From b905a14ef59c122be0eea6efb484090d40fb359d Mon Sep 17 00:00:00 2001 From: Davide Grilli Date: Fri, 9 Oct 2026 23:39:52 +0200 Subject: [PATCH] Aggiunge presentazione per la discussione e riassunto della tesi; aggiorna indice, log e figure Include slide Marp, discorso e figure in presentazione/, il riassunto in wiki/analyses/ e le modifiche pendenti a index, log, raw/ e wiki/figures. Co-Authored-By: Claude Sonnet 5.5 --- .obsidian/graph.json | 2 +- index.md | 3 +- log.md | 12 ++ presentazione/Riassunto_tesi.docx | Bin 0 -> 180393 bytes presentazione/discorso.md | 170 ++++++++++++++++ presentazione/discussione.pptx | Bin 0 -> 286172 bytes presentazione/immagini/fig1-dpp.jpg | Bin 0 -> 13200 bytes presentazione/immagini/fig2-sintesi-dpp1.jpg | Bin 0 -> 21393 bytes .../immagini/fig3-alchilazione-dpp2.jpg | Bin 0 -> 21403 bytes .../immagini/fig4-copolimerizzazione.jpg | Bin 0 -> 23421 bytes .../immagini/fig5-rop-bottle-brush.jpg | Bin 0 -> 32846 bytes presentazione/immagini/fig6-uv-em-3.2b.jpg | Bin 0 -> 52818 bytes .../immagini/fig7-bandgap-vs-dpp.jpg | Bin 0 -> 31109 bytes presentazione/riassunto_tesi.md | 110 ++++++++++ presentazione/slides.md | 189 ++++++++++++++++++ wiki/analyses/riassunto-tesi.md | 141 +++++++++++++ 16 files changed, 625 insertions(+), 2 deletions(-) create mode 100644 presentazione/Riassunto_tesi.docx create mode 100644 presentazione/discorso.md create mode 100644 presentazione/discussione.pptx create mode 100644 presentazione/immagini/fig1-dpp.jpg create mode 100644 presentazione/immagini/fig2-sintesi-dpp1.jpg create mode 100644 presentazione/immagini/fig3-alchilazione-dpp2.jpg create mode 100644 presentazione/immagini/fig4-copolimerizzazione.jpg create mode 100644 presentazione/immagini/fig5-rop-bottle-brush.jpg create mode 100644 presentazione/immagini/fig6-uv-em-3.2b.jpg create mode 100644 presentazione/immagini/fig7-bandgap-vs-dpp.jpg create mode 100644 presentazione/riassunto_tesi.md create mode 100644 presentazione/slides.md create mode 100644 wiki/analyses/riassunto-tesi.md diff --git a/.obsidian/graph.json b/.obsidian/graph.json index 83ecb44..0baffdb 100644 --- a/.obsidian/graph.json +++ b/.obsidian/graph.json @@ -17,6 +17,6 @@ "repelStrength": 10, "linkStrength": 1, "linkDistance": 250, - "scale": 0.2588386562181621, + "scale": 0.3628873693012104, "close": true } \ No newline at end of file diff --git a/index.md b/index.md index e2a88c6..aa60475 100644 --- a/index.md +++ b/index.md @@ -1,6 +1,6 @@ # Indice della wiki -_Catalogo di tutte le pagine. Aggiornato a ogni ingest/query. Pagine curate: 28 · Figure generate: 78 · Fonti ingerite: 1 (la tesi)_ +_Catalogo di tutte le pagine. Aggiornato a ogni ingest/query. Pagine curate: 29 · Figure generate: 78 · Fonti ingerite: 1 (la tesi)_ ## Overview - [[overview]] — problema, strategia, risultati dichiarati e limiti della tesi @@ -44,3 +44,4 @@ _Catalogo di tutte le pagine. Aggiornato a ogni ingest/query. Pagine curate: 28 ## Analisi - [[difetti-noti]] — difetti noti della tesi e incoerenze rilevate nell'ingest +- [[riassunto-tesi]] — riassunto in formato 10 pagine (testo continuo, 7 figure, 3 tabelle, 10 riferimenti) diff --git a/log.md b/log.md index d1ca4bc..7e3c5fb 100644 --- a/log.md +++ b/log.md @@ -45,3 +45,15 @@ _Append-only. Formato: `## [YYYY-MM-DD] tipo | titolo`_ - `cv-risultati-copolimeri` + `cv-risultati-bottle-brush` -> `techniques/cv-risultati` (Tab. 13 e 14); link in entrata aggiornati - `compounds/reagenti-e-materiali` -> `techniques/reagenti-e-materiali` (non è un composto numerato) - Rimossi i `.gitkeep`; CLAUDE.md, `index.md`, `wiki/tesi.md` aggiornati. Lasciate invariate `dpp-sintesi-letteratura` (1.515) e `fluorofori-in-polimeri` + +## [2026-10-09] query | Riassunto della tesi in formato 10 pagine +- Richiesta: riassunto secondo le regole del formato (copertina placeholder, testo continuo senza sottotitoli/elenchi, max 10 pagine, bibliografia a parte, usare la Figura 74) +- Salvato in `wiki/analyses/riassunto-tesi.md` (Fig. 74 della tesi = Figura 6 del riassunto); 7 figure, 3 tabelle, 10 riferimenti dalle schede `raw/fonti/` +- Esclusi i valori di band gap/R² delle Conclusioni (incoerenti con Tab. 13) e la durata del reflusso ROP (4 h/24 h): vedi `difetti-noti` + +## [2026-10-09] query | Seconda stesura del riassunto in registro da ricercatore +- `wiki/analyses/riassunto-tesi.md` riscritto: affermazioni non supportate rimosse (es. «forte fluorescenza in soluzione»), emissione solida di 3.2b qualificata come da specie aggregate (ACQ attenuato, non eliminato), aggiunte note critiche (copolimeri oligomerici, correlazione bandgap su 3 punti, scarto gap elettrochimico/ottico) +- Le inferenze dell'autore sono elencate nella sezione Collegamenti della pagina + +## [2026-10-09] query | Terza stesura del riassunto, allineata alla tesi +- `wiki/analyses/riassunto-tesi.md`: rimosse le inferenze della seconda stesura; contenuti e interpretazioni solo dalla tesi (limiti e prospettive dalle sezioni 4.2-4.3 e Conclusioni); per le incoerenze interne si usa il capitolo dei risultati (vedi `difetti-noti`, punti 5-7) diff --git a/presentazione/Riassunto_tesi.docx b/presentazione/Riassunto_tesi.docx new file mode 100644 index 0000000000000000000000000000000000000000..31864beed8aa7327caa5fe34934514240fcce663 GIT binary patch literal 180393 zcmZ^Kb8si^vv0VuwXtn&%#Cf^w(aB_+qP}nwry_g8HA$ z{&Y`|oFph1G|)endxg06zr=rT;D4X4whl)0a{pfznEz(cbuhMa{2xZhe|6d@?h&Clp*laK$3i}Stb}#>tMz^o0gf`M_#b+Q1 zZPvH|22iH=&_@gdv|9x+CgW2UHv{)hC0r5s-WQG`rX<e?@haCoztJ1 zd1}o0xF55R=SSEARL$W87lXtOQbQSaoA;D80%KVT&BA;cGm}`sl%3HjPUfE{%-!Ud 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zwm%gxFTeHbo3-TiS2?Rehx5Z9d92q8XV#1@trO8C%=D5Hr!7K@H{R?m|AT zL-vq?4_M=Oc|e!Cbknn%Qh}KBP*fh7YI|i**_G&MskpBsa9(`VW50ra&)%Wr36hlm zLceICWz>snUB1E1CR-raGOnSmmsQ~>FOf-3Oh|>6WD_3jg!f*3P9}89@8Lvy-~a{>7Jr2!To{SEyAep z$k~;MqvqF=^LUKWt}?ZqFP-|UU>vj)t2d=4(mk}X4d(F`G`hmc5~e-17P=2BE;$7+N;HGK8T`yUaeV}K)bFxJ=FEIg5fD37_QeBR4>tm zle-pX>RleUD8Wa)Uo77~4nD}yacZcSMHSkKq-myye5B7t0oy-`S?D`aqU&fqgGDN= zoupNrreDJvm;+A|9fx)XXRpS|?wnT_Fta4YS@4q&1mS{wF1yC#p3&7GZ2VwdVz}g` z1 Per impiegarli in un dispositivo occorre governarne le proprietà ottiche ed elettroniche, cioè ingegnerizzare il band gap. La strategia d'elezione è l'approccio donatore-accettore (D-A), che alterna unità fortemente elettron-deficienti e unità elettron-ricche lungo lo scheletro π-coniugato: l'orbitale HOMO è determinato principalmente dalla porzione donatrice e il LUMO dall'unità accettrice, e il trasferimento di carica intramolecolare che ne deriva riduce il salto energetico e permette di centrare assorbimento ed emissione nel visibile.2 + +I materiali semiconduttori π-coniugati perdono spesso le proprietà ottiche allo stato solido. La natura altamente planare del loro scheletro induce intense interazioni di π-stacking tra le catene adiacenti, che causano la drastica dissipazione non radiativa dell'energia eccitonica e lo smorzamento della fluorescenza: è l'ACQ. Questo limita le applicazioni pratiche dei materiali, perché nello strato emissivo di un OLED è richiesta proprio l'emissione. Per ovviare al problema, la tesi propone una strategia di design macromolecolare basata su architetture a spazzola (bottle brush), il cui scopo è promuovere la separazione fisica dei segmenti planari coniugati, ripristinando le proprietà emissive allo stato solido e preservando integrità elettrochimica e stabilità del sistema. + +Come unità accettrice è stato scelto il DPP, formato da due anelli lattamici a cinque termini condensati, con sostituenti aromatici o