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دانلود پروژه: ساخت و مشخصه­یابی لایه­های نازک نانوکامپوزیتی Graphene-WO3 و بررسی خواص الکتروکرمیک

تعداد119صفحه در فایل word

کارشناسی ارشد رشته مهندسی نانومواد

ساخت و مشخصه­یابی لایه­های نازک نانوکامپوزیتی Graphene-WO3 و بررسی خواص الکتروکرمیک

چکيده

در این پژوهش، لایه نانوکامپوزیت WO3/rGOبر روی زیرلایه­های FTOلایه­نشانی­شده و خواص الکتروکرمیک آن مورد­بررسی قرار­گرفته­است. بدین­منظور،به ترتیبلایه­نازک گرافن­اکسید (GO) از محلول آبی گرافن­اکسید ولایه­نازک­WO3با استفاده از الکترولیت حاوی یون پلی­تانگستیک­اسیدبر روی زیرلایه FTOبه­روش لایه­نشانی الکتروشیمیاییلایه­نشانیشدند.بعد از عملیات حرارتی لایه­های به‌دست‌آمده،تأثیروجود لایه rGO در فصل مشترک الکترود/لایه WO3 بر خواص و رفتار الکتروکرمیک لایه­های آمورف و بلورینWO3مورد بررسی قرار گرفت. به­منظور ارزیابی نمونه­ها، از آنالیزهای پراش اشعه ایکس (XRD)، میکروسکوپ الکترونی روبشی گسیل میدان (FESEM)، تست‌های الکتروشیمیایی شامل ولتامتری چرخه­ای و کرونوآمپرومتری و تست‌های الکتروکرمیک شامل طیف­نگاری اپتیکی UV-Vis و اسپکتروالکتروشیمیایی استفاده­شد. نتایج نشان داد که وجود لایه rGO در فصل مشترک الکترود FTO و لایه WO3آمورف باعث افزایش نفوذ یونلیتیم موجود در الکترولیتبه لایه و در نتیجه افزایش فعالیت الکتروشیمیایی لایه شده­است. در نتیجه رفتار الکتروکرمیک نانوکامپوزیت آمورف WO3/rGO در مقایسه با لایه WO3 بهبود یافته و تغییرات عبور لایه در دو حالت رنگی و بی‌رنگ بیشتر، پاسخ‌دهی رنگی­شدن و بی‌رنگی لایه سریع‌تر و بازده رنگی­شدن آن بزرگ‌ترشده­است. بهبود عملکرد الکتروکرمیک لایه نانوکامپوزیت WO3/rGO آمورف ناشی از فضای باز زیاد در ریزساختار لایهWO3 است که باعث کوتاه‌تر شدن مسیر نفوذ یون Li در لایه WO3می‌شود وبدین­ترتیب سطحویژهبیشتریبرایواکنش­هایانتقالباروجودخواهد داشت.از سوی دیگر بررسی لایه­های بلورین کامپوزیت WO3/rGO نشان داد که وجود لایه rGO باعث عدم چسبندگی مطلوبلایه WO3 در مقیاس میکروسکوپی شده­است.

کليد واژه:الکتروکرمیزم، لایه­نازک WO3،  نانوکامپوزیت rGO-WO3، گرافن­اکسید، فصل مشترک

