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MINISTRYOFEDUCATION ANDTRAINING QUYNHONUNIVERSITY TRUONGDUYHUONG SYNTHESISANDMODIFICATIONOFMS2(M= Mo,W)WITHg-C3N4FORPHOTOCATALYSIS MAJOR: PHYSICAL AND THEORETICAL CHEMISTRYCODENo.: 9440119 DOCTORALTHESISINCHEMISTRY BINHDINH-2021 TRUONGDUYHUONG SYNTHESISANDMODIFICATIONOFMS2(M= Mo,W)WITHg-C3N4FORPHOTOCATALYSIS MAJOR: PHYSICAL AND THEORETICAL CHEMISTRYCODENO.: 9440119 Reviewer 1:Dr Nguyen Van ThangReviewer 2:Assoc Prof Nguyen Duc CuongReviewer3:Assoc.Prof.TranThiVanThi Supervisor: Assoc.Prof.VOVIEN–QuyNhonUniversity BINHDINH–2021 DECLARATION This thesis has been completed at Quy Nhon University, in cooperationwithKULeuven,underthesupervisorofAssoc.Prof.VoVien.Iherebyassuret hatthisresearchprojectismine.Alltheresultsarehonest,havebeenapprovedbycoauthorsandhave not beenreleasedbyanyoneelsebefore Supervisor Author Assoc.Prof.VOVIEN TRUONGDUYHUONG ACKNOWLEDGEMENTS Firstly, from my heart, I would like to express my gratitude to both ofmy promoters, Assoc Prof Vo Vien and Prof M Enis Leblebici not only fortheir enthusiastic guidance, expertise and invaluable time, but also for theirencouragement when I encountered difficulties during the time of doing theresearch Furthermore, from the beginning to the very end of my study time inKULeuven,Belgium,Icould saythat without theconstant supportfromProf M Enis Leblebici my study would have not accomplished any progress as Ihave today Meanwhile, the belief that I have ability to the research fromAssoc Prof Vo Vien made me more energetic to overcome the tough time onmyscientificpathway Another professor who inspired me a lot and that also the one always isin my heart, Prof Tom Van Gerven He always gave me a warm welcome anda lovely smile that made me feel more confident and relax when we hadunforgetablegroupmeetingstogetheralongwithProf.M.EnisLeblebici.Iamnot exaggerated when say that the meeting time with both of you has been themostbeautifulmomentsthatIhaveexperiencedinmylife.Eveninthetimeofwriting this acknowledgement,Istillfeelthathappytimeinmymind.So,itisnoteasytoexpressthatfeelinginwords,especiallyinEnglish,I justtrytosayhowkindof youare Having the opportunity to study in Belgium, a heart of Europe how canIforgetthefinancialsupportfromVLIR-UOS,BelgiumwithTEAMprojectofcode ZEIN2016PR431 and title “Reinforcing the capabilities of Quy NhonUniversity- Vietnaminsolvinglocalproblemsbybuildingupadoctoral trainingprogram”.Withoutthisprojectalongwiththeeffortfromalltheprojectmaker members, including Prof Do Ngoc My (Rector of QNU), Prof NguyenTienTrung,Prof.VuThiNgan,Prof.VoVien,especiallyfromProf.MinhThoNguyen,m ydreamcouldnotcome true Ialsowouldliketothankmyfriendswhostoodwithmeinanycircumstances Those from Vietnam like Ms Vu Thi Lien Huong, rector of LeKhietHighSchoolfortheGifted,Mr.LeVanTrungchemistrygroupleaderofthe school and alllovelycolleagues.ToPhamHoangQuan,oneofmyclosestfriendswhotaughtmesomebasicexperimentalskillsfromthe beginning, thefact that you suddenly passed away made me could not believe, I promise totake care of your little daughter as much as I can within my ability, Mr TranDuc Trung for your help in heating my samples at Dung Quat Technology andEngineeringandencouragingmeintimewhenIhadtroubles,mystudentsQuoc Nhat