eteroaromatici in posizione 3 e 6 *(Figura 1)*. Nato come pigmento rosso industriale, il DPP ha punto di fusione superiore a 350 °C e solubilità molto bassa, dovute a un fitto network di legami a idrogeno ammidici e di π-stacking tra i piani molecolari.3 Il nucleo è planare e fortemente elettron-deficiente, e la rigidità dello scheletro limita il rilassamento vibrazionale e lo Stokes shift. Nel passaggio dalla soluzione al film il DPP mostra un allargamento della banda di assorbimento e un marcato effetto batocromico, con spostamento del picco di circa 30 nm. + +![](immagini/fig1-dpp.jpg) + +Figura 1. Struttura generica di un dichetopirrolopirrolo. + +L'inserimento di un fluoroforo in un sistema polimerico richiede un accurato design molecolare, perché l'architettura scelta influenza drasticamente le proprietà finali. Nei sistemi host-guest il fluoroforo è disperso fisicamente nella matrice: la preparazione è semplice, ma la scarsa stabilità a lungo termine, con migrazione e aggregazione dell'ospite, porta a perdita di resa quantica. Nei sistemi main-chain il fluoroforo è parte integrante della catena principale, con sintesi più complessa; una strategia riuscita è il grafting-from, in cui un DPP bifunzionalizzato con gruppi ossidrilici inizia la crescita di due catene di PCL, dando PCL-DPP-PCL.4 Nei sistemi side-chain le unità luminescenti sono catene laterali, spesso con uno spaziatore flessibile che limita le interazioni tra cromofori; nei sistemi cross-linked il cromoforo è ancorato da ponti chimici e non aggrega, ma l'eccessiva rigidità rende il materiale fragile, insolubile e difficile da lavorare. La tesi adotta il grafting-from per innestare catene laterali di PCL su uno scheletro semiconduttore DPP-3HT. + +Il monomero è un derivato del DPP definito ortogonale e tetrafunzionale: gli anelli tiofenici forniscono i siti per la polimerizzazione ossidativa dello scheletro, mentre i due gruppi ossidrilici primari, portati dalle catene esiliche sugli azoti lattamici, fungono da iniziatori per la polimerizzazione ad apertura di anello (ROP). Il gruppo aveva già studiato fluorofori DPP con sostituenti diversi in para sull'anello benzonitrilico: quelli elettron-attrattori davano sistemi altamente emissivi, quelli elettron-donatori un isomero strutturale (iso-DPP) a fluorescenza inibita. In questo lavoro i benzeni sono sostituiti da tiofeni e i gruppi ammidici sono N-alchilati, con aumento della solubilità e una procedura semplice e scalabile. Il 3HT è il comonomero donatore: i politiofeni sono tra i più efficienti polimeri semiconduttori organici5 e la catena esilica aumenta la solubilità nei solventi organici. La polimerizzazione ossidativa con FeCl3 è stata preferita ai cross-coupling al palladio perché non richiede pre-funzionalizzazione dei monomeri, opera a temperatura e pressione ambiente ed è scalabile, a fronte di un controllo minore su polidispersità e regioregolarità. La distribuzione statistica dei monomeri aumenta l'entropia conformazionale, limita il packing e rende più accessibili gli ossidrili per la funzionalizzazione. + +Il PCL è stato scelto sulla base di studi precedenti del gruppo, per la bassa temperatura di transizione vetrosa e la buona solubilità nei solventi organici; la ROP dell'ε-caprolattone catalizzata da stagno ottanoato (Sn(Oct)2) è un processo lineare ed efficiente, procede per coordinazione-inserzione con un alcol come coiniziatore e permette di regolare il peso molecolare e di mantenere bassa la dispersità delle catene.6 La lunghezza delle catene si modula con il rapporto molare monomero/ossidrili, con valori nominali di 1500, 5000 e 10000 Da. I copolimeri sono stati alimentati con il 20%, 50% e 80% in moli di DPP; i bottle brush sono stati preparati da **3b** e **3c**, mentre **3a** non è stato usato a causa della scarsa efficienza della sua via sintetica, con basse rese e difficoltà di work-up, e di volumi di solventi e costi di reagenti troppo elevati per isolarne quantità utili. + +Lo scopo del progetto è sintetizzare e caratterizzare copolimeri bottle brush foto-elettro attivi a base di DPP e 3HT con catene laterali di PCL, al fine di superare l'ACQ allo stato solido mantenendo l'integrità elettrochimica del nucleo DPP. Il lavoro comprende due macroaree: la sintesi del monomero ortogonale e l'ottenimento dei materiali, cioè scheletro coniugato e catene innestate. + +Il DPP tiofenico **1** *(Figura 2)* è stato ottenuto per ciclizzazione pseudo-Stobbe tra 2-cianotiofene e diisopropil succinato.7 La base forte è il teramilato di sodio, ottenuto dal sodio in alcol ter-amilico con FeCl3 catalitico: deprotona il succinato in α al carbonile, il carbanione attacca il carbonio nitrilico e il composto imminico tautomerizza a enammina, che attacca il carbonile estereo chiudendo il primo anello a cinque termini; una seconda deprotonazione e l'attacco di una seconda molecola di tiofene portano al secondo anello. Il succinato è stato aggiunto lentamente, perché una concentrazione locale troppo alta in condizioni basiche induce autocondensazione di Claisen, e si è scelto il diisopropil succinato per aumentare l'ingombro intorno al carbonile e ridurre questa reazione.8 Il prodotto, un solido rosso scuro violaceo, è stato purificato sfruttando la netta differenza di solubilità tra reagenti e prodotto, con lavaggi in acqua e metanolo. Il 1H-NMR in DMSO mostra a circa 11 ppm il singoletto allargato dei protoni ammidici; in THF **1** ha massimo di assorbimento a 531 nm, di emissione a 542 nm e Stokes shift di 11 nm. + +![](immagini/fig2-sintesi-dpp1.jpg) + +Figura 2. Sintesi del DPP **1** da 2-cianotiofene e diisopropil succinato con teramilato di sodio e FeCl3 catalitico. + +L'N-alchilazione di **1** con 6-bromo-1-esanolo *(Figura 3)* sfrutta la reattività dei gruppi ammidici, deprotonati da ter-butossido di potassio in DMSO, che attaccano per sostituzione nucleofila il carbonio adiacente al bromo, e dà il monomero **2** con due braccia idrossiesiliche. La tesi segnala come reazione collaterale la ciclizzazione del 6-bromo-1-esanolo, favorita da un eccesso di base. Il prodotto è stato lavato con soluzione satura di KCl e purificato per cristallizzazione da etanolo a −20 °C. L'N-alchilazione è confermata nel 1H-NMR dai multipletti alifatici a 4,1 ppm (metileni legati all'azoto lattamico) e a 3,6 ppm (metileni adiacenti all'ossidrile terminale), e nel FT-IR dalla banda larga dell'O-H a circa 3400 cm-1 insieme al C=O lattamico a circa 1650 cm-1. Il massimo di assorbimento passa da 531 nm (**1**) a 541 nm (**2**): lo spostamento batocromico è attribuito all'effetto induttivo elettron-donatore delle catene alifatiche, che arricchiscono di densità elettronica gli azoti, destabilizzano l'HOMO e restringono il band gap ottico. + +![](immagini/fig3-alchilazione-dpp2.jpg) + +Figura 3. N-alchilazione del DPP **1** con 6-bromo-1-esanolo (DMSO, ter-butossido di potassio, 40 °C) a dare il monomero **2** con due catene idrossiesiliche. + +Il monomero **2** è stato copolimerizzato con 3HT per via ossidativa, con FeCl3 in nitrometano e cloroformio anidro *(Figura 4)*. Il FeCl3, in eccesso stechiometrico, estrae per trasferimento mono-elettronico un elettrone dagli anelli tiofenici, generando cationi radicalici delocalizzati che formano i nuovi legami C-C. Il nitrometano rompe i dimeri di FeCl3 e ne modera acidità di Lewis e potere ossidante, prevenendo sovraossidazione e difetti di reticolazione; il cloroformio anidro evita che l'acqua si coordini al FeCl3 e spenga per attacco nucleofilo gli intermedi