فهرستجدول‌ها ‌د

فهرستشکل‌‌ها ‌ه

فصل 1-   مقدمه…………………………………. …………………………………. 1

1-1- موادهوشمند 2

1-2- رنگ 3

1-3- پدیدهالکتروکرمیزم 4

1-4- پنجره‌هایهوشمند 5

1-5- لایه‌هایالکتروکرمیکنانوساختار 6

1-6- اجزایابزارالکتروکرمیک 6

1-6-1-  الکترودرسانایشفاف 7

2-6-1-  الکترولیت………………………………… ………………………………… 8

3-6-1-  الکترودکار 9

4-6-1-  الکترودمقابلیالایهذخیرهسازیونی 9

1-7- موادالکتروکرم 9

1-7-1-  الکتروکرمهایمحلولیانوعیک 10

1-7-2-  الکتروکرمهایمحلولجامدیانوعدو 10

1-7-3-  الکتروکرمهایجامدیانوعسه 10

1-8- تنگستن اکسید 12

1-8-1-  معرفی 12

1-8-2-  فازهایبلورینمختلفتنگستناکسید 13

1-9- سازوکارعملکردالکتروکرمیک 17

1-10- پارامترهایعملکردالکتروکرمیک 20

1-10-1-  مدولاسیوناپتیکی 21

1-10-2-  زمانپاسخ‌دهی 21

1-10-3-  پایداریسیکلی 21

1-10-4-  بازدهرنگیشدن 22

1-11- گرافن…………………………………. …………………………………. 23

1-11-1-  معرفی 23

1-11-2-  روش‌هایتولیدگرافن 24

1-12- گرافن‌اکسید 25

1-12-1-  روش‌هایسنتزگرافن‌اکسید 26

1-12-2-  معرفیساختار 27

1-13- مروریبرمنابعمطالعاتی 29

1-13-1-  افزودنجزءناخالصیبهالکترودالکتروکرمیک 29

1-13-2-  معرفیتخلخلمنظمبهلایه 31

1-13-3-  اصلاحفصلمشترکلایهالکتروکرمیکوالکترودهادی 31

1-14- هدفپژوهش 35

فصل 2-   فعالیتهایتجربی 37

2-1- تمیزکردنزیرلایه‌هایرسانا 38

2-2- سنتزگرافن‌اکسیدبروشهامر 38

2-2-1-  تهیهالکترولیتگرافن‌اکسید 39

2-3- لایه‌نشانیگرافن‌اکسید 40

2-4- ساختلایه‌نازکتنگستناکسید 41

2-4-1-  تهیهپیشمادهپروکسیتانگستیکاسید 41

2-4-2-  تهیهالکترولیت 41

2-4-3-  لایه‌نشانیالکتروشیمیاییلایه‌هایتنگستناکسید 41

2-4-4-  عملیاتحرارتیلایهتنگستناکسید 43

2-5- تهیهکامپوزیتدولایهگرافن‌اکسید-تنگستناکسید 44

2-6- مشخصهیابی 45

2-6-1-  مشخصهیابیگرافن‌اکسید 45

2-6-2-  مشخصهیابیلایه‌هاینازک 47

2-6-3-  تهیهالکترولیتبرایتستهایالکتروشیمیایی 48

2-6-4-  ولتامتریچرخه‌ای 48

2-6-5-  کرونوآمپرومتری 49

2-6-6-  مشخصهیابیاپتیکی 50

فصل 3-   نتایجوبحث 52

3-1- گرافن‌اکسید 53

3-1-1-  طیفپراشاشعهایکس 53

3-1-2-  طیف‌سنجینورمرئی-فرابنفش 54

3-1-3-  طیف‌نگاریتبدیلفوریهمادونقرمز 55

3-1-4-  میکروسکوپنیرویاتمیAFM 55

3-1-5-  پتانسیلزتا……………………………….. ……………………………….. 56

3-2- لایه‌نازکگرافن‌اکسید 57

3-2-1-  بررسیمیکروسکوپیلایهگرافن‌اکسید 57

3-2-2-  تستعبورفرابنفش-مرئی 61

3-3- لایه‌نازکتنگستناکسید 62

3-3-1-  لایه‌نشانیتنگستناکسید 62

3-4- خواصلایهتنگستناکسیدآمورف 65

3-4-1-  بررسیساختارلایه 65

3-4-2-  بررسیریزساختارلایهها 67

3-4-3-  آنالیزالکتروشیمیایی 70

