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Katóda LiFePO4

LiFePO4, LiFeYPO4, atd., zkušenosti, rady, tipy ...

Katóda LiFePO4

Příspěvekod rottenkiwi » stř říj 07, 2020 5:35 pm

Lítium-iónové batérie

Prvé lítiové batérie na báze Li/Li+/LixTiS2 boli rýchlo stiahnuté z trhu
okolo r. 1970, kvôli formovaniu dendritov Li, ktoré viedlo k skratu batérie.

V r. 1991 uviedla firma Sony na trh batérie na báze LixC6/Li+/Li1-xCoO2.
Lítiová metalická anóda bola nahradená grafitovou anódou, ktorá má schopnosť
reverzibilne interkalovať Li+ a má výrazne nižší potenciál voči lítiu.
Aby sa zlepšili parametre batérií, bolo nutné zlepšiť materiály katódy.
Katódové materiály sú typicky oxidy a fosfáty rôznych kovov.
Štrukturálna stabilita katódy je dôležitá hlavne počas nabíjania,
keď sa skoro všetko lítium presúva do anódy.

Pri výrobe lítium-iónových batérií, je batéria konštruovaná vo vybitom stave,
ergo ióny lítia sú v katóde a grafitová anóda neobsahuje ióny lítia.
Na rozdiel od iných technológií, kde elektródy reagujú s elektrolytom,
u lítium-iónových batérií, je to presun Li+ a elektrónov.

Interkalačný proces prepieha nasledovne:

Typ: LixC6/Li+/Li1-xMaXb

C6 + xLi+ + xe- <-> LixC6

katóda: Li1MaXb <-> Li1-xMaXb + xLi+ + xe-

Efektivita interkalačného procesu je determinovaná vlastnosťami iónového
a elektrónového transportu materiálov oboch elektród, množstvom miest
dostupných pri Li+ a hustotou dostupných elektronických stavov.
Prúdová hustota tiež závisí na iónovo-elektrónových transportných vlastnostiach
materiálov oboch elektród. V dôsledku toho aj napatie, kapacita, energetická
hustota, prúdová hustota sú definované vlastnosťami materiálov elektród.
Počet nabíjacích cyklov a kalendárna životnosť sú podmienené procesmi,
ktoré prebiehajú na rozhraní elektródy a elektrolytu. Bezpečnosť článkov
závisí na teplotnej a chemickej stabilite materiálov elektród a elektrolytu.
Dotupnosť Li+ na rozhraní povrchu elektród a elektrolytu určuje maximálny
vybíjací prúd.

LiFePO4

Hlavnými interkalačnými oxidmi sú LiCoO2, LiNiO2, LiMnO2 a ich kompozity.
LiCoO2 je drahý a toxický. Čistý LiNiO2 podlieha exotermickej oxidácii elektrolytu
s kolabujúcou delítiovanou štruktúrou LixNiO2. Cyklická a termálna stabilita
LiMn2O4 je tiež limitujúcim faktorom. Potrebujeme katódový materiál, ktorý
je lacnejší, bezpečnejší a výkonnejší ako LiCoO2.

Katódové materiály: / tab 1 /

life_tab_1.png



/ tab 2 /

life_tab_2.png



Dôležitým katódovým materiálom je LiMPO4 / M = Fe, Co, Ni, Mn /. Má olivínovú štruktúru.
Katódy LiMnPO4, LiCoPO4 a LiNiPO4 majú vyššie OCV / 4.1 až 4.8 V / v porovnaní
s LiFePO4 / 3.5 V /. LiFePO4 má reakčný potenciál okolo 3.5 V, má dobrú cyklickú
a termálnu stabilitu, tiež je environmentálne nezávadný.


