From 8e38f81d2ec8fe93241f6f98c337021636880e27 Mon Sep 17 00:00:00 2001 From: Davide Grilli Date: Thu, 15 Oct 2026 18:55:28 +0200 Subject: [PATCH] Allinea la presentazione ai valori della tesi aggiornata MIME-Version: 1.0 Content-Type: text/plain; charset=UTF-8 Content-Transfer-Encoding: 8bit Aggiorna % DPP reale, Mn e PDI dei copolimeri, GPC e NMR dei bottle brush, HOMO/LUMO/bandgap (due decimali) e rimuove la Tg dei copolimeri non più presente nella tesi. Modifiche in slides.md, discorso.md e presentazione.pptx. Co-Authored-By: Claude Sonnet 5.5 --- presentazione/discorso.md | 8 ++--- presentazione/presentazione.pptx | Bin 729131 -> 726451 bytes presentazione/slides.md | 54 +++++++++++++++---------------- 3 files changed, 31 insertions(+), 31 deletions(-) diff --git a/presentazione/discorso.md b/presentazione/discorso.md index f0023f1..fc68bbd 100644 --- a/presentazione/discorso.md +++ b/presentazione/discorso.md @@ -89,7 +89,7 @@ Poi l'N-alchilazione con 6-bromo-1-esanolo, in DMSO con ter-butossido di potassi Seconda fase: il monomero **2** viene copolimerizzato con il 3HT per via ossidativa, con cloruro ferrico in nitrometano e cloroformio anidro. Abbiamo scelto il cloruro ferrico perché non richiede la pre-funzionalizzazione dei monomeri e lavora a temperatura e pressione ambiente, a fronte di un minor controllo su polidispersità e regioregolarità. [L'ossidante è stato rimosso con lavaggi acidi, perché tracce di metalli di transizione spegnerebbero la fluorescenza.] -Abbiamo alimentato il 20, il 50 e l'80% in moli di DPP, ma, come mostra la tabella, la percentuale reale, determinata via ¹H-NMR, non supera il 35%: il tiofene, più reattivo e meno voluminoso, addiziona preferenzialmente rispetto al DPP, ingombrante. Le masse molecolari medie in numero sono tra 1402 e 2149 dalton, e i valori di PD intorno a 2 o superiori sono attesi per una polimerizzazione non controllata. +Abbiamo alimentato il 20, il 50 e l'80% in moli di DPP, ma, come mostra la tabella, la percentuale reale, determinata via ¹H-NMR, è del 3, 12 e 35% e non supera il 35%: il tiofene, più reattivo e meno voluminoso, addiziona preferenzialmente rispetto al DPP, ingombrante. Le masse molecolari medie in numero sono intorno ai 2000 dalton, e i valori di PDI, tra 1,9 e 3,6, sono attesi per una polimerizzazione non controllata. **▶ CAMBIA SLIDE** @@ -97,7 +97,7 @@ Abbiamo alimentato il 20, il 50 e l'80% in moli di DPP, ma, come mostra la tabel Come si comportano questi copolimeri? In soluzione di THF i tre hanno profili ottici pressoché identici a quello del monomero, con assorbimento tra 540 e 544 nm ed emissione intorno a 550 nm. -Allo stato solido, però, il comportamento cambia drasticamente. Come si vede dai film sotto lampada UV, non c'è emissione apprezzabile: l'intenso impaccamento delle catene forma aggregati che disattivano i fluorofori. L'ACQ è quindi confermata. [La DSC mostra una transizione vetrosa intorno a −10 °C e nessuna fusione, a conferma della natura random dei copolimeri.] Questo giustifica il passaggio al design bottle brush. +Allo stato solido, però, il comportamento cambia drasticamente. Come si vede dai film sotto lampada UV, non c'è emissione apprezzabile: l'intenso impaccamento delle catene forma aggregati che disattivano