3-4-4-  بررسیرفتارالکتروکرمیک 74

3-4-5-  تغییراتعبورلایهa-WO3/rGOبرحسبطول‌موج 77

3-4-6-  تغییراتعبورلایهa-WO3/rGOبرحسبزمان 78

3-4-7-  بازدهرنگیشدنلایهa-WO3/rGO 79

3-5- لایهتنگستناکسیدکلسینهشده 82

3-5-1-  طیفپراشاشعهایکس 82

3-5-2-  بررسیریزساختارلایه‌هایبلورین 83

3-5-3-  بررسیرفتارالکتروشیمیایی 87

3-5-4-  بررسیرفتارالکتروکرمیک 91

فصل 4-   نتیجهگیریوپیشنهادات 96

4-1- نتیجهگیری 97

4-2- پیشنهادات 99

فهرستمراجع 100

فهرست جدول‌ها

عنوان                                         صفحه

جدول‏1‑1رنگبرخیازاکسیدهایفلزیالکتروکرم. 12

جدول‏1‑2 روش‌هایشیمیاییتهیهگرافن‌اکسید. 26

جدول‏3‑1مقادیرکمیآنالیزEDSتهیهشدهازمقطعلایهGOکهبهروشلایه‌نشانیالکتروشیمیاییبررویFTOنشاندهشدهاست. 62

جدول‏3‑2مقادیرعددیآنالیزEDS. 71

جدول‏3‑3 نتایجکمیآنالیزهایالکتروشیمیاییلایه‌هایآمورفa-WO3وa-WO3/rGOکهبهمدتیکساعتدردمای 150 درجهسلسیوسخشکشده‌اند. 74

جدول‏3‑4نتایجتست‌هایالکتروکرمیکلایه‌هایآمورف. 81

جدول‏3‑5 سایزبلورکنمونه‌هایبلورین. 84

جدول‏3‑6 نتایجآنالیزهایالکتروشیمیایی 90

جدول‏3‑7 نتایجتستکرونوآمپرومتریلایه‌هایبلورین. 92

جدول‏3‑8 پارامترهایاسپکتروالکتروشیمیاییلایه‌هایبلورین. 95

فهرست شکل‌‌ها

عنوان                                         صفحه

شکل‏1‑1پنجره‌هایهوشمندتجاریدردوحالترنگیوبی‌رنگ. 6

شکل‏1‑2 طرحشماتیکیکسیستمالکتروکرمیک 7

شکل‏1‑3عناصرانتقالیباقابلیتتشکیلاکسیدهایدارایخاصیتالکتروکرمیک. 11

شکل‏1‑4الگویچرخشودماهایپایداریچندشکلیهایمختلفتنگستناکسید. 14

شکل‏1‑5 تصویرشماتیکفازهایمختلفتنگستناکسید؛دایرههایتوپرمحلبیننشینشدنیونواردشوندهبهفازهایمختلفرانشانمیدهد. 15

شکل‏1‑6 a ) سلولواحدشبکهپروسکایتی (قسمتاول) وتقارنهایهشت‌وجهی (قسمتدوم) درساختارپروسکایت؛b) یکلایهWO3دارایساختارمنوکلینیککهدرآنگوشههایهشت‌وجهیهابهاشتراکگذاشتهشدهاست (نوع- ReO3 )؛c) ساختارWO3منوکلینیک (نوع- ReO3)؛d) یکلایهازساختارمنوکلینیکWO3کهدرآنهشت‌وجهیهالبه‌هایمشترکدارند. 17

شکل‏1‑7مدلفرایندرنگیشدندرالکترودتنگستناکسید. 18

شکل‏1‑8تصویرشماتیکفرایندرنگی/بی‌رنگشدنلایهتنگستناکسیددرالکترولیتحاوییوننفوذکنندهلیتیم؛درفرایندرنگیشدنبااعمالپتانسیلاحیایییونوالکترونبه‌طورهم‌زمانواردلایهWO3می‌شود. فرایندبی‌رنگشدنعکسفرایندرنگیشدناست. 20

شکل‏1‑9یکورقهگرافنکهبراثرنوساناتدماییموجدارشدهاست. 23

شکل‏1‑10رویکردهاوروش‌هایمختلفسنتزگرافن. 25

شکل‏1‑11 ساختارگرافن‌اکسیدبرمبنایمدللرف-کلینووسکی 28

شکل‏1‑12 مراحلشماتیکسنتزنانوکامپوزیتrGO/WO3بهروشسولوترمالوسازوکاررشدنانوسیمهایWO3بررویورقههایگرافن‌اکسید. 31