cationico-radicalici. L'ossidante è stato rimosso con lavaggi con HCl 0,6 M fino a saggio negativo del tiocianato, perché tracce di metalli di transizione abbatterebbero la mobilità dei portatori e spegnerebbero la fluorescenza, e l'omopolimero del 3HT è stato eliminato per precipitazione in metanolo freddo. L'integrazione di DPP si è limitata a un massimo del 35% *(Tabella 1)*: la tesi lo attribuisce alla differenza nei rapporti di reattività dei comonomeri, influenzata dall'ingombro sterico del DPP, mentre il tiofene, più reattivo e meno voluminoso, addiziona preferenzialmente. Le percentuali reali sono state determinate via 1H-NMR. + +![](immagini/fig4-copolimerizzazione.jpg) + +Figura 4. Copolimerizzazione ossidativa del DPP **2** con 3-esiltiofene con FeCl3 a dare i copolimeri **3a**, **3b** e **3c**. + +Tabella 1. Composizione dei copolimeri e pesi molecolari da GPC. + +| **Copolimero** | **% DPP teorica (mol/mol)** | **% DPP reale (mol/mol)** | **Mn (Da)** | **Mw (Da)** | **PD** | +|---|---|---|---|---|---| +| **3a** | 20 | 25,2 | 2149 | 5526 | 2,571 | +| **3b** | 50 | 32,6 | 1402 | 6439 | 4,592 | +| **3c** | 80 | 35,3 | 2134 | 4223 | 1,979 | + +I copolimeri hanno Mn tra 1402 e 2149 Da. Valori di PD intorno a 2 o superiori sono attesi per una polimerizzazione non controllata, con distribuzione più probabile di Flory; **3c** ha la distribuzione più omogenea (PD 1,979), mentre **3b**, con Mn più bassa ma Mw più alta, indica una frazione significativa di oligomeri a catena corta accanto a macromolecole di peso molecolare più elevato. Il FT-IR conferma l'incorporazione del DPP con il C=O lattamico a circa 1650 cm-1, e la DSC mostra per tutti i campioni una transizione vetrosa intorno a −10 °C e nessuna transizione di fusione, a conferma della natura random dei copolimeri, il cui disordine impedisce la cristallizzazione. In soluzione di THF i tre copolimeri hanno profili ottici pressoché identici, simili a quello del monomero: assorbimento tra 540 e 544 nm, emissione intorno a 550 nm e Stokes shift tra 6 e 10 nm. Allo stato solido il comportamento è drasticamente diverso: l'intenso impaccamento delle catene forma aggregati che disattivano i fluorofori per decadimento non radiativo, e i film su vetrino sotto lampada UV non mostrano emissione apprezzabile. È la principale criticità dei sistemi lineari per l'uso in dispositivi optoelettronici e giustifica il passaggio al design bottle brush. + +I sei bottle brush **3.1b**, **3.2b**, **3.3b**, **3.1c**, **3.2c** e **3.3c** sono stati ottenuti per ROP dell'ε-caprolattone dagli ossidrili di **3b** e **3c**, in toluene a 110 °C con Sn(Oct)2 catalitico, con il monomero dosato sul numero di ossidrili per ottenere catene di 1500, 5000 e 10000 Da *(Figura 5)*. L'avvenuto innesto è verificato dal 1H-NMR, con il tripletto del PCL a circa 4,0 ppm (CH2-O adiacente all'ossigeno estereo) e il segnale a 2,3 ppm dei protoni in α al carbonile, e dal FT-IR, in cui la banda dell'O-H a 3600-3200 cm-1 dei macroiniziatori scompare e compare il C=O estereo a circa 1720 cm-1. La GPC fornisce Mn tra 12188 e 21269 Da e indici di dispersità contenuti (1,238-1,521). + +![](immagini/fig5-rop-bottle-brush.jpg) + +Figura 5. Polimerizzazione ad apertura di anello dell'ε-caprolattone sui gruppi OH dei copolimeri DPP-3HT, a dare i bottle brush con catene di PCL. + +I pesi molecolari da GPC *(Tabella 2)* sono significativamente sottostimati rispetto ai teorici: la GPC separa per volume idrodinamico e restituisce valori relativi agli standard di polistirene lineare, mentre un polimero altamente ramificato assume in soluzione una conformazione compatta, con volume idrodinamico nettamente inferiore. I dati non indicano quindi il peso molecolare assoluto né una bassa resa, ma confermano indirettamente una struttura ramificata altamente impaccata e permettono il confronto tra i polimeri. Il campione **3.3c** si discosta dall'andamento generale; la tesi ipotizza che, essendo il materiale di partenza random, elevate concentrazioni locali di DPP e di ossidrili abbiano ridotto la crescita delle catene laterali per ingombro sterico, e indica che le discrepanze saranno investigate in futuro con ulteriori analisi. Per superare i limiti della GPC è stato calcolato il peso molecolare via 1H-NMR dal grado di polimerizzazione delle catene di PCL, ottenendo una stima descritta come più vicina ai valori teorici. Dal punto di vista termico, la DSC mostra per tutti i bottle brush transizioni dominate dal PCL, con fusione tra 55 e 60 °C e cristallizzazione tra 25 e 35 °C. + +Tabella 2. Pesi molecolari dei bottle brush da GPC e da 1H-NMR, con il valore teorico. + +| **Polimero** | **Mn PCL teorico (Da)** | **Mn GPC (Da)** | **PD** | **Peso molecolare teorico (Da)** | **Peso molecolare da 1H-NMR (Da)** | +|---|---|---|---|---|---| +| **3.1b** | 1500 | 12188 | 1,521 | 6500 | 8900 | +| **3.2b** | 5000 | 17302 | 1,314 | 18000 | 20500 | +| **3.3b** | 10000 | 21269 | 1,238 | 34500 | 88000 | +| **3.1c** | 1500 | 13999 | 1,301 | 10000 | 18200 | +| **3.2c** | 5000 | 19119 | 1,275 | 28500 | 35500 | +| **3.3c** | 10000 | 14445 | 1,351 | 55000 | 41300 | + +La caratterizzazione ottica in soluzione di THF mostra che la funzionalizzazione sterica non perturba l'integrità elettronica del core DPP: i massimi di assorbimento cadono tra 544 e 554 nm, quelli di emissione tra 557 e 564 nm e gli Stokes shift tra 8 e 14 nm. Le piccole fluttuazioni nelle due serie non seguono un andamento lineare con il peso molecolare del PCL e sono trascurabili, quindi l'ingombro sterico non perturba livelli energetici e natura delle transizioni. Il basso Stokes shift conferma la conservazione dell'assetto planare del cromoforo e la minima riorganizzazione tra stato fondamentale ed eccitato, e i domini flessibili di PCL allontanano le catene principali, riducendo l'impaccamento senza distorcere la geometria del backbone. + +La caratterizzazione allo stato solido è stata condotta sul campione **3.2b**, confrontando soluzione e solido *(Figura 6)*. Le misure in soluzione diluita indagano la singola catena isolata e solvatata; allo stato solido la vicinanza tra le macromolecole genera forti interazioni intermolecolari che alterano i livelli energetici e i processi di assorbimento ed emissione. In soluzione il massimo di assorbimento è a circa 550 nm e quello di emissione a circa 560-565 nm, con banda stretta e strutturata. Allo stato solido l'assorbimento mostra un significativo allargamento e un marcato effetto batocromico, con il massimo nell'intervallo 570-580 nm, attribuito alla planarizzazione dello scheletro, che estende la lunghezza di coniugazione effettiva. L'emissione è notevolmente allargata e fortemente spostata verso il rosso, con massimo centrato intorno a 650-660 nm e Stokes shift di circa 80-90 nm, probabilmente legato al maggiore ingombro delle catene, che obbliga gli anelli aromatici a torsioni maggiori, ed evidenza di una forte aggregazione intermolecolare. Secondo la tesi, dopo la fotoeccitazione l'energia migra verso siti a minore energia generati dalla vicinanza dei piani coniugati e il rilassamento radiativo avviene prevalentemente da stati aggregati o specie eccimeriche, nel quadro dell'accoppiamento eccitonico di Kasha tra aggregati H e J.9,10 Nonostante questi riarrangiamenti, l'architettura bottle brush mantiene un'apprezzabile emissione nel rosso, attenuando i percorsi di disattivazione non radiativa tipici dell'ACQ non controllato, in accordo con il ruolo del PCL come spaziatore sterico. + +![](immagini/fig6-uv-em-3.2b.jpg) + +Figura 6. Confronto