and Quang Tan for your effort to the experiments in the schoollaboratory in the early days for the first Vsef that we achieved the best prize,the second group with Tuan Anh and Nguyen Khang, the third group with VuQuan and Anh Kiet, Mr Dinh Trong Nghia and Le Van Phuong for your timein coffee shops whenever I need someone to talk and those who I worked andmetinKULeuvensuchasLiefintheAdmissionOffice,AlenaintheSecretaryOffice,C hristineforyourinstructionsinthelabandcharacterizingmysamples,Michelle for your ordering chemicals, Ruijun for some wonderful parties,watching a football match of OH Leuven and XPS analysis, Thomas and Glenforyoursupportinthelab,Mohammedforyourniceconversation,Joris inMTM for your acceptance and instruction of using inert atmosphere furnace,the CIT football team which gave me a chance to be a goalkeeper for the firstseasonand thetimefrom adefenderforthesecond,Tri who being with meall CameloTorestoHomeVesalius,thetwonicefamilyofMr.ThanhHai&Mis.MienTrung, Hung&Hangwithalotofsupportfromtheearlydays,TanHung(little Hung) for your unforgettable Martini wine party and Hung, Linh, TuyetAnh, brother Giang for the last but beautiful visit My lovely group, Ms Lan,ThanhTam,ToNu,ZoanAn,HuuHa,allofyouarealsostillinmymindtodayandfuture Now, I would like to give all of my loving heart to my wife and twodaughtersHaKhanhandCaoNguyen,whoalwaysgivemeanunlimitedenergysour ceandthestrongestmotivationtoovercomethedifficultiesduringthetimeofstudying.Tomybeloved wife,youknow,yoursacrificeandhardworkingto take care our angels during the time I was away from home is the mostvaluable thing that I have ever had, that reminded me of the responsibility notonly to our little family but also to myself to keep my spirit on track withoutgiving up regardless the inevitable obstacles To my father, you have alwaysbeenbesidemeonmywayinspiteofthefactthatyouhaveletusaloneonthisplanet for sixyears,Imissyousomuch.Mama,howcanIshowhowmuchimportant you are to me when now you are become unique for my life, you donothavedirectcontributiontomywork,butthewayyou have overcome thebig loss made me feel that you have been hiding your broken heart to help metofocusmoreonmywork.Ialsowouldliketogivemysinceregratitudetomymotherandfather-inlawforyouruncountablesupportintermsoffinanceandemotion.MysiblingsThuy,Tai,Mis Tramandmybrother-in-lawBinh,allofyou alsoinmymindfor yoursentimentalvaluethatyougave me ItwouldbemybigmistakeifIdonotincludeagreatdealofefforttoreadandcor rectmythesisfromthemembersoftheBoardofJuriesforbothPremilinaryandPublicDefenc estothisacknowledgement.T h i s helpsmealot to realize that my thesis still need to be further revised, especially from thecarefulreadinganddetailedcorrectionsofthereviewer,Dr.NguyenVanThang.Addition to this, the useful comments from secretary of the Jury Dr Tran ThiThu Phuong also help me to pay much more attention to the last edit beforecompleting the thesis The others in the Juries in many ways also gave me theencouragement and positiveenergyto defensemythesissuccessfully Duetothepademic,thePublicDefencewasheldonlineandIwasatthepoint of Le Khiet Gifted High School There were some of my colleagues, theschoolleaders,myteacher(NguyenTruong)andfriends,therefore,attendedtomy defence Especially, Director of Education