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Masiraidhi anoratidza zvinyorwa zvitatu pane siraidhi.Shandisa mabhatani ekumashure neanotevera kufamba nemumasiraidhi, kana mabhatani ekudzora masiraidhi ari kumagumo kuti ufambe nemumasiraidhi ega ega.
yakashuma pamusoro pe electrochemical stratification ye-non-conducting boron mu-tete-layer borons.Iyi yakasarudzika mhedzisiro inowanikwa nekubatanidza yakawanda boron mune mesh yesimbi inoita kuti magetsi afambe uye anovhura nzvimbo yekugadzira boron neiyi nzira inoshanda.Maedzo akaitwa mumhando dzakasiyana-siyana dze electrolyte zvinopa chishandiso chine simba chekuwana mabore flakes ezvikamu zvakasiyana neukobvu hwe ~ 3–6 nm.Iyo nzira yekubvisa boron ye electrochemical inoratidzwawo uye inokurukurwa.Nekudaro, iyo nzira yakatsanangurwa inogona kushanda sechishandiso chitsva cheyakakura-yakakura kugadzirwa kwematete-layer burs uye nekukasira kusimudzira tsvagiridzo ine chekuita nemabhura uye zvavanogona kushandisa.
Zviviri-dimensional (2D) zvinhu zvakawana kufarira kwakawanda mumakore achangopfuura nekuda kwezvakasiyana zvimiro zvakaita semagetsi conductivity kana nzvimbo dzine mukurumbira dzinoshanda.Kuvandudzwa kwezvinhu zvegraphene kwakwevera kutarisa kune zvimwe zve2D, saka zvitsva zve2D zviri kutsvagirwa zvakanyanya.Pamusoro peiyo inozivikanwa graphene, shanduko yesimbi dichalcogenides (TMD) yakadai seWS21, MoS22, MoSe3, uye WSe4 zvakare yakadzidziswa zvakanyanya munguva pfupi yapfuura.Zvisinei nezvataurwa pamusoro apa, hexagonal boron nitride (hBN), black phosphorus uye ichangobva kubudirira kugadzirwa boronene.Pakati pavo, boron yakakwezva kutarisisa zvakanyanya seimwe yediki diki-dimensional masisitimu.Yakaturikidzana senge graphene asi inoratidza zvinonakidza zvimiro nekuda kweiyo anisotropy, polymorphism uye chimiro chekristaro.Boron yakawanda inoratidzika seyakakosha kuvaka muB12 icosahedron, asi mhando dzakasiyana dzemakristasi eboron anoumbwa kuburikidza nenzira dzakasiyana dzekujoinha uye dzekubatanidza muB12.Nekuda kweizvozvo, mabhuroki eboron kazhinji haana kuturika senge graphene kana graphite, izvo zvinonetsa maitiro ekutora boron.Pamusoro pezvo, akawanda mapolymorphic mafomu eborophene (eg, α, β, α1, pmmm) anoita kuti zvinyanye kuomarara5.Matanho akasiyana-siyana anowanikwa panguva yekubatanidza anokanganisa zvakananga maitiro eharrows.Naizvozvo, kuvandudzwa kwemaitiro ekugadzira anoita kuti zvikwanise kuwana phase-specific borocenes ane hombe lateral dimensions uye kukora kudiki kwemaflakes parizvino kunoda kudzidza kwakadzama.
Nzira dzakawanda dzekugadzira zvinhu zve 2D dzinobva pane sonochemical process umo zvinhu zvakawanda zvinoiswa mu solvent, kazhinji organic solvent, uye sonicated kwemaawa akawanda.Ranjan et al.6 yakabudirira kubvisa boron yakawanda muborophene uchishandisa nzira yatsanangurwa pamusoro apa.