tra spettri UV-Vis (in nero) ed emissione (in rosso) del polimero **3.2b** in soluzione (linea continua) e allo stato solido (linea tratteggiata). + +La ciclovoltammetria mostra per i polimeri un trasferimento di carica irreversibile di tipo elettrochimico-chimico, dovuto all'elevata reattività dei cationi e degli anioni radicali all'interfaccia elettrodica. Dagli onset di ossidazione e riduzione, calibrati sul ferrocene (posto a −4,8 eV rispetto al livello del vuoto), sono stati ricavati HOMO, LUMO e band gap elettrochimico *(Tabella 3)*. Nei copolimeri lineari si osserva un allargamento progressivo del band gap all'aumentare della frazione reale di DPP, da 0,970 a 1,371 eV *(Figura 7)*, con correlazione lineare (R² = 0,9719) guidata soprattutto dallo spostamento del potenziale di riduzione verso valori più negativi. La tesi lo interpreta come riduzione della lunghezza di coniugazione effettiva dovuta all'unità DPP, che limita la delocalizzazione π e aumenta la separazione HOMO-LUMO, e vi riconosce la possibilità di un controllo mirato del band gap calibrando il rapporto tra i monomeri. Rispetto al poli-3HT, che si ossida a potenziali accessibili ma non mostra contributi faradici in riduzione, nei copolimeri il DPP, forte porzione elettron-attrattrice in un'architettura D-A, stabilizza il LUMO e rende favorevole l'iniezione di elettroni. + +![](immagini/fig7-bandgap-vs-dpp.jpg) + +Figura 7. Correlazione tra band gap elettrochimico e frazione reale di DPP nei copolimeri lineari. + +Tabella 3. Livelli HOMO, LUMO e band gap elettrochimici dei copolimeri lineari e dei bottle brush. + +| **Polimero** | **HOMO (eV)** | **LUMO (eV)** | **Bandgap (eV)** | +|---|---|---|---| +| **3a** | -5,038 | -4,068 | 0,970 | +| **3b** | -4,854 | -3,538 | 1,316 | +| **3c** | -4,799 | -3,428 | 1,371 | +| **3.1b** | -4,617 | -3,580 | 1,037 | +| **3.2b** | -4,625 | -3,527 | 1,098 | +| **3.3b** | -4,630 | -3,598 | 1,032 | +| **3.1c** | -4,774 | -3,253 | 1,521 | +| **3.2c** | -4,688 | -3,269 | 1,419 | +| **3.3c** | -4,479 | -3,550 | 0,929 | + +I bottle brush mantengono l'elettroattività dello scheletro: i processi redox avvengono a carico del core DPP-3HT, mentre i rami alifatici fungono da matrice dielettrica circostante. Le ingombranti catene laterali modificano HOMO e LUMO rispetto ai lineari, e quindi l'ampiezza del band gap, che nei bottle brush è compresa tra 0,929 e 1,521 eV; la tesi attribuisce l'effetto all'ingombro sterico dei rami di PCL sul grado di coplanarità locale dello scheletro, e quindi sull'estensione effettiva della delocalizzazione. L'ingegnerizzazione con PCL non compromette, secondo la tesi, le spiccate potenzialità optoelettroniche del sistema. + +In conclusione, i risultati confermano secondo la tesi la validità del design proposto: l'approccio ortogonale basato su scheletri semiconduttori DPP-3HT modificati con catene laterali di PCL combina proprietà elettrochimiche modulabili e capacità emissiva allo stato solido. Dal punto di vista sintetico, monomeri ortogonali derivati dal DPP, polimerizzazione ossidativa con FeCl3 e ROP hanno portato a tre copolimeri statistici e a due serie di bottle brush con catene laterali di PCL di lunghezza nominale crescente. Il nucleo DPP conserva in soluzione le proprietà ottiche e, allo stato solido, il bottle brush **3.2b** mantiene un'apprezzabile emissione nel rosso; la composizione monomerica si rivela un parametro di controllo del band gap. I limiti dichiarati nel testo sono l'integrazione di DPP non superiore al 35%, l'esclusione di **3a** dall'innesto, la sottostima dei pesi molecolari da GPC e le discrepanze di **3.3c**, da indagare con ulteriori analisi. La prospettiva indicata dalla tesi è l'impiego di questi materiali in dispositivi optoelettronici, in particolare come strato elettro-luminescente in OLED. + +**Bibliografia** +- Ostroverkhova, O. Organic Optoelectronic Materials: Mechanisms and Applications. *Chem. Rev.* **2016**, *116*, 13279-13412. https://doi.org/10.1021/acs.chemrev.6b00127 +- Kroon, R.; Lenes, M.; Hummelen, J. C.; Blom, P. W. M.; de Boer, B. Small Bandgap Polymers for Organic Solar Cells (Polymer Material Development in the Last 5 Years). *Polym. Rev.* **2008**, *48*, 531-582. https://doi.org/10.1080/15583720802231833 +- Bao, W. W.; Li, R.; Dai, Z. C.; Tang, J. X.; Shi, X.; Geng, J. T.; Deng, Z. F.; Hua, J. Diketopyrrolopyrrole (DPP)-Based Materials and Its Applications: A Review. *Front. Chem.* **2020**, *8*, 679. https://doi.org/10.3389/fchem.2020.00679 +- Wang, K. Y.; Luo, Y.; Huang, S.; Yang, H.; Liu, B.; Wang, M. Highly Fluorescent Polycaprolactones Decorated with Di(thiophene-2-yl)-diketopyrrolopyrrole: A Covalent Strategy of Tuning Fluorescence Properties in Solid States. *J. Polym. Sci., Part A: Polym. Chem.* **2015**, *53*, 1032-1042. https://doi.org/10.1002/pola.27531 +- Abdel Aziz, I.; Tullii, G.; Antognazza, M. R.; Criado-Gonzalez, M. Poly(3-hexylthiophene) as a Versatile Semiconducting Polymer for Cutting-Edge Bioelectronics. *Mater. Horiz.* **2025**, *12*, 5570-5593. https://doi.org/10.1039/d5mh00096c +- Labet, M.; Thielemans, W. Synthesis of Polycaprolactone: A Review. *Chem. Soc. Rev.* **2009**, *38*, 3484. https://doi.org/10.1039/b820162p +- Iqbal, A. F. M.; Jost, M.; Kirchmayr, R.; Pfenninger, J.; Rochat, A.; Wallquist, O. The Synthesis and Properties of 1,4-Diketo-pyrrolo[3,4-C]pyrroles. *Bull. Soc. Chim. Belg.* **1988**, *97*, 615-644. https://doi.org/10.1002/bscb.19880970804 +- Grzybowski, M.; Gryko, D. T. Diketopyrrolopyrroles: Synthesis, Reactivity, and Optical Properties. *Adv. Opt. Mater.* **2015**, *3*, 280-320. https://doi.org/10.1002/adom.201400559 +- Kasha, M.; Rawls, H. R.; El-Bayoumi, M. A. The Exciton Model in Molecular Spectroscopy. *Pure Appl. Chem.* **1965**, *11*, 371-392. https://doi.org/10.1351/pac196511030371 +- Spano, F. C.; Silva, C. H- and J-Aggregate Behavior in Polymeric Semiconductors. *Annu. Rev. Phys. Chem.* **2014**, *65*, 477-500. https://doi.org/10.1146/annurev-physchem-040513-103639 diff --git a/presentazione/slides.md b/presentazione/slides.md new file mode 100644 index 0000000..d185ae1 --- /dev/null +++ b/presentazione/slides.md @@ -0,0 +1,189 @@ +--- +marp: true +theme: default +paginate: true +size: 16:9 +style: | + section { font-size: 26px; } + h1 { color: #8b1a1a; } + h2 { color: #8b1a1a; } + img { display: block; margin: 0 auto; } + .cols { display: grid; grid-template-columns: 1fr 1fr; gap: 1em; align-items: center; } + small { font-size: 0.6em; } +--- + + + +# Sintesi e caratterizzazione di copolimeri *bottle brush* foto-elettro attivi + +Aurora Luzi +Relatore: Dr. Stefano Scurti + +Tesi magistrale in Chimica Industriale — Università di Bologna, Dip. "Toso Montanari" — a.a. 2025-2026 + + + +--- + +## Contesto: perché polimeri π-coniugati emissivi + +- Optoelettronica organica (OLED, fotovoltaico): materiali leggeri, flessibili, depositabili da soluzione a bassa T +- Band gap ingegnerizzato con l'approccio **donatore-accettore (D-A)**: HOMO sul donatore, LUMO sull'accettore, trasferimento di carica intramolecolare +- **Problema: ACQ** (Aggregation-Caused Quenching) — il π-stacking delle catene planari dissipa l'energia in modo non radiativo → niente emissione nel film, proprio dove serve (strato emissivo OLED) + + + +--- + +## Scopo e strategia + +**Research question:** un'architettura *bottle brush* può superare l'ACQ allo stato solido, mantenendo l'integrità elettrochimica del core DPP? + +- Scheletro semiconduttore **DPP-3HT** (polimerizzazione ossidativa, FeCl3) +- Catene laterali di **PCL** per ROP dell'ε-caprolattone (*grafting-from*) dagli OH pendenti +- Il PCL agisce da **spaziatore sterico**: separa i segmenti planari coniugati + + + +--- + +## Il building block: il DPP + +