and Training Department ofQuangNgaiprovinceMr.NguyenNgocThaialsopresentedthere.Thepresence of the Director made me feel much more excited and the atmosphereofthedefence become much more formal I sincerely yoursignificantsupportinthatday ThankyouALL thank Mr Thai and theothers for CONTENTS DECLARATIONACKNO WLEDGEMENTSLIST OFTABLES LISTOFFIGURES INTRODUCTION Chapter1.LITERATUREREVIEW 1.1 OVERVIEWOFCURRENTPHOTOCATALYSTS 1.2 MS2-BASED(M=Mo,W)PHOTOCATALYSTS 1.2.1 StructuresofMS2(M=Mo,W) 1.2.2 MS2-basedcomposites 10 1.2.3 Synthesismethods 11 1.2.3.1 MS2(M=Mo,W)synthesis 11 1.2.3.2 MS2/g-C3N4synthesis .12 1.3 PHOTOCATALYTIC PROCESS, LIGHT SOURCES ANDASSESSMENTBENCHMARKS .13 1.3.1 Photocatalyticdegradationmechanism 13 1.3.2 Reactionkinetics 15 1.3.3 Adsorptionroleinphotocatalyticprocess 16 1.3.4.Lightsourcesforphotocatalysis–Lightemittingdiodes(LEDs)18 1.3.5 Photocatalyticreactorassessment 19 1.4 PHOTODEGRADATION OF ANTIBIOTICS AND DYES INAQUEOUSSOLUTION 21 1.4.1 Antibioticsphotodegradation 21 1.4.2 Dyesphotodegradation 22 1.5 PHOTOCATALYTICPILOTDESIGNOVERVIEW 24 1.5.1 Slurryreactorsversusimmobilizedcatalystreactors 25 1.5.2 Photocatalystseparation .26 1.5.2.1 Catalystimmobilization 26 1.5.2.2 Catalystseparation 27 Chapter2.EXPERIMENTALSECTION 28 2.1 CHEMICALSANDEQUIPMENT 28 2.2 MATERIALSFABRICATION .29 2.2.1 FabricationofWS2/g-C3N4 29 2.2.2 FabricationofMoS2/g-C3N4 31 2.3 CHARACTERIZATIONS 34 2.3.1 Materialcharacterizations .34 2.3.2 Determiningpointofzerocharge 34 2.3.3 Lightspectraandintensity 35 2.4 PHOTOCATALYTICEXPERIMENTS .35 2.4.1 Reactionsystem 35 2.4.2 Photocatalyticactivityevaluation 36 2.4.3 Calibrationcurves 38 2.4.4 Measurement of emitted irradiance using spectrophotometerprobe 39 2.4.5 CODmeasurement 40 2.4.6 High performance liquid chromatography (HPLC) and massspectrometry(MS) 40 2.4.7 Activespeciesdetermination 41 2.4.8 Oxidizingagent .41 2.5 PILOTDESIGN 42 2.5.1 Pilotdescriptionandoperatingprinciples 42 2.5.2 Detailedinstructions 43 2.5.3 TimingprogramforArduinocircuit 46 2.5.4 Sedimentationprocedureandcatalystrecoverypercentage .46 2.6 CALCULATIONS .47 2.6.1 Reaction rate constant and photochemical space-time yield(PSTY) 47 2.6.2 Adsorption capacity .47 2.6.3 Flowrate forturbulentregime 48 2.6.4 Throughput forphotocatalytic pilot 48 Chapter3.RESULTSANDDISCUSSION 49 3.1 MATERIALCHARACTERIZATIONS .49 3.1.1 WS2/g-C3N4characterizations .49 3.1.1.1 X-raydiffraction 49 3.1.1.2 Scanning electronmicroscopy .50 3.1.1.3 Energy-dispersiveX-rayelementalmapping 51 3.1.1.4 Transmissionelectronmicroscopy 52 3.1.1.5 Infraredspectroscopy .53 3.1.1.6 Raman spectroscopy .54 3.1.1.7 X-rayphotoelectronspectroscopy 55 3.1.1.8 Thermogravimetricanalysis 57 3.1.1.9 UV-Visdiffusereflectancespectroscopy 58 3.1.2 MoS2/g-C3N4characterizations .59 3.1.2.1 X-raydiffraction 59 3.1.2.2 Infraredspectroscopy .60 3.1.2.3 X-rayphotoelectronspectroscopy 61 3.1.2.4 BETSurfacearea analysis 62 3.1.2.5 Thermogravimetricanalysis 63 3.1.2.6 UV–vis diffusereflectance spectroscopy 65 3.1.2.7 Energy-dispersiveX-rayelementalmapping 65 3.2 MATERIALPHOTOCATALYTICACTIVITY 67 3.2.1 Adsorption-desorption equilibriumtime 67 3.2.2 Photocatalyticactivitycomparisons .69 3.2.3 Effectofcatalyst loading 72
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