Štruktúra a charakteristika LiFePO4

LiFePO4 ma dostatočnú reverzibilnú kapacitu okolo 3.5 V ako aj významnú
cyklickú životnsoť, pretože zmeny objemu sú okolo 6.8 %.
V štruktúre LiFePO4, Li má náboj +1, Fe +2 a PO4 -3. Po odstránení Li+,
sa materiál konvertuje na FePO4. Fe a 6 atómov kyslíka tvoria oktohedrálnu štruktúru.
Fe je uprostred. 3D štruktúra je tvorené zdieľanými atómami O. Li+ ležia v oktahedrálnych
kanáloch v cik-cak štruktúre. b = 6.008 Å, a = 10.334 Å, and c = 4.693 Å. Objem: 291.4 Å3.
Hlavnými nevýhodami LiFePO4 je nízka elektrónová vodivosť a nízka Li+ difúzia.


Syntéza LiFePO4


Práškový LiFePO4 je pripravovaný pevnými metódami ako aj metódami založenými na roztokoch.
Solid-state syntéza, mechanochemická aktivácia, uhlíkovotermálna redukcia a mikrovlný ohrev
sú najčastejšími medódami pre prípavu LiFePO4.

Solid-state syntéza prebieha pri vysokých teplotách a tlakoch. Nevýhodou je však neuniformita
častíc v nekryštalickej forme ako aj časová náročnosť procesu. Väčšie častice vedú k horším
elektrochemickým vlastnostiam. LiF, Li2CO3, LiOH.2H2O a CH3COOLi sú zdrojmi lítia,
FeC2O4.2H2O, Fe/CH3COO2/2 a FePO4/H2O/2 sú zdrojmi Fe a NH4H2PO4 a /NH4/2HPO4 sú zdrojmi P.
Produkcia LiFePO4 prášku začína mletím prekurzorov. Potom nastáva peletizácia a kalcinácia.
Prekalcinácia začína pri 250 - 300 *C a druhý krok finálnej kalcinácie je pri 400 - 800 *C.
Teplota vypaľovania má významný vplyv na štruktúru, veľkosť častíc ako aj vybíjaciu kapacitu
LiFePO4. Sintrovanie prebieha vačšinou pri 650 - 700 *C.


Mechanochemická aktivácia sa používa na zvýšenie chemickej reaktivity. Nevýhodami je viac nečistôt
ako aj nárast teploty. Nárast teploty vedie k dekompozícii prekurzorov. Mixtúry sú neskôr
peletizované a kalcinované pri 600 - 900 *C, v atmosfére 95 % Ar a 5 % H2 a N2.

Pri týchto procesoch sa stáva, že FeII začína tvoriť FeIII. Uhlíkovo-termálna redukcia dovoľuje
použiť lacnejšie FeIII zlúčeniny, oproti nestabilným FeII zlúč. Čierny uhlík, grafit a pyrolizované
organické zlúč., sú používané ako redukčný agent. Rýchlosť reakcie závisí od veľkosti častíc,
redukčných prostriedkov, premiešania, koncentrácie plynov atď. Vlastnosti výsledného prášku
závisia na teplote, tlaku, prekurzoroch a redukčných agentoch. Procedúra zahŕňa premiešanie
stechiometrického množstva prekurzorov a redukčných agentov a kalcinácie pri 550 - 850 *C,
v inertnej atmosfére.

Mikrovlnové ohrievanie je ďalšou metódou produkujúcou LiFePO4. Toto ohrievanie prebieha
na molekulárnej úrovni, čo umožňuje volumetrické ohrievanie materiálu absorbovaním energie
mikrovĺn. Stupeň ohrevu je kontrolovaný výkonom žiariča a disipáciou tepla povrchom častíc.
Výhodami metódy sú krátky čas ohrevu, malé množstvo energie a nízka cena. Nie je potrebný
redukujúci plyn. Takto pripravený prášok má častice s malými rozmermi, uniformnú veľkosť
častíc, plynulejšiu povrchovú morfológiu častíc a tým vačšiu vybíjaciu kapacitu.
Ako mikrovlnový absorbér sa používa uhlík. Príprava prebieha vo vzduchu. Dlhšie ohrievanie
spôsobuje vačšie častice, nižší Li difúzny koeficient, ergo významnú stratu kapacity.
Dlho trvajúce ohrievanie tiež spôsobuje vyšší obsah Fe2P. Ak dosiahne Fe2P kritické množstvo,
časť LiFePO4 sa zmení na izolujúci Li4P2O7. Ak je ohrievanie veľmi krátke, tvoria sa kontaminanty,
ktoré zhoršujú vybíjaciu kapacitu.

