臺灣博碩士論文加值系統

在本論文中，我們研究了LaxTiyOz高介電常數有機材料作為（EIS）感測器的傳感器，使用溶膠凝膠合成法在0.2M條件下製備，隨後在800℃下在O2環境中進行退火 30分鐘。
為了避免柵極絕緣體的水化層的產生，並減少La-矽酸鹽的形成，所以我們在La2O3傳感器中摻雜了Ti。
分別通過XRD，AFM，XPS和SIMS分析，研究了傳感器的結構特性、表面形態、化學形態和材料組成。
透過HP 4284A LCR儀器在室溫下使用Ag / AgCl作為參考電極去量測EIS感測器元件的（C-V）曲線進而求出LaxTiyOz的pH靈敏度，磁滯電壓和漂移率。
在p型半導體上使用高介電質材料LaTi2O5作為傳感器表現出較高的表面粗糙度（Rrms）為1.07nm、pH靈敏度為70.60mV / pH，並且有極高的線性度為0.999，與LaxTiyOz中La和Ti的其他組合相比，此感測器有較低的磁滯電壓 和漂移速率分別為3.74 mV和0.95 mV / hr。
有這樣的結果歸因於傳感器中有最佳的La 和Ti摻雜比例，導致抑制吸濕，而提高結晶度。
我們還製造了電解質 - 氧化物 - 納米粒子 - 氧化物半導體（EONOS）結構的記憶生物傳感器其中使用AuNP作為電荷捕獲層。 在這裡，我們在不同的旋塗條件下製造了兩個器件，並在施加應力偏差之前和之後測量了它們的靈敏度。
施加應力偏壓後，兩種裝置的靈敏度都有了很大的提高。 測量漂移速率和滯後效應也可以了解設備的穩定性。 樣品1不僅具有更好的靈敏度，而且與樣品-2相比具有較低的漂移率和較低的滯後電壓。 通過XRD，AFM和SIMS分析研究了EONOS結構的結構，形態和組成。
SIMS深度剖面和AFM圖像證實AuNPs的形成。 將來，我們將對這種EONOS結構作為記憶生物傳感器進行更多的研究。

In this thesis, we investigated the LaxTiyOz high dielectric constant organic materials as a sensing membrane of the electrolyte- insulator- semiconductor (EIS) sensors using sol gel synthesis have been fabricated under the 0.2 M condition with subsequent annealing at 800 oC in O2 ambient for 20 min. In order to avoid the generation of hydration layer of the gate insulator and reduce the formation of La- silicate, we doped Ti in La2O3 sensing membranes. The structural properties, surface morphology, chemical states, and materials composition of the sensing films have been investigated by XRD, AFM, XPS and SIMS analysis respectively. The pH sensitivity, hysteresis voltage and drift rate of the LaxTiyOz were measured by capacitance– voltage (C-V) curves of the EIS sensor devices with Ag/AgCl reference electrode by HP 4284A LCR meter at room temperature. To use the LaTi2O5 high-k sensing film on bare p-type semiconductor exhibited the higher surface roughness (Rrms) of 1.07 nm, pH sensitivity of 70.60 mV/pH, better linearity 0.999, and the reliability of the sensor is a lower hysteresis voltage and drift rate 3.74 mV and 0.95 mV/hr respectively, compared with other combination of La and Ti in LaxTiyOz. This finding behavior attribute to the optimal La/Ti ratio content in sensing membrane leading to inhibit the moisture absorption hence improving the crystallinity.
We also fabricated Electrolyte- Oxide- Nano particle- Oxide- Semiconductor (EONOS) structure as a memory biosensor in which AuNP was used as the charge trapping layer. Here, we fabricated two devices at different spin coating conditions and measured their sensitivity before and after applying stress bias. After applying stress bias the sensitivity of both the devices has increased a lot. The drift rate and hysteresis effect also measured to know the device stability. Sample-1 exhibited not only better sensitivity but also have lower drift rate and lower hysteresis voltage compared to the sample-2. The structural, morphological and composition of the EONOS structure has been investigated by XRD, AFM and SIMS analysis respectively. SIMS depth profile and AFM image confirm the formation of AuNPs. In the future, we will have more research on this EONOS structure as a memory bio-sensor.