شکل‏1‑13 توابعکارالکترودهایمختلفمرجع 32

شکل‏1‑14 شکلشماتیکالکترودهایالکتروکرمیکتهیهشدهکهداراوفاقدلایهگرافندرفصلمشترکالکترودهادیشفافولایهالکتروکرمیکهستند. 34

شکل‏2‑1 سوسپانسیونگرافن‌اکسید؛الف) بعدازافزودنهیدروژنپروکسید؛ب) بعدازخشکشدنبهمدت 24 ساعتدردمای 50 درجهسلسیوس. 39

شکل‏2‑2دستگاهپتانسیواستات/گالوانواستاتاستفادهشدهدراینپژوهش. 40

شکل‏2‑3 الف) شکلشماتیکچیدمانلایه‌نشانیگرافن‌اکسید؛ب) FTOپوششدادهشدهباگرافن‌اکسید. 40

شکل‏2‑4 لایه‌هایWO3تهیهشدهبروشلایه‌نشانیالکتروشیمیایی؛الف- بعدازخروجازسللایه‌نشانی؛ب- بعدازیکساعتعملیاتحرارتیدردمای 450 درجهسلسیوس. 42

شکل‏2‑5 تصویرشماتیکسِللایه‌نشانیالکتروشیمیاییWO3ازپیشمادهپروکسیتنگستیکاسید. 43

شکل‏2‑6 لایه‌هایکامپوزیت GO/WO3تهیهشده؛الف) بعدازخروجازسِللایه‌نشانی،ب) بعدازیکساعتعملیاتحرارتیدر 450 درجهسلسیوس. 44

شکل‏2‑7تصویرسِلاستفادهشدهبرایآنالیزالکتروشیمیاییلایهها. 48

شکل‏2‑8 تغییراتپتانسیلدرحینیکسیکلولتامتریچرخه‌ای. 49

شکل‏2‑9 نمودارشکلموجپتانسیلنسبتبهزماندرتستکرونوآمپرومتری 50

شکل‏2‑10 شکلشماتیکسِلاستفادهشدهبرایتستهایاسپکتروالکتروشیمیایی؛تستدرسلدوالکترودیودرحضورسیمنقرهبه‌عنوانالکترودمقابلانجامشد. 51

شکل‏3‑1 پراشاشعهایکسپودرگرافن‌اکسید. 54

شکل‏3‑2 الف) طیفUV-VisسوسپانسیونآبیGO؛ب) نمودارتائکسوسپانسیونآبیGO. 54

شکل‏3‑3 طیفFTIRنمونهGOخشکشدهدردمایC⁰50 بهمدت 24 ساعت. 55

شکل‏3‑4 تصویرAFMنمونهGOرویمیکاوپروفایلارتفاعمربوطبهآن. 56

شکل‏3‑5 الف)تصویرFESEMسطحلایهGOکهبهروشلایه‌نشانیالکتروشیمیاییبررویFTOنشاندهشدهاست؛ب) تصویرFESEMلایهFTOبدونپوشش. 58

شکل‏3‑6 اسپکتروسکوپیEDSسطحلایهGOکهبهروشلایه‌نشانیالکتروشیمیاییبررویFTOنشاندهشدهاست. 59

شکل‏3‑7 تصویرالکترونبرگشتیلایهGOکهبهروشلایه‌نشانیالکتروشیمیاییبررویFTOنشاندهشدهاست. 60

شکل‏3‑8 تصویرFESEMمقطعیلایه‌نازکGOرویFTO. 60

شکل‏3‑9 اسپکتروسکوپیEDSمقطعشکستلایه‌نازکGOکهبهروشلایه‌نشانیالکتروشیمیاییبررویFTOنشاندهشدهاست. 61

شکل‏3‑10 الف) تستعبورلایه‌نازکGOرویFTO؛ب) نمودارتائکمربوط. 62

شکل‏3‑11 نمودارجریان-زمانلایه‌نشانیتنگستناکسیددرپتانسیلثابت. 64

شکل‏3‑12طیفپراشاشعهایکسنرمالنمونهa-WO3/rGOکهدردمای 150 درجهسلسیوسبهمدتیکساعتخشکشدهاست. 66

شکل‏3‑13آنالیزGrazing XRDلایه‌نازکa-WO3/rGOکهبهمدتیکساعتدردمای 150 درجهسلسیوسخشکشدهاست. 67

