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US2019/0048483A1 Feb.14,2019 copertobeexposedtotheelectrolyteononeside.The sampleholderwithsubstratewasthenloadedinthebench flow cel. [05] Flowwasinitiatedonthebenchcelforboththe aqueousandnon-aqueouselectrolytes,andtheflowratewas controledforeach.ThepH oftheaqueouselectrolytewas monitoredduringthedeposition.TheinitialpHwas6.13, andthefinalpH was5.94.Apotentiostatwasusedto performthedepositionat-3.75voltsfor720secondsusing a chronoamperometry mode. The ionizing electric current spikedat-71.57mA,withafolowoncurentatapproxi mately -41mA.Attheendofdeposition,thesamplewas removed from the sample holder,washed three times with dimethylcarbonate,anddried.Thelithium platingonthe samples demonstrated that pure lithium can be plated directlyfrom alithium chloridebrinefed.Specificaly,the resultantlithium film exhibited ablue color,which isindica tiveofanano-rodmorphologywithinthelithiummetalfilm. Withoutwishingtobeboundby anyparticulartheory,itis believedthattheblueappearancemightbeduetoastruc turalcolorationefect,wherebythefinemicroscopicsurface produces a structural color by interference among light wavesscateredbytwoorsurfacesofthefilm. Example2 10056]. ThecelusedinExample2isshownschematically inFIGS.5-6.75mmx50mmx25micronpiecesofcopper were washed in a concentrated sulfuric acid solution. The samples were then rinsed with deionized water three times, anddriedwithawipe.Thesampleswerethenloadedintoan argonatmosphereglovebox,exchangingtheatmosphereof theantechamberthretimes.Thebench flow celshow in FIGS.5-6wassetupwithan8M aqueouslithium chloride solution circulating through the anode sideofthe cel,and a 1M LiPF6 EC-DMC organic electrolyte circulating throughthecathode(plating)sideofthecel.Asilustrated in FIG . 6, an anionic selective membrane 14 is inserted betweenthecathode18(coperfilm)andtheanode12,and onlylithium flowsthroughthemembrane14.Thesamples werethenloadedintoasampleholderwherethecoperwas masked,allowing 16 square centimeters ofcopper tobe exposedtotheelectrolyteononeside.Thesampleholder with substratewasthenloadedinthebench flow cel. 100571 Flowwasinitiatedonthebenchcelforboththe aqueousandnon-aqueouselectrolytes,andtheflowratewas hydroxideorlithiumhydroxidemonohydrate,theproces controledforeach.ThepH oftheaqueouselectrolytewas monitored during the deposition. The initialpH was 5.94, and the final pH was 5.75. A potentiostat was used to perform thedepositionat-3.75voltsfor2500secondsusing a chronoamperometry mode . The ionizing electric current spikedat-72.9mA,withafolow oncurentatapproxi mately-44mA.Theresultantlithiumfilmexhibitedagrey color,whichisindicativeofadensesphericalmorphology withinthelithiummetalfilm. [058] Itshouldbeunderstodthatvariouschangesand modifications to the presently prefered embodiments describedhereinwillbeapparenttothoseskiledintheart. Such changes and modifications can be made without departing from the spirit and scope of the present subject materandwithoutdiminishingitsintendedadvantages.Itis thereforeintendedthatsuchchangesandmodificationsbe coveredbytheappendedclaims. comprising: providinganaqueouslithium fedsolutionselectedfrom thegroupconsistingofalithiumhydroxidesolution,a lithiumhydroxidemonohydratesolution,andacom binationthereof; providingthelithium fedsolutioninanelectrolysiscel comprising a cathode suitable for electrolysis of lithium,andananode; providinganionizingelectriccurenttotheelectrolysis cel,therebyprovidinglithiummetalatthecathode. 17.Theprocesofclaim 16,whereinthelithiumhydrox idesolutioncontains1.5-18%lithium. 18.Theprocessofclaim 16,whereinthelithiumhydrox ide solution contains 1-18 % lithium . 19.Theprocesofclaim 16,whereinthelithium fed solutioniscontinuouslyprovidedtotheelectrolysiscel,and thelithiummetaliscontinuouslyproducedatthecathode. Theinventionisclaimedasfolows: 1. A process for producing lithium directly from lithium containingbrineorliquor,theprocess comprising: providingalithium fedsolutionselectedfrom thegroup consistingoflithium chloridebrine,lithium sulfate spodumeneliquor,andacombinationthereof; providingthelithiumfedsolutiontoanelectrolysiscel comprising a cathode suitable for electrolysis of lithium,andananode; providinganionizingelectriccurenttotheelectrolysis cel,therebyprovidinglithiummetalatthecathode. 2.Theprocessofclaim 1,whereinthelithiumchloride brinecontains1.5-18%lithium. 3.Theprocesofclaim 1,whereinthelithiumchloride brinecontains4-6% lithium. 4.Theprocesofclaim 3,whereinthelithium chloride brineispreparedbyevaporationinanevaporationpond. 5.Theprocessofclaim 4,whereintheevaporationpond isselectedfromthegroupconsistingofasolarevaporation pond and an electric evaporation pond. 6. The process of claim 4,wherein the lithium chloride brineisreturnedfrom theelectrolysisceltotheevaporation pond. 7.Theprocessofclaim 1,whereinthelithium sulfate spodumene liquor contains 1-18 % lithium . 8.Theprocessofclaim 1,wherein thelithium sulfate spodumeneliquorcontains1.5-18% lithium. 9.Theprocesofclaim 1,whereinthelithium sulfate spodumeneliquorcontains16-18%lithium. 10.Theprocesofclaim 1,whereinthelithiumsulfate spodumeneliquorisprovidedfrom areservoir,andthe lithium sulfate spodumene liquor is returned from the elec trolysisceltothereservoir. 1.Theprocesofclaim 1,whereinthelithium fed solutionispreparedwithoutremovingboronormagnesium. 12.Theprocessofclaim 1,whereinthelithiumfed solutioniscontinuouslyprovidedtotheelectrolysiscel,and thelithiummetaliscontinuouslyproducedatthecathode. 13.Theprocesofclaim1,whereinthetemperatureinthe electrolysiscelforprovidinglithiummetalis15to40°C. 14.Theprocessofclaim 1,whereinthetemperatureinthe electrolysiscelforprovidinglithiummetalisaproximately 23° C. 15.Theprocesofclaim 1,wherein thelithium fed solutionhasapH of3-9. 16 . A process for producing lithium directly from lithiumPDF Image | Patent PRODUCING LITHIUM DIRECTLY FROM LITHIUM FEED SOURCES
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