Recommendation letter from the thesis advisor………………………..
Thesis oral defence committee certification…………………………….
Acknowledgements……………………………………………………..iii
Abstract in Chinese……………………………………………………..iv
Abstract……………………………………………………….................vi
Contents……………………………………………………..................vii
Figure caption……………………………………………......................x
List of Table……………………………...……………………………..xiv
Chapter 1: Introduction……………………………………………….-1-
1.1 Background of Research………………………………………-1-
1.2 Motivation and objective…………………………....................-2-
1.3 EIS and ISFET………………………………………………...-4-
1.4 Organization of this thesis……………………………………..-5-
Chapter 2: Theory Description……………………………………….-7-
2.1 EIS structure………………………….....................................-7-
2.2 Site binding model…………………………………………....-9-
Chapter 3: Physical and Electrical properties of LaxTiyOz/Si- EIS structures……………………………………………………………...-18-
3.1 Material…………………………………………..………......-18-
3.2 Sol-gel process……………………………………………….-19- 3.3 Spin coating……………………………..................................-21-
3.4 The fabrication process of EIS sensor………………………..-26-
3.5 Physical properties of sensing membrane……………………-30-
3.5.1 XRD analysis…………………………………………...-30-
3.5.2 AFM analysis…………………………………………..-31-
3.5.3 XPS analysis…………………………………………..-35-
3.5.3 SIMS analysis………………………………………..... -40-
3.6 Electrical characterization of EIS structure…………………..-44-
3.6.1 Sensing mechanism………………………………….....-44-
3.6.2 Sensitivity of sensing membranes...…………………..-45-
3.6.3 Drift characteristics of the sensing film……………......-49-
3.6.4 Hysteresis characteristics of the sensing film……….....-51-
3.6.5 Summary…………………………………………….....-55-
Chapter 4: Electrolyte-Oxide-Nano particle-Oxide-Semiconductor
……………….…………..……………………………………………-56-
4.1 Introduction…………………………………..........................-56-
4.2 The fabrication process of EONOS sensor…...……………...-57-
4.2.1 Silanization…………………………………………......-57-
4.2.2 Gold nanoparticle deposition………..............................-58-
4.2.3 Gate oxide deposition and device fabrication…………..-59-
4.3 Physical characterization……………………………………..-61-
4.3.1 XRD analysis…………………………………………...-61-
4.3.2 AFM analysis…………………………………………..-62-
4.3.3 SIMS analysis………………………………………......-63-


4.4 Electrical characterization…………………………………..-65-
4.4.1 Sensitivity of sensing membranes...………………........-65-
4.4.2 Drift characteristics of the sensing films...………..........-73-
4.4.3 Hysteresis characteristics of the sensing films…….....-74-
4.5 Summary…………….………………………………………-76-
Chapter 5: Conclusion and scope of future work.……………..…...-77-
5.1 Conclusion...…….…………………………………………...-77-
5.2 Future work…….…………..………………………………...-78-
References…………..…………………………….………...………...-79-