شکل‏3‑14تصاویرFESEMلایه‌نازکآمورفa-WO3کهدردمای 150 درجهسلسیوسبهمدتیکساعتخشکشدهاست. 68

شکل‏3‑15 تصاویرFESEMسطحلایه‌نازکa-WO3/rGOکهدردمای 150 درجهسلسیوسبهمدتیکساعتخشکشدهاست. 69

شکل‏3‑16پروفایلEDSسطحلایه‌نازککامپوزیتیآمورف؛الف) ازنقطه 1،وب) ازنقطه 2 کهدرتصویرFESEMشکل 3-15 مشخصشدهاست. 71

شکل‏3‑17نمودارولتامتریچرخه‌ایلایه‌نازکهایآمورفa-WO3وa-WO3/rGOکهدرسلالکتروشیمیاییسهالکترودیدرالکترولیت1/0مولارلیتیمپرکلراتدرپروپیلنکربناتانجامشدهاست. 72

شکل‏3‑18 تغییراتعبورلایهa-WO3آمورفدرحالاترنگی/بی‌رنگبرحسبطول‌موج؛اینلایهبهمدتیکساعتدر 150 درجهسلسیوسخشکشدهاست.. 76

شکل‏3‑19تغییراتمیزانعبوربرحسبزماندرلایهآمورفa-WO3؛اینلایهبهمدتیکساعتدر 150 درجهسلسیوسخشکشدهاست. 77

شکل‏3‑20 اندازه‌گیریزمانتغییراترنگیشدن/ بی‌رنگیدرلایهa-WO3. 78

شکل‏3‑21 بازدهرنگیشدنلایهa-WO3کهبهمدتیکساعتدردمای 150 درجهسلسیوسخشکشدهوآمورفاست. بازدهرنگیشدنشیبقسمتخطینموداراست. 78

شکل‏3‑22طیفمیزانشفافیتبرحسبطول‌موجدردوحالترنگیوبیرنگلایه‌نازکتنگستناکسیدآمورفکهبهمدتیکساعتدر 150 درجهسلسیوسخشکشدهاست. 80

شکل‏3‑23تغییراتعبورلایهکامپوزیتa-WO3/rGOبرحسبزمان،اینلایهبهمدتیکساعتدر 150 درجهسلسیوسخشکشدهاستوآمورفاست. 80

شکل‏3‑24 بازدهرنگیشدنلایهa-WO3/rGO،اینلایهبهمدتیکساعتدر 150 درجهسلسیوسخشکشدهوآمورفاست. 81

شکل‏3‑25طیفپراشاشعهایکسلایه‌هایکلسینهشدهدردمای⁰C450. 83

شکل‏3‑26 تصویرFESEMنمونهبلورینWO3؛اینلایهبهمدتیکساعتدر 450 درجهسلسیوسکلسینهشده‌اندوبلوریناست. 85

شکل‏3‑27تصویرFESEMمقطعلایهc-WO3؛اینلایههابهمدتیکساعتدر 450 درجهسلسیوسکلسینهشده‌اندوبلورینهستند. 86

شکل‏3‑28 تصاویرFESEMلایهc-WO3/rGO؛اینلایههابهمدتیکساعتدر 450 درجهسلسیوسکلسینهشده‌اندوبلورینهستند. 87

شکل‏3‑29ولتاموگرامچرخه‌ایلایه‌هایبلورین. 88

شکل‏3‑30تستکرونوآمپرومتریلایه‌هایبلورین. 91

شکل‏3‑31تغییراتعبور-زماننمونهبلورینc-WO3. 93

شکل‏3‑32تغییراتعبورلایهc-WO3برحسبزمان. 93

شکل‏3‑33 تغییراتعبور-طول‌موجلایهc-WO3/rGO. 94

شکل‏3‑34تغییراتنوریلایهکامپوزیتبلورینبازمان. 95

231 دیدگاه برای دانلود پروژه: ساخت و مشخصه­یابی لایه­های نازک نانوکامپوزیتی Graphene-WO3 و بررسی خواص الکتروکرمیک

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