Pre dosiahnutie lepších výsledkov sa používa aj mokré metódy. Medzi ne patrí hydrotermálna syntéza,
sol-gel syntéza, sprejová pyrolýza, koprecipitácia a mikroemulzia.

Hydrotermálna syntéza je chemický proces, ktorý prebieha pri zahriatí roztoku nad bod varu vody.
Počas procesu zohriata voda akceleruje difúziu častíc a rast kryštálov je rýchly.
Reaktor / autokláv / je environmentálne neškodný. Po zmixovaní prekurzorov v stechiometrickom
pomere sa teplota zvýši na 120 - 220 *C. Ak je nutná karbonizácia, zaradí sa krok kalcinácie
pri 400 - 750 *C. Ako zdroj uhlíka sa používa cukor, askorbová kyselina, MWCNT a organický
surfaktant acetyl trimetyl amónium bromid / CTAB /. Reakčný čas, stupeň ionizácie, veľkosť
častíc a kryštalická štruktúra LiFePO4 sú závislé na teplote.

Sol-gel syntéza je nízkoteplotný mokrý proces, ktorý sa používa na prípravu oxidov kovov.
Vytvorí sa koloidná suspenzia a tá sa zmení na gel. Gel sa vysuší na xerogel. Teplota,
čas, pH, prekurzory, rozpúšťadlá, ich koncentrácia a viskozita determinujú veľkosť častíc,
ich tvar, porozitu atď. Sol-gel syntéza je nízkonákladová a vyznačuje sa vysokou čistotou
častíc, ich uniformnou štruktrou a malými rozmermi častíc. Pomalé zahrievanie produkuje
drsnejšie a menej porézne štruktúry. Rýchle zahrievanie produkuje poréznejšie štruktúry.

Sprejová pyrolýza je ultrasonická metóda, ktorá je veľmi efektívna. Veĺkosť častíc je kontrolovateĹná
v submikrometrovom rozsahu. Kvapky slúžia ako nukleačné centrá a z nich vznikajú kryštalické
a husté partikuly. Takto produkovaný prášok má častice menšie ako 1 um, s veľkým povrchom
a vysokou čistotou. Roztok prekurzorov sa pumpuje do pyrolyzačnej pece okolo 400 - 600 *C.
Zberaný prášok sa potom zahrieva na 700 - 800 *C. Môže sa pridať zdroj uhlíka, aby mali
LiFePo4/C častice väčší povrch.


Koprecipitácia je ďalšou metódou, ktorá vedie k časticiam vysokej čistoty a malých rozmerov.
Koprecipitácia mixtúr prekurzorov je kontrolovaná pH. Sušené prekurzory vytvoria amorfný LiFePO4.
Kryštalický prášok je získaný ďalšou kalcináciou pri 500 - 800 *C pri N2 atmosfére. Častice
majú rozmery od 100 nm do niekoľkých um. Vlastnosti LiFePO4 môžu byť ďalej zlepšené intrudovaním
zdroja C alebo zdroja kovu do koprecipitačného procesu.

LiFePO4 prášok može byť tiež pripravený vysušením mikroemulzie. Tú tvorí voda, olej a emulzifikačný
agent. Začína sa prípravou vodných roztokov prekurzorov v stechiometrickom pomere. Potom je vodná
a hydrokarbónová fáza spolu zmixovaná. Získaná mikroemulzia je sušená pri 300 - 400 *C. V ďalšom
kroku je vysušená emulzia calcinovaná pri 650 - 850 *C pod argónovou atmosférou.