Figure caption
Figure 1-1: The schematic cross-section of the ISFET. ……………….-5-
Figure 1-2: Comparison of EIS and ISFET structures ………………...-5-
Figure 2-1: Equivalent capacitance of the EIS structure …………......-14-
Figure 2-2: Basic and multi-phase diagram of EIS structure ………...-15-
Figure 2-3: Typical C-V curves for electrolyte-SiO2-Si EIS structure..-15-
Figure 2-4: Schematic representation of the site binding model …..…-16-
Figure 2-5: Experimental results of the surface potential (Ψ) on the SiO2
surface, using the theoretical parameters: pHpzc=2.2, β=0.14, pKa=5.7,
pKb=1.3, Ns= 5x1014
cm
-2
and CDL= 20 µF/cm2 …….……...………....-16-
Figure 2-6: Experimental results of the threshold voltage variation of the
ISFET with Al2O3 gate, using the theoretical parameters: pHpzc=8, β=4.8,
pKa=10, pKb=-6, Ns=8x1014
cm
-2
and CDL=20µF/cm-2 ………………..-17-
Figure 3-1: sol-gel process……………………………………………-24-
Figure 3-2: Four key stages of spin coating technique.……….…...….-25-
Figure 3-3: Relationship between film thickness and spin speed….....-25-
Figure 3-4: Chart classifying five different types of gels that are relevant
in sol– gel synthesis of materials………………………………………-28-
Figure 3-5: The EIS structure and process flow……………..………..-29-
Figure 3-6: Process flow of biosensor based on EIS structure. ………-29-
Figure 3-7: XRD analysis of LaxTiyOz films annealed at 800°С ….....-31-
Figure 3-8: Schematic diagram of an atomic force microscope………-32-
Figure 3-9: 3x3 µm 2D and 3D AFM image of La2O3 film……….….-33-
Figure 3-10: 3x3 µm 2D and 3D AFM image of LaTiO3 film…….….-34-
Figure 3-11: 3x3 µm 2D and 3D AFM image of LaTi2O5 film…....….-34-
Figure 3-12: 3x3 µm 2D and 3D AFM image of La2TiO5 film…….....-35-
Figure 3-13: 3x3 µm 2D and 3D AFM image of La2Ti2O7 film…....…-35-
Figure 3-14: XPS spectra of the corresponding (a) La 3d, (b) O 1s energy
levels of La2O3 film annealed at 800 °С…………………………….…-37-
Figure 3-15: XPS spectra of the corresponding (a) La 3d, (b) Ti 2p, (c) O
1s energy levels of LaTiO3 film annealed at 800 °С…………………..-37-
Figure 3-16: XPS spectra of the corresponding (a) La 3d, (b) Ti 2p, (c) O
1s energy levels of LaTi2O5 film annealed at 800 °С………………….-38-
Figure 3-17: XPS spectra of the corresponding (a) La 3d, (b) Ti 2p, (c) O
1s energy levels of La2TiO5 film annealed at 800 °С…………….…..-39-
Figure 3-18: XPS spectra of the corresponding (a) La 3d, (b) Ti 2p, (c) O
1s energy levels of La2Ti2O7 film annealed at 800 °С………………...-40-
Figure 3-19: SIMS depth profile for La2O3 film annealed at 800
°С………………………………………………………………………-41-
Figure 3-20: SIMS depth profile for LaTiO3 film annealed at 800
°С………………………………………………………………………-42-
Figure 3-21: SIMS depth profile for LaTi2O5 film annealed at 800
°С………………………………………………………………………-42-
Figure 3-22: SIMS depth profile for La2TiO5 film annealed at 800
°С……………………………………………………………………....-43-
Figure 3-23: SIMS depth profile for La2Ti2O7 film annealed at 800
°С………………………………………………………………………-43-
Figure 3-24: (a) C-V curves and (b) linearity for the La2O3 sensing
membrane……………………………………………………………...-47-
Figure 3-25: (a) C-V curves and (b) linearity for the LaTiO3 sensing
membrane……………………………………………………………...-47-
Figure 3-26: (a) C-V curves and (b) linearity for the LaTi2O5 sensing
membrane……………………………………………………………...-48-
Figure 3-27: (a) C-V curves and (b) linearity for the La2TiO5 sensing
membrane……………………………………………………………...-48-
Figure 3-28: (a) C-V curves and (b) linearity for the La2Ti2O7 sensing
membrane……………………………………………………………...-49-
Figure 3-29: Drift rates of the LaxTiyOz sensing membranes……..…..-51-
Figure 3-30: Hysteresis curve of the La2O3 sensing membrane……....-53-
Figure 3-31: Hysteresis curve of the LaTiO3 sensing membrane…..…-53-
Figure 3-32: Hysteresis curve of the LaTi2O5 sensing membrane…...-54-
Figure 3-33: Hysteresis curve of the La2TiO5 sensing membrane……-54-
Figure3-34: Hysteresis curve of the La2Ti2O7 sensing membrane…...-55-
Figure 4-1: Silanization and AuNPs immobilization…………………-58-
Figure 4-2: EONOS device structure…………………………………-60-
Figure 4-3: XRD analysis of the devices annealed at 400°С…………-61-
Figure 4-4: 3x3 µm AFM surface image of sample- 1…….……….…-62-
Figure 4-5: 3x3 µm AFM surface image of sample- 2…….………….-63-
Figure 4-6: SIMS depth profile of sample-1………………………….-64-
Figure 4-7: SIMS depth profile of sample-2………………………….-64-
Figure 4-8: (a) The C-V curves and (b) linearity of sample-1 without
bias…………………………………………………………………….-67-
Figure 4-9: (a) The C-V curve shift after applying bias (b) C-V curves
and (c) linearity of sample-1 with bias +15 V…………………………-68-
Figure 4-10: (a) The C-V curve shift after applying bias (b) C-V curves
and (c) linearity of sample-1 with bias -15 V………………………….-69-
Figure 4-11: (a) The C-V curves and (b) linearity of sample-2 without
bias…………………………………………………………………….-70-
Figure 4-12: (a) The C-V curve shift after applying bias (b) C-V curves
and (c) linearity of sample-2 with bias +15 V………………………....-71-
Figure 4-13: (a) The C-V curve shift after applying bias (b) C-V curves
and (c) linearity of sample-2 with bias -15 V……………………….…-72-
Figure 4-14: Drift rates of the EONOS devices at pH7 for 12h..…-73-
Figure 4-15: Hysteresis curves of the EONOS devices at the pH
loop7→4→7→10→7 for 1500 sec…………………………………....-75-


List of Table
Table 3-1: Sensitivity, linearity, hysteresis and drift of the sensing
membranes.…........................................................................................-52-
Table 4-1: Spin coating parameters....................................................-59-
Table 4-2: Deposition condition of Al2O3 thin film using RF
sputtering................................................................................................-60-
Table 4-3: Sensitivity and linearity of the samples before and after stress
bias.…………………………...……………………………………….-67-
Table 4-4: Drift, hysteresis and surface roughness of the samples.…...-75-

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