i fluorofori. L'ACQ è quindi confermata. [La DSC non mostra alcuna transizione di fusione, a differenza del P3HT, a conferma della natura random dei copolimeri.] Questo giustifica il passaggio al design bottle brush. **▶ CAMBIA SLIDE** @@ -125,7 +125,7 @@ Nonostante questi riarrangiamenti, però, il bottle brush mantiene un'apprezzabi Resta da verificare che il design bottle brush non comprometta le proprietà elettroniche, da cui dipende il comportamento da semiconduttore. Con la ciclovoltammetria, calibrata sul ferrocene, abbiamo ricavato HOMO, LUMO e band gap elettrochimico. -Nei copolimeri lineari il band gap cresce da 0,970 a 1,371 elettronvolt all'aumentare della frazione reale di DPP, da 25,2 a 35,3%, con andamento lineare, come si vede nel grafico. Il DPP riduce la lunghezza di coniugazione effettiva e stabilizza il LUMO, favorendo l'iniezione di elettroni: la composizione monomerica diventa quindi un parametro di controllo del band gap. +Nei copolimeri lineari il band gap cresce da 0,97 a 1,37 elettronvolt all'aumentare della frazione reale di DPP, dal 3 al 35%, con andamento lineare, come si vede nel grafico. Il DPP riduce la lunghezza di coniugazione effettiva e stabilizza il LUMO, favorendo l'iniezione di elettroni: la composizione monomerica diventa quindi un parametro di controllo del band gap. Nei bottle brush il band gap è compreso tra 0,929 e 1,521 elettronvolt. I processi redox avvengono sul core DPP-3HT, mentre i rami alifatici fungono da matrice dielettrica: l'elettroattività dello scheletro è conservata. @@ -154,5 +154,5 @@ Dopo la slide 14 ci sono tre diapositive di scorta; per mostrarle torna indietro | Slide | Quando usarla | |---|---| | 15 · UV-Vis ed emissione di **1** e **2** | domande sull'effetto dell'alchilazione: 531 → 541 nm per l'effetto induttivo donatore delle catene alifatiche, che destabilizza l'HOMO e restringe il band gap ottico | -| 16 · Pesi molecolari dei bottle brush | domande su GPC e NMR: i pesi da ¹H-NMR sono più vicini ai teorici di quelli da GPC | +| 16 · Pesi molecolari dei bottle brush | domande su GPC e NMR: il rapporto GPC/¹H-NMR tende a 1 con pochi siti di innesco (3.2b: 1,0) e scende fino a 0,4-0,5 con più catene laterali (3.2c, 3.3c) | | 17 · HOMO, LUMO e band gap | domande sui valori elettrochimici dei singoli campioni | diff --git a/presentazione/presentazione.pptx b/presentazione/presentazione.pptx 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b/presentazione/slides.md index 5852f72..4e1838f 100644 --- a/presentazione/slides.md +++ b/presentazione/slides.md @@ -146,11 +146,11 @@ Lo scheletro π-coniugato è planare: le catene vicine si impilano (**π-stackin ![w:960](images/fig4-copolimerizzazione.jpg) -| Copolimero | % DPP teorica | % DPP reale | Mn (Da) | PD | +| Copolimero | % DPP teorica | % DPP reale | Mn (Da) | PDI | |---|---|---|---|---| -| **3a** | 20 | 25,2 | 2149 | 2,571 | -| **3b** | 50 | 32,6 | 1402 | 4,592 | -| **3c** | 80 | 35,3 | 2134 | 1,979 | +| **3a** | 20 | 3 | 2200 | 2,5 | +| **3b** | 50 | 12 | 2400 | 3,6 | +| **3c** | 80 | 35 | 2100 | 1,9 | - FeCl3 senza pre-funzionalizzazione; **DPP incorporato al massimo 35%** (reattività dei comonomeri) @@ -162,7 +162,7 @@ Lo scheletro π-coniugato è planare: le catene vicine si impilano (**π-stackin - **In THF**: assorbimento 540-544 nm, emissione ~550 nm, come il monomero - **Film solidi** sotto lampada UV: **nessuna emissione apprezzabile** -- DSC: Tg ~ −10 °C, nessuna fusione → copolimeri random +- DSC: nessuna transizione di fusione (a differenza del P3HT) → copolimeri random → ACQ confermata: serve il design **bottle brush** @@ -172,11 +172,11 @@ Lo scheletro π-coniugato è planare: le catene vicine si impilano (**π-stackin ![w:960](images/fig5-rop-bottle-brush.jpg) -| Polimero | Mn PCL teorico (Da) | Mn GPC (Da) | PD | +| Polimero | Mn PCL teorico (Da) | Mn GPC (Da) | PDI | |---|---|---|---| -| **3.1b** · **3.1c** | 1500 | 12188 · 13999 | 1,521 · 1,301 | -| **3.2b** · **3.2c** | 5000 | 17302 · 19119 | 1,314 · 1,275 | -| **3.3b** · **3.3c** | 10000 | 21269 · 14445 | 1,238 · 1,351 | +| **3.1b** · **3.1c** | 1500 | 12200 · 14000 | 1,5 · 1,3 | +| **3.2b** · **3.2c** | 5000 | 17300 · 19200 | 1,3 · 1,3 | +| **3.3b** · **3.3c** | 10000 | 21300 · 14500 | 1,2 · 1,3 | - Innesto: 1H-NMR PCL a ~4,0 ppm; FT-IR scompare O-H, compare C=O estereo ~1720 cm-1 @@ -200,7 +200,7 @@ Lo scheletro π-coniugato è planare: le catene vicine si impilano (**π-stackin ![bg right:46% fit](images/fig7-bandgap-vs-dpp.jpg) - Ciclovoltammetria: HOMO, LUMO e **band gap elettrochimico** -- Copolimeri lineari: da **0,970 a 1,371 eV** all'aumentare del DPP reale (25,2 → 35,3%), andamento lineare +- Copolimeri lineari: da **0,97 a 1,37 eV** all'aumentare del DPP reale (3 → 35%), andamento lineare - Il DPP stabilizza il LUMO e favorisce l'iniezione di elettroni - **Bottle brush: 0,929-1,521 eV**, elettroattività conservata: redox sul core, PCL come matrice dielettrica @@ -244,16 +244,16 @@ Aurora Luzi # Diapositive di scortaBottle brush: pesi molecolari -| Polimero | Mn PCL teorico (Da) | Mn GPC (Da) | PD | Peso mol. teorico (Da) | Peso mol. da 1H-NMR (Da) | +| Polimero | Mn PCL teorico (Da) | Mn GPC (Da) | PDI | Mn 1H-NMR (Da) | Rapporto GPC/1H-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 | -| **3.1c** | 1500 | 13999 | 1,301 | 10000 | 18200 | -| **3.2c** | 5000 | 19119 | 1,275 | 28500 | 35500 | -| **3.3c** | 10000 | 14445 | 1,351 | 55000 | 41300 | +| **3.1b** | 1500 | 12200 | 1,5 | 8200 | 1,5 | +| **3.2b** | 5000 | 17300 | 1,3 | 18000 | 1,0 | +| **3.3b** | 10000 | 21300 | 1,2 | 28000 | 0,8 | +| **3.1c** | 1500 | 14000 | 1,3 | 18200 | 0,8 | +| **3.2c** | 5000 | 19200 | 1,3 | 35500 | 0,5 | +| **3.3c** | 10000 | 14500 | 1,3 | 41300 | 0,4 | -GPC (standard di polistirene lineare) sottostima: i polimeri ramificati sono compatti in soluzione. +GPC (standard di polistirene lineare): con pochi siti di innesco i valori sono coerenti con l'NMR (rapporto verso 1); con più catene laterali la GPC sottostima, perché i polimeri ramificati sono compatti in soluzione. --- @@ -263,12 +263,12 @@ GPC (standard di polistirene lineare) sottostima: i polimeri ramificati sono com | 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 | +| **3a** | -5,04 | -4,07 | 0,97 | +| **3b** | -4,85 | -3,54 | 1,32 | +| **3c** | -4,80 | -3,43 | 1,37 | +| **3.1b** | -4,62 | -3,58 | 1,04 | +| **3.2b** | -4,63 | -3,53 | 1,10 | +| **3.3b** | -4,63 | -3,60 | 1,03 | +| **3.1c** | -4,77 | -3,25 | 1,52 | +| **3.2c** | -4,69 | -3,27 | 1,42 | +| **3.3c** | -4,48 | -3,55 | 0,93 |