AlN/SiO2 gate ISFET.………………… 71
Fig. 2-10 Simulation of the IDS-VGS curves of the AlN/SiO2 gate ISFET………………… 72
Fig. 2-11 Simulation of the temperature characteristics of the AlN/SiO2 gate ISFET……. 72
Fig. 3-1 Schematic diagram of the r.f. sputtering system…………………………….. 73
Fig. 3-2 AlN thin films prepared on different structures, (a) EIS structure; (b) MIS structure………………………………………………………………………… 73
Fig. 3-3 Photo-masks of the ISFET……………………………..………………………. 74
Fig. 3-4 A flow chart for packaging processes………………………………………….. 75
Fig. 3-5 Diagrammatic sketch of the ISFET, (a) sensor head; (b) ISFET device………… 76
Fig. 3-6 C-V measurement system with a PID temperature controller………………….. 77
Fig. 3-7 I-V measurement system for the ISFET with a PID temperature controller….... 77
Fig. 3-8 Drift and hysteresis measurement system………………………………………. 78
Fig. 3-9 Constant current constant voltage read out circuit……………………………… 78
Fig. 3-10 Measurement system for light-induced characteristic variations.………………. 79
Fig. 4-1 X-ray diffraction pattern of the AlN thin film………………..………………… 80
Fig. 4-2 SEM photograph of the AlN film deposited at 90%Ar-10%N2 with a sputtering pressure of 30 mTorr, substrate temperature of 150℃ and rf power of 65 W, (a) cross-section of the AlN / p-Si structure; (b) surface morphology of the AlN film……………………………………………………………………………… 81
Fig. 4-3 Capacitance - voltage curves of the AlN MIS structure………………………… 82
Fig. 4-4 Capacitance - voltage curves for the AlN/SiO2 sensing structure……………… 82
Fig. 4-5 IDS versus VGS curves for the AlN pH-ISFET………………………………….. 83
Fig. 4-6 IDS versus VDS curves for the AlN pH-ISFET………………………………….. 83
Fig. 4-7 IDS versus VGS curves for the ISFET and MOSFET……………………………. 84
Fig. 4-8 Surface potential of the AlN pH-ISFET……………………..…………………. 84
Fig. 4-9 Time dependence of the pH sensitivity for the AlN pH-ISFET……………..…. 85
Fig. 4-10 Response time of the AlN pH-ISFET…………………………………………… 85
Fig. 4-11 Reproducibility of the AlN pH-ISFET in the pH=1 solution, tested two times during 30 min…………………………………………………………………… 86
Fig. 4-12 Relationship between the threshold voltage and pH value extracted from the first testing and after a month……………………………………………………….. 87
Fig. 4-13 Relationship between pH sensitivity and time…………….…………………… 88
Fig. 4-14 pH sensitivities extracted by CCCV circuit…………………………..………… 88
Fig. 4-15 Drift response of the AlN pH-ISFET in the pH=7 buffer solution……………… 89
Fig. 4-16 Relationship between the drift rate and the pH value of the AlN pH-ISFET…… 89
Fig. 4-17 Residual plot of hysteresis curves for AlN pH-ISFET at various loop time….… 90
Fig. 4-18 IDS-VGS curves of the AlN pH-ISFET measured at the ambient temperature between 5℃ and 65℃ (step 10℃) in the pH=1 buffer solution……………… 90
Fig. 4-19 Isothermal points of the AlN pH-ISFET for various pH values……………….. 91
Fig. 4-20 pH sensitivity of the AlN pH-ISFET measured at 5, 15, 25, 35, 45, 55 and 65℃, respectively…………………………………………………………………….. 91
Fig. 4-21 Relationship between pH sensitivity and ambient temperature………………… 92
Fig. 4-22 Comparison of the sensitivities obtained by I-V measurement and CCCV circuit…………………………………………………………………………… 92
Fig. 4-23 Relationship between the gate voltage and drain current under different light intensities……………………………………………………………………….. 93
Fig. 4-24 Relationship between the drain voltage and drain current under different light intensities………………………………………………………………………. 94
Fig. 4-25 Relationship between the light intensity and drain current…………………….. 95
Fig. 4-26 Relationship between the light intensity and sensitivity……………………….. 95
Fig. 4-27 XRD pattern of AlN film with and without annealing treatment……………………………………………………………………….. 96
Fig. 4-28 SEM photograph of the AlN film with annealing treatment, (a) 200℃; (b) 300℃; (c) 400℃; (d) 500℃; (e) 600℃………………………………………………... 97
Fig. 4-29 Gate voltage of the AlN pH-ISFET with and without annealing treatment……………………………………………………………………….. 98
Fig. 4-30 IDS－VGS curves of the AlN pH-ISFET with and without annealing treatment……………………………………………………………………….. 98
Fig. 4-31 IDS－VDS curves of the AlN pH-ISFET with and without annealing treatment……………………………………………………………………….. 99
Fig. 4-32 pH sensitivity curves for various sensing membranes………………………… 100
Fig. 4-33 Relationship between sensitivity and temperature for various sensing film….. 100
Fig. 4-34 Block diagram of an ISFET-based pH meter…………………………………. 101
Fig. 4-35 Schematic of an analog circuit………………………………………………… 101
Fig. 4-36 Schematic of a digital circuit………………………………………………….. 102
Fig. 4-37 Schematic of a pH meter system………………………………………………. 102


List of Tables

Page
Table 2-1 Simulation parameters of the AlN thin film…………………………………… 103
Table 3-1 Preparation conditions of the AlN thin film…………………………..………. 104
Table 3-2 Scanning parameters for the X-ray diffraction analysis………………….…… 104
Table 4-1 JCPDS datas of the AlN powder……..……….………………………………. 105
Table 4-2 Sensitivity and percentage of the Nernstian response for different exposure time……………………………………………………………………………. 106
Table 4-3 Temperature coefficients and composition of the different buffer solutions… 107
Table 4-4 Comparison of sensitivities for different sensing membranes………………… 108
Table 4-5 Comparison of drift rate in pH=7 for various pH sensing materials………….. 108
Table 4-6 Comparison of the hysteresis of various sensing gate materials……………… 109
Table 4-7 Comparison of the temperature coefficient of sensitivity for various sensing materials……………………………………………………………………….. 110
Table 4-8 Comparison of the read-out values of AlN pH-ISFET pH meter and commercial pH meter with glass electrode at 25℃………………………………………… 111
Table 4-9 Comparison of the operation conditions for different sensitive gate ISFETs….. 112

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