+ + + +--- + +## Sintesi del monomero DPP **1** → **2** + +![h:230](immagini/fig2-sintesi-dpp1.jpg) +![h:230](immagini/fig3-alchilazione-dpp2.jpg) + +- **1**: ciclizzazione pseudo-Stobbe (2-cianotiofene + diisopropil succinato, teramilato di sodio); λabs 531 nm, λem 542 nm (THF) +- **2**: N-alchilazione con 6-bromo-1-esanolo; NMR 4,1 e 3,6 ppm, IR O–H ~3400 cm-1; λabs 541 nm + + + +--- + +## Copolimeri lineari DPP-3HT (**3a**, **3b**, **3c**) + +![h:190](immagini/fig4-copolimerizzazione.jpg) + +| | % DPP teorica | % DPP reale | Mn (Da) | PD | +|---|---|---|---|---| +| **3a** | 20 | 25,2 | 2149 | 2,571 | +| **3b** | 50 | 32,6 | 1402 | 4,592 | +| **3c** | 80 | 35,3 | 2134 | 1,979 | + +- FeCl3 / nitrometano / CHCl3; DPP incorporato ≤ 35% (reattività e ingombro) +- DSC: Tg ~ −10 °C, nessuna fusione → struttura random +- Allo stato solido: **nessuna emissione apprezzabile** → ACQ + + + +--- + +## Bottle brush: innesto del PCL per ROP + +![h:250](immagini/fig5-rop-bottle-brush.jpg) + +- ROP di ε-caprolattone, Sn(Oct)2, toluene 110 °C, da **3b** e **3c** +- Catene nominali 1500 / 5000 / 10000 Da → 6 campioni (**3.1b–3.3b**, **3.1c–3.3c**) +- Conferma: NMR (~4,0 e 2,3 ppm), IR (scompare O–H, compare C=O estereo ~1720 cm-1) + + + +--- + +## Pesi molecolari e proprietà termiche + +| Polimero | Mn PCL teor. | Mn GPC | PD | Peso mol. teorico | Peso mol. da NMR | +|---|---|---|---|---|---| +| **3.1b** | 1500 | 12188 | 1,521 | 6500 | 8900 | +| **3.2b** | 5000 | 17302 | 1,314 | 18000 | 20500 | +| **3.3b** | 10000 | 21269 | 1,238 | 34500 | 88000 | +| **3.2c** | 5000 | 19119 | 1,275 | 28500 | 35500 | + +Selezione di 4 campioni su 6; tabella completa nel riassunto (Tab. 2). + +- GPC **sottostima** (standard PS lineari; volume idrodinamico compatto) → conferma indiretta della struttura ramificata +- Stima da 1H-NMR più vicina ai teorici; **3.3c** anomalo (da indagare) +- DSC: dominata dal PCL, Tf 55–60 °C, Tc 25–35 °C + + + +--- + +## Risultato 1 — emissione allo stato solido (**3.2b**) + +![h:330](immagini/fig6-uv-em-3.2b.jpg) + +- Soluzione (THF): abs ~550 nm, em ~560–565 nm, banda stretta +- Solido: abs 570–580 nm; **em ~650–660 nm**, allargata, Stokes shift ~80–90 nm → aggregati H/J (Kasha) +- Il bottle brush **mantiene emissione nel rosso**, a differenza dei lineari + + + +--- + +## Risultato 2 — proprietà elettrochimiche (CV) + +
+
+ +![w:440](immagini/fig7-bandgap-vs-dpp.jpg) + +
+
+ +- Trasferimento di carica irreversibile (EC); HOMO/LUMO calibrati sul ferrocene +- Lineari: band gap **0,970 → 1,371 eV** al crescere del % DPP reale (R² = 0,9719) +- Bottle brush: 0,929–1,521 eV; core DPP-3HT resta elettroattivo, PCL = matrice dielettrica + +
+
+ + + +--- + +## Conclusioni e limiti + +**Conclusioni** +- Approccio ortogonale DPP-3HT + PCL → 3 copolimeri e 6 bottle brush +- PCL come spaziatore sterico: **emissione rossa allo stato solido** (3.2b) +- Band gap modulabile con la composizione; integrità elettrochimica preservata + +**Limiti dichiarati** +- DPP ≤ 35%; **3a** non innestato; GPC sottostimata; **3.3c** anomalo + +**Prospettive:** strato elettroluminescente in OLED + + + +--- + +## Grazie per l'attenzione + +Domande? + +Riferimenti principali: Ostroverkhova, *Chem. Rev.* 2016 · Bao et al., *Front. Chem.* 2020 · Wang et al., *J. Polym. Sci. A* 2015 · Labet & Thielemans, *Chem. Soc. Rev.* 2009 · Spano & Silva, *Annu. Rev. Phys. Chem.* 2014 + + diff --git a/wiki/analyses/riassunto-tesi.md b/wiki/analyses/riassunto-tesi.md new file mode 100644 index 0000000..4f86ea3 --- /dev/null +++ b/wiki/analyses/riassunto-tesi.md @@ -0,0 +1,141 @@ +--- +title: Riassunto della tesi (formato 10 pagine) +type: analysis +tags: [riassunto, query, tesi] +created: 2026-10-09 +updated: 2026-10-09 +tesi_loc: "Riassunto r.13-23; Abstract r.25-33; §1 r.66-542; §2 r.545-559; §3 r.562-715; §4 r.717-1277; §5 r.1279-1291" +refs: [45, 48, 1, 42, 52, 56, 5, 7, 58, 59] +figures: ["fig-001", "fig-x-185efd", "fig-x-f6eeb1", "fig-x-cc3f54", "fig-x-136800", "fig-071", "fig-074"] +status: draft +--- + + + +_[PAGINA 1 - COPERTINA: da inserire a parte]_ + +--- + +Il lavoro è stato svolto presso il Dipartimento di Chimica Industriale "Toso Montanari" dell'Università di Bologna, in un gruppo specializzato in materiali polimerici ingegnerizzati, con attenzione alla soft optoelectronics, il ramo interdisciplinare che combina emissione e rilevamento della luce con dispositivi flessibili e adattabili. L'obiettivo generale è sviluppare semiconduttori polimerici emissivi π-coniugati che superino le limitazioni imposte dall'Aggregation-Caused Quenching (ACQ). Il lavoro si è articolato in quattro fasi: sintesi di un monomero a base di dichetopirrolopirrolo (DPP), copolimerizzazione ossidativa con 3-esiltiofene (3HT) per ottenere lo scheletro coniugato, innesto di catene laterali di poli(ε-caprolattone) (PCL) e caratterizzazione dei materiali. La scelta del 3HT deriva dalla collaborazione con il gruppo del Prof. Lanzi, la cui esperienza pregressa ha convalidato la polimerizzazione ossidativa su questa classe di derivati tiofenici. + +L'optoelettronica organica studia dispositivi basati sull'interazione tra radiazione elettromagnetica e semiconduttori: conversione di segnali elettrici in fotoni, come nei diodi organici a emissione di luce (OLED), o viceversa, come nelle celle fotovoltaiche. Rispetto ai semiconduttori inorganici rigidi, come il silicio, i materiali organici con estesi sistemi π-coniugati sono leggeri e meccanicamente flessibili e si depositano da soluzione a basse temperature, con tecniche come lo spin-coating e la stampa su larga scala, con riduzione dei costi e dell'impatto ambientale.1 Per impiegarli in un dispositivo occorre governarne le proprietà ottiche ed elettroniche, cioè ingegnerizzare il band gap. La strategia d'elezione è l'approccio donatore-accettore (D-A), che alterna unità fortemente elettron-deficienti e unità elettron-ricche lungo lo scheletro π-coniugato: l'orbitale HOMO è determinato principalmente dalla porzione donatrice e il LUMO dall'unità accettrice, e il trasferimento di carica intramolecolare che ne deriva riduce il salto energetico e permette di centrare assorbimento ed emissione nel visibile.2 + +I materiali semiconduttori π-coniugati perdono spesso le proprietà ottiche allo stato solido. La natura altamente planare del loro scheletro induce intense interazioni di π-stacking tra le catene adiacenti, che causano la drastica dissipazione non radiativa dell'energia eccitonica e lo smorzamento della fluorescenza: è l'ACQ. Questo limita le applicazioni pratiche dei materiali, perché nello strato emissivo di un OLED è richiesta proprio l'emissione. Per ovviare al problema, la tesi propone una strategia di design macromolecolare basata su architetture a spazzola (bottle brush), il cui scopo è promuovere la separazione fisica dei segmenti planari coniugati, ripristinando le proprietà emissive allo stato solido e preservando integrità elettrochimica e stabilità del sistema. + +Come unità accettrice è stato scelto il DPP, formato da due anelli lattamici a cinque termini condensati, con sostituenti aromatici o eteroaromatici in posizione 3 e 6 *(Figura 1)*. Nato come pigmento rosso industriale, il DPP ha punto di fusione superiore a 350 °C e solubilità molto bassa, dovute a un fitto network di legami a idrogeno ammidici e di π-stacking tra i piani molecolari.3 Il nucleo è planare e fortemente elettron-deficiente, e la rigidità dello scheletro limita il rilassamento vibrazionale e lo Stokes shift. Nel passaggio dalla soluzione al film il DPP mostra un allargamento della banda di assorbimento e un marcato effetto batocromico, con spostamento del picco di circa 30 nm. + +![[immagini/455dd3d0c7bf0fe6ac581ee70795075c998d4dc7156eaa77a4576774f6fd8050.jpg|300]] + +Figura 1. Struttura generica di un dichetopirrolopirrolo. + +L'inserimento di un fluoroforo in un sistema polimerico richiede un accurato design molecolare, perché l'architettura scelta influenza drasticamente le proprietà finali. Nei sistemi host-guest il fluoroforo è disperso fisicamente nella matrice: la preparazione è semplice, ma la scarsa stabilità a lungo termine, con migrazione e aggregazione dell'ospite, porta a perdita di resa quantica. Nei sistemi main-chain il fluoroforo è parte integrante della catena principale, con sintesi più complessa; una strategia riuscita è il grafting-from, in cui un DPP bifunzionalizzato con gruppi ossidrilici inizia la crescita di due catene di PCL, dando PCL-DPP-PCL.4 Nei sistemi side-chain le unità luminescenti sono catene laterali, spesso con uno spaziatore flessibile che limita le interazioni tra cromofori; nei sistemi cross-linked il cromoforo è ancorato da ponti chimici e non aggrega, ma l'eccessiva rigidità rende il materiale fragile, insolubile e difficile da lavorare. La tesi adotta il grafting-from per innestare catene laterali di PCL su uno scheletro semiconduttore DPP-3HT. + +Il monomero è un derivato del DPP definito ortogonale e tetrafunzionale: gli anelli tiofenici forniscono i siti per la polimerizzazione ossidativa dello scheletro, mentre i due gruppi ossidrilici primari, portati dalle catene esiliche sugli azoti lattamici, fungono da iniziatori per la polimerizzazione ad apertura di anello (ROP). Il gruppo aveva già studiato fluorofori DPP con sostituenti diversi in para sull'anello benzonitrilico: quelli elettron-attrattori davano sistemi altamente emissivi, quelli elettron-donatori un isomero strutturale (iso-DPP) a fluorescenza inibita. In questo lavoro i benzeni sono sostituiti da tiofeni e i gruppi ammidici sono N-alchilati, con aumento della solubilità e una procedura semplice e scalabile. Il 3HT è il comonomero donatore: i politiofeni sono tra i più efficienti polimeri semiconduttori organici5 e la catena esilica aumenta la solubilità nei solventi organici. La polimerizzazione ossidativa con FeCl3 è stata preferita ai cross-coupling al palladio perché non richiede pre-funzionalizzazione dei monomeri, opera a temperatura e pressione ambiente ed è scalabile, a fronte di un controllo minore su polidispersità e regioregolarità. La distribuzione statistica dei monomeri aumenta l'entropia conformazionale, limita il packing e rende più accessibili gli ossidrili per la funzionalizzazione. + +Il PCL è stato scelto sulla base di studi precedenti del gruppo, per la bassa temperatura di transizione vetrosa e la buona solubilità nei solventi organici; la ROP dell'ε-caprolattone catalizzata da stagno ottanoato (Sn(Oct)2) è un processo lineare ed efficiente, procede per coordinazione-inserzione con un alcol come coiniziatore e permette di regolare il peso molecolare e di mantenere bassa la dispersità delle catene.6 La lunghezza delle catene si modula con il rapporto molare monomero/ossidrili, con valori nominali di 1500, 5000 e 10000 Da. I copolimeri sono stati alimentati con il 20%, 50% e 80% in moli di DPP; i bottle brush sono stati preparati da **3b** e **3c**, mentre **3a** non è stato usato a causa della scarsa efficienza della sua via sintetica, con basse rese e difficoltà di work-up, e di volumi di solventi e costi di reagenti troppo elevati per isolarne quantità utili. + +Lo scopo del progetto è sintetizzare e caratterizzare copolimeri bottle brush foto-elettro attivi a base di DPP e 3HT con catene laterali di PCL, al fine di superare l'ACQ allo stato solido mantenendo l'integrità elettrochimica del nucleo DPP. Il lavoro comprende due macroaree: la sintesi del monomero ortogonale e l'ottenimento dei materiali, cioè scheletro coniugato e catene innestate. + +Il DPP tiofenico **1** *(Figura 2)* è stato ottenuto per ciclizzazione pseudo-Stobbe tra 2-cianotiofene e diisopropil succinato.7 La base forte è il teramilato di sodio, ottenuto dal sodio in alcol ter-amilico con FeCl3 catalitico: deprotona il succinato in α al carbonile, il carbanione attacca il carbonio nitrilico e il composto imminico tautomerizza a enammina, che attacca il carbonile estereo chiudendo il primo anello a cinque termini; una seconda deprotonazione e l'attacco di una seconda molecola di tiofene portano al secondo anello. Il succinato è stato aggiunto lentamente, perché una concentrazione locale troppo alta in condizioni basiche induce autocondensazione di Claisen, e si è scelto il diisopropil succinato per aumentare l'ingombro intorno al carbonile e ridurre questa reazione.8 Il prodotto, un solido rosso scuro violaceo, è stato purificato sfruttando la netta differenza di solubilità tra reagenti e prodotto, con lavaggi in acqua e metanolo. Il 1H-NMR in DMSO mostra a circa 11 ppm il singoletto allargato dei protoni ammidici; in THF **1** ha massimo di assorbimento a 531 nm, di emissione a 542 nm e Stokes shift di 11 nm. + +![[immagini/185efd9de96189fb7fefd271e19709d672e7eda09572a645d13092c3196248e1.jpg|400]] + +Figura 2. Sintesi del DPP **1** da 2-cianotiofene e diisopropil succinato con teramilato di sodio e FeCl3 catalitico. + +L'N-alchilazione di **1** con 6-bromo-1-esanolo *(Figura 3)* sfrutta la reattività dei gruppi ammidici, deprotonati da ter-butossido di potassio in DMSO, che attaccano per sostituzione nucleofila il carbonio adiacente al bromo, e dà il monomero **2** con due braccia idrossiesiliche. La tesi segnala come reazione collaterale la ciclizzazione del 6-bromo-1-esanolo, favorita da un eccesso di base. Il prodotto è stato lavato con soluzione satura di KCl e purificato per cristallizzazione da etanolo a −20 °C. L'N-alchilazione è confermata nel 1H-NMR dai multipletti alifatici a 4,1 ppm (metileni legati all'azoto lattamico) e a 3,6 ppm (metileni adiacenti all'ossidrile terminale), e nel FT-IR dalla banda larga dell'O-H a circa 3400 cm-1 insieme al C=O lattamico a circa 1650 cm-1. Il massimo di assorbimento passa da 531 nm (**1**) a 541 nm (**2**): lo spostamento batocromico è attribuito all'effetto induttivo elettron-donatore delle catene alifatiche, che arricchiscono di densità elettronica gli azoti, destabilizzano l'HOMO e restringono il band gap ottico. + +![[immagini/f6eeb10de88591bd0358f146073c675489133b4c8bb70f71131b343bb8a25794.jpg|400]] + +Figura 3. N-alchilazione del DPP **1** con 6-bromo-1-esanolo (DMSO, ter-butossido di potassio, 40 °C) a dare il monomero **2** con due catene idrossiesiliche. + +Il monomero **2** è stato copolimerizzato con 3HT per via ossidativa, con FeCl3 in nitrometano e cloroformio anidro *(Figura 4)*. Il FeCl3, in eccesso stechiometrico, estrae per trasferimento mono-elettronico un elettrone dagli anelli tiofenici, generando cationi radicalici delocalizzati che formano i nuovi legami C-C. Il nitrometano rompe i dimeri di FeCl3 e ne modera acidità di Lewis e potere ossidante, prevenendo sovraossidazione e difetti di reticolazione; il cloroformio anidro evita che l'acqua si coordini al FeCl3 e spenga per attacco nucleofilo gli intermedi cationico-radicalici. L'ossidante è stato rimosso con lavaggi con HCl 0,6 M fino a saggio negativo del tiocianato, perché tracce di metalli di transizione abbatterebbero la mobilità dei portatori e spegnerebbero la fluorescenza, e l'omopolimero del 3HT è stato eliminato per precipitazione in metanolo freddo. L'integrazione di DPP si è limitata a un massimo del 35% *(Tabella 1)*: la tesi lo attribuisce alla differenza nei rapporti di reattività dei comonomeri, influenzata dall'ingombro sterico del DPP, mentre il tiofene, più reattivo e meno voluminoso, addiziona preferenzialmente. Le percentuali reali sono state determinate via 1H-NMR. + +![[immagini/cc3f5409e11922aee7835c8eb96ff0f9826afea68af08f1473159279af625b8a.jpg|400]] + +Figura 4. Copolimerizzazione ossidativa del DPP **2** con 3-esiltiofene con FeCl3 a dare i copolimeri **3a**, **3b** e **3c**. + +Tabella 1. Composizione dei copolimeri e pesi molecolari da GPC. + +| Copolimero | % DPP teorica (mol/mol) | % DPP reale (mol/mol) | Mn (Da) | Mw (Da) | PD | +| --- | --- | --- | --- | --- | --- | +| **3a** | 20 | 25,2 | 2149 | 5526 | 2,571 | +| **3b** | 50 | 32,6 | 1402 | 6439 | 4,592 | +| **3c** | 80 | 35,3 | 2134 | 4223 | 1,979 | + +I copolimeri hanno Mn tra 1402 e 2149 Da. Valori di PD intorno a 2 o superiori sono attesi per una polimerizzazione non controllata, con distribuzione più probabile di Flory; **3c** ha la distribuzione più omogenea (PD 1,979), mentre **3b**, con Mn più bassa ma Mw più alta, indica una frazione significativa di oligomeri a catena corta accanto a macromolecole di peso molecolare più elevato. Il FT-IR conferma l'incorporazione del DPP con il C=O lattamico a circa 1650 cm-1, e la DSC mostra per tutti i campioni una transizione vetrosa intorno a −10 °C e nessuna transizione di fusione, a conferma della natura random dei copolimeri, il cui disordine impedisce la cristallizzazione. In soluzione di THF i tre copolimeri hanno profili ottici pressoché identici, simili a quello del monomero: assorbimento tra 540 e 544 nm, emissione intorno a 550 nm e Stokes shift tra 6 e 10 nm. Allo stato solido il comportamento è drasticamente diverso: l'intenso impaccamento delle catene forma aggregati che disattivano i fluorofori per decadimento non radiativo, e i film su vetrino sotto lampada UV non mostrano emissione apprezzabile. È la principale criticità dei sistemi lineari per l'uso in dispositivi optoelettronici e giustifica il passaggio al design bottle brush. + +I sei bottle brush **3.1b**, **3.2b**, **3.3b**, **3.1c**, **3.2c** e **3.3c** sono stati ottenuti per ROP dell'ε-caprolattone dagli ossidrili di **3b** e **3c**, in toluene a 110 °C con Sn(Oct)2 catalitico, con il monomero dosato sul numero di ossidrili per ottenere catene di 1500, 5000 e 10000 Da *(Figura 5)*. L'avvenuto innesto è verificato dal 1H-NMR, con il tripletto del PCL a circa 4,0 ppm (CH2-O adiacente all'ossigeno estereo) e il segnale a 2,3 ppm dei protoni in α al carbonile, e dal FT-IR, in cui la banda dell'O-H a 3600-3200 cm-1 dei macroiniziatori scompare e compare il C=O estereo a circa 1720 cm-1. La GPC fornisce Mn tra 12188 e 21269 Da e indici di dispersità contenuti (1,238-1,521). + +![[immagini/136800375cf0b441570672093e255d90a47c45a009bd254929fb74b1f17b382d.jpg|400]] + +Figura 5. Polimerizzazione ad apertura di anello dell'ε-caprolattone sui gruppi OH dei copolimeri DPP-3HT, a dare i bottle brush con catene di PCL. + +I pesi molecolari da GPC *(Tabella 2)* sono significativamente sottostimati rispetto ai teorici: la GPC separa per volume idrodinamico e restituisce valori relativi agli standard di polistirene lineare, mentre un polimero altamente ramificato assume in soluzione una conformazione compatta, con volume idrodinamico nettamente inferiore. I dati non indicano quindi il peso molecolare assoluto né una bassa resa, ma confermano indirettamente una struttura ramificata altamente impaccata e permettono il confronto tra i polimeri. Il campione **3.3c** si discosta dall'andamento generale; la tesi ipotizza che, essendo il materiale di partenza random, elevate concentrazioni locali di DPP e di ossidrili abbiano ridotto la crescita delle catene laterali per ingombro sterico, e indica che le discrepanze saranno investigate in futuro con ulteriori analisi. Per superare i limiti della GPC è stato calcolato il peso molecolare via 1H-NMR dal grado di polimerizzazione delle catene di PCL, ottenendo una stima descritta come più vicina ai valori teorici. Dal punto di vista termico, la DSC mostra per tutti i bottle brush transizioni dominate dal PCL, con fusione tra 55 e 60 °C e cristallizzazione tra 25 e 35 °C. + +Tabella 2. Pesi molecolari dei bottle brush da GPC e da 1H-NMR, con il valore teorico. + +| Polimero | Mn PCL teorico (Da) | Mn GPC (Da) | PD | Peso molecolare teorico (Da) | Peso molecolare da 1H-NMR (Da) | +| --- | --- | --- | --- | --- | --- | +| **3.1b** | 1500 | 12188 | 1,521 | 6500 | 8900 | +| **3.2b** | 5000 | 17302 | 1,314 | 18000 | 20500 | +| **3.3b** | 10000 | 21269 | 1,238 | 34500 | 88000 | +| **3.1c** | 1500 | 13999 | 1,301 | 10000 | 18200 | +| **3.2c** | 5000 | 19119 | 1,275 | 28500 | 35500 | +| **3.3c** | 10000 | 14445 | 1,351 | 55000 | 41300 | + +La caratterizzazione ottica in soluzione di THF mostra che la funzionalizzazione sterica non perturba l'integrità elettronica del core DPP: i massimi di assorbimento cadono tra 544 e 554 nm, quelli di emissione tra 557 e 564 nm e gli Stokes shift tra 8 e 14 nm. Le piccole fluttuazioni nelle due serie non seguono un andamento lineare con il peso molecolare del PCL e sono trascurabili, quindi l'ingombro sterico non perturba livelli energetici e natura delle transizioni. Il basso Stokes shift conferma la conservazione dell'assetto planare del cromoforo e la minima riorganizzazione tra stato fondamentale ed eccitato, e i domini flessibili di PCL allontanano le catene principali, riducendo l'impaccamento senza distorcere la geometria del backbone. + +La caratterizzazione allo stato solido è stata condotta sul campione **3.2b**, confrontando soluzione e solido *(Figura 6)*. Le misure in soluzione diluita indagano la singola catena isolata e solvatata; allo stato solido la vicinanza tra le macromolecole genera forti interazioni intermolecolari che alterano i livelli energetici e i processi di assorbimento ed emissione. In soluzione il massimo di assorbimento è a circa 550 nm e quello di emissione a circa 560-565 nm, con banda stretta e strutturata. Allo stato solido l'assorbimento mostra un significativo allargamento e un marcato effetto batocromico, con il massimo nell'intervallo 570-580 nm, attribuito alla planarizzazione dello scheletro, che estende la lunghezza di coniugazione effettiva. L'emissione è notevolmente allargata e fortemente spostata verso il rosso, con massimo centrato intorno a 650-660 nm e Stokes shift di circa 80-90 nm, probabilmente legato al maggiore ingombro delle catene, che obbliga gli anelli aromatici a torsioni maggiori, ed evidenza di una forte aggregazione intermolecolare. Secondo la tesi, dopo la fotoeccitazione l'energia migra verso siti a minore energia generati dalla vicinanza dei piani coniugati e il rilassamento radiativo avviene prevalentemente da stati aggregati o specie eccimeriche, nel quadro dell'accoppiamento eccitonico di Kasha tra aggregati H e J.9,10 Nonostante questi riarrangiamenti, l'architettura bottle brush mantiene un'apprezzabile emissione nel rosso, attenuando i percorsi di disattivazione non radiativa tipici dell'ACQ non controllato, in accordo con il ruolo del PCL come spaziatore sterico. + +![[immagini/04f625a8b25744bf2d07d569e55558174b59a5cb564c8bdd0a53c704dfbde545.jpg|420]] + +Figura 6. Confronto tra spettri UV-Vis (in nero) ed emissione (in rosso) del polimero **3.2b** in soluzione (linea continua) e allo stato solido (linea tratteggiata). + +La ciclovoltammetria mostra per i polimeri un trasferimento di carica irreversibile di tipo elettrochimico-chimico, dovuto all'elevata reattività dei cationi e degli anioni radicali all'interfaccia elettrodica. Dagli onset di ossidazione e riduzione, calibrati sul ferrocene (posto a −4,8 eV rispetto al livello del vuoto), sono stati ricavati HOMO, LUMO e band gap elettrochimico *(Tabella 3)*. Nei copolimeri lineari si osserva un allargamento progressivo del band gap all'aumentare della frazione reale di DPP, da 0,970 a 1,371 eV *(Figura 7)*, con correlazione lineare (R² = 0,9719) guidata soprattutto dallo spostamento del potenziale di riduzione verso valori più negativi. La tesi lo interpreta come riduzione della lunghezza di coniugazione effettiva dovuta all'unità DPP, che limita la delocalizzazione π e aumenta la separazione HOMO-LUMO, e vi riconosce la possibilità di un controllo mirato del band gap calibrando il rapporto tra i monomeri. Rispetto al poli-3HT, che si ossida a potenziali accessibili ma non mostra contributi faradici in riduzione, nei copolimeri il DPP, forte porzione elettron-attrattrice in un'architettura D-A, stabilizza il LUMO e rende favorevole l'iniezione di elettroni. + +![[immagini/6c7bd8393eb8c1a329f65b7fc74e5f338a866e514455c0122a43d13ca340ded5.jpg|380]] + +Figura 7. Correlazione tra band gap elettrochimico e frazione reale di DPP nei copolimeri lineari. + +Tabella 3. Livelli HOMO, LUMO e band gap elettrochimici dei copolimeri lineari e dei bottle brush. + +| Polimero | HOMO (eV) | LUMO (eV) | Bandgap (eV) | +| --- | --- | --- | --- | +| **3a** | -5,038 | -4,068 | 0,970 | +| **3b** | -4,854 | -3,538 | 1,316 | +| **3c** | -4,799 | -3,428 | 1,371 | +| **3.1b** | -4,617 | -3,580 | 1,037 | +| **3.2b** | -4,625 | -3,527 | 1,098 | +| **3.3b** | -4,630 | -3,598 | 1,032 | +| **3.1c** | -4,774 | -3,253 | 1,521 | +| **3.2c** | -4,688 | -3,269 | 1,419 | +| **3.3c** | -4,479 | -3,550 | 0,929 | + +I bottle brush mantengono l'elettroattività dello scheletro: i processi redox avvengono a carico del core DPP-3HT, mentre i rami alifatici fungono da matrice dielettrica circostante. Le ingombranti catene laterali modificano HOMO e LUMO rispetto ai lineari, e quindi l'ampiezza del band gap, che nei bottle brush è compresa tra 0,929 e 1,521 eV; la tesi attribuisce l'effetto all'ingombro sterico dei rami di PCL sul grado di coplanarità locale dello scheletro, e quindi sull'estensione effettiva della delocalizzazione. L'ingegnerizzazione con PCL non compromette, secondo la tesi, le spiccate potenzialità optoelettroniche del sistema. + +In conclusione, i risultati confermano secondo la tesi la validità del design proposto: l'approccio ortogonale basato su scheletri semiconduttori DPP-3HT modificati con catene laterali di PCL combina proprietà elettrochimiche modulabili e capacità emissiva allo stato solido. Dal punto di vista sintetico, monomeri ortogonali derivati dal DPP, polimerizzazione ossidativa con FeCl3 e ROP hanno portato a tre copolimeri statistici e a due serie di bottle brush con catene laterali di PCL di lunghezza nominale crescente. Il nucleo DPP conserva in soluzione le proprietà ottiche e, allo stato solido, il bottle brush **3.2b** mantiene un'apprezzabile emissione nel rosso; la composizione monomerica si rivela un parametro di controllo del band gap. I limiti dichiarati nel testo sono l'integrazione di DPP non superiore al 35%, l'esclusione di **3a** dall'innesto, la sottostima dei pesi molecolari da GPC e le discrepanze di **3.3c**, da indagare con ulteriori analisi. La prospettiva indicata dalla tesi è l'impiego di questi materiali in dispositivi optoelettronici, in particolare come strato elettro-luminescente in OLED. + +--- + +Bibliografia + +1. Ostroverkhova, O. Organic Optoelectronic Materials: Mechanisms and Applications. *Chem. Rev.* **2016**, *116*, 13279-13412. https://doi.org/10.1021/acs.chemrev.6b00127 +2. Kroon, R.; Lenes, M.; Hummelen, J. C.; Blom, P. W. M.; de Boer, B. Small Bandgap Polymers for Organic Solar Cells (Polymer Material Development in the Last 5 Years). *Polym. Rev.* **2008**, *48*, 531-582. https://doi.org/10.1080/15583720802231833 +3. Bao, W. W.; Li, R.; Dai, Z. C.; Tang, J. X.; Shi, X.; Geng, J. T.; Deng, Z. F.; Hua, J. Diketopyrrolopyrrole (DPP)-Based Materials and Its Applications: A Review. *Front. Chem.* **2020**, *8*, 679. https://doi.org/10.3389/fchem.2020.00679 +4. Wang, K. Y.; Luo, Y.; Huang, S.; Yang, H.; Liu, B.; Wang, M. Highly Fluorescent Polycaprolactones Decorated with Di(thiophene-2-yl)-diketopyrrolopyrrole: A Covalent Strategy of Tuning Fluorescence Properties in Solid States. *J. Polym. Sci., Part A: Polym. Chem.* **2015**, *53*, 1032-1042. https://doi.org/10.1002/pola.27531 +5. Abdel Aziz, I.; Tullii, G.; Antognazza, M. R.; Criado-Gonzalez, M. Poly(3-hexylthiophene) as a Versatile Semiconducting Polymer for Cutting-Edge Bioelectronics. *Mater. Horiz.* **2025**, *12*, 5570-5593. https://doi.org/10.1039/d5mh00096c +6. Labet, M.; Thielemans, W. Synthesis of Polycaprolactone: A Review. *Chem. Soc. Rev.* **2009**, *38*, 3484. https://doi.org/10.1039/b820162p +7. Iqbal, A. F. M.; Jost, M.; Kirchmayr, R.; Pfenninger, J.; Rochat, A.; Wallquist, O. The Synthesis and Properties of 1,4-Diketo-pyrrolo[3,4-C]pyrroles. *Bull. Soc. Chim. Belg.* **1988**, *97*, 615-644. https://doi.org/10.1002/bscb.19880970804 +8. Grzybowski, M.; Gryko, D. T. Diketopyrrolopyrroles: Synthesis, Reactivity, and Optical Properties. *Adv. Opt. Mater.* **2015**, *3*, 280-320. https://doi.org/10.1002/adom.201400559 +9. Kasha, M.; Rawls, H. R.; El-Bayoumi, M. A. The Exciton Model in Molecular Spectroscopy. *Pure Appl. Chem.* **1965**, *11*, 371-392. https://doi.org/10.1351/pac196511030371 +10. Spano, F. C.; Silva, C. H- and J-Aggregate Behavior in Polymeric Semiconductors. *Annu. Rev. Phys. Chem.* **2014**, *65*, 477-500. https://doi.org/10.1146/annurev-physchem-040513-103639 + +--- + +## Collegamenti +_(sezione solo wiki, non parte del riassunto)_ +- [[overview]] · [[tesi]] · [[bottle-brush]] · [[acq-e-stato-solido]] · [[fluorofori-in-polimeri]] · [[dpp-struttura-e-proprieta]] +- [[dpp-1]] · [[dpp-2]] · [[copolimeri-3a-3b-3c]] · [[bottle-brush-3-x]] · [[cv-risultati]] · [[difetti-noti]] +- Figure usate: 1 = [[fig-001]]; 2-5 = [[fig-x-185efd|schema DPP 1]], [[fig-x-f6eeb1|schema DPP 2]], [[fig-x-cc3f54|schema copolimeri]], [[fig-x-136800|schema bottle brush]]; 6 = [[fig-074]]; 7 = [[fig-071]] +- Allineamento alla tesi (terza stesura): contenuti e interpretazioni sono quelli della tesi; rimosse le inferenze della seconda stesura (stima delle unità ripetitive, confronto gap elettrochimico/ottico, commenti sul numero di campioni, giudizi sulle misure di massa molare). Dove la tesi è incoerente con sé stessa si è scelto il capitolo dei risultati: non sono riportati «da 3,42 eV a oltre 4,30 eV» e «fusione oltre 110 °C» delle Conclusioni ([[difetti-noti]], punti 5-6); la stima NMR è citata come la descrive la tesi, i dati sono in Tabella 2 ([[difetti-noti]], punto 7); l'assorbimento solido di 3.2b è dato come nel testo (570-580 nm), mentre il grafico mostra massimi a circa 550 e 580 nm ([[fig-074]]). La durata del reflusso ROP non è riportata (4 h nello schema, 24 h nel testo). +- Le citazioni 1-10 provengono dalle schede in `raw/fonti/` (non riverificate su fonte originale), numerate per ordine di apparizione.