Zlepšenie vlastností LiFePO4

Nízka elektrónová vodivosť LiFePO4 a nízky difúzny koeicient Li+ sú hlavnými nedostatkami,
ktoré limitujú uplatnenie LiFePO4. LiFePO4 má vodivosť 10-9 až 10-10 S.cm-1 a difúzny
koeficient 10-12 až 10-14 cm2.s-1, v závisloti na koncentrácii Li+.
Preskúmanie metód na elimináciu týchto nevýhod je veľmi dôležité.

/ tab 3 /

life_tab_3.png



Existuje niekoľko prístupov:

1, zlepšiť elektrónovú vodivosť potiahnutím častíc uhlíkom alebo využiť disperziu
Cu a Ag do roztokov počas syntézy, prípadne použiť nanočastice Al2O3 a MgO
2, kontrolovať veľkosť častíc, aby sa dosiahli homogénne polykryštalické nano partikuly
LiFePO4 optimalizíciou podmienok syntézy
3, selektívne dopovanie supervalentnými katiónmi voči Li


Potiahnutie častíc uhlíkom viedlo k teoretickým kapacitám 170 mAh g-1 pri izbovej teplote.
Jednou z jeho funkcií je zlepšiť elektrónovú vodivosť. Ďalšou funkciou je zabránenie agregácie
nanočastíc a poskytnutie cesty pre Li+. Je potvrdené, že vodivý uhlík musí byť homogénne
rozptýlený po katóde, aby zlepšil elektrónovú vodivosť. Tiež sa zistilo, že difúzny koef.
je ovplyvnený uhlíkom. Pri syntéze LiFePO4 je čierny uhlík pridaný ako prekurzor.
Potianutie uhlíkom však znižuje volumetrickú energetickú hustotu, preto obsah uhlíka
musí byť optimalizovaný. Preto je kľúčovým nájsť vhodný zdroj uhlíka a vytvoriť lacné
a efektívne fabrikačné procesy.


Pozorovaný úbytok kapacity pri cyklovaní je dôsledkom veľkých častíc, ktoré majú malý povrch
a tým sa znižuje difúzia na LiFePO4/FePO4 interfejse. Ergo, aby sa dosiahli lepšie vlastnosti
katódy, je nutné minimalizovať veľkosť partikúl a dosiahnuť vačší špecifický povrch.
Nanoštruktrovaný materiál je benefitom, najmä ak potrebujeme dosiahnuť prúdy 5C.
Nanočastice tiež zlepšujú kinetiku Li+, pretože redukujú difúznu vzdialenosť.


Vlastnosti katódy možu byť zlepšené dopovaním iónmi Mg2+, Al3+, Ti4+, Zr4+ a Nb5+, čím sa
dosahuje lepšia elektrónová vodivosť. Tiež je známe, že parciálna substitúcia Fe2+ iónmi Mn2+,
vedie k lepšej špecifickej kapacite a menšiemu ubytku kapacity. Nb zlepšuje elektrónovú vodivosť
a tiež zlepšuje reverzibilnú kapacitu pri vysokých prúdoch. Substitúcia katiónmi tiež redukuje
polarizáciu. Vysoké hodnoty vodivosti dopovaného fosfo-olivínu sú zapríčinené formáciou
fosfidov na povrchu zŕn, čoho príčinou je parciálna redukcia LiePO4 na Fe2P.
Značne zlepšené vlastnosti majú napr. kompozitné katódy Li1-5xNbxFePO4/C.

Dopovanie LiFePO4 ytriom vedie k pravidelnejšej morfológii.

Povrch LiFePO4/C potiahnutý nanočasticami Sn je odolný voči rozkladu Fe v elektrolyte
založenom na LiPF6.

Odkazy:

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Re: Katóda LiFePO4

Příspěvekod KUTIL » stř říj 07, 2020 8:39 pm

Dúfam že si tie odkazy do bodky preštudoval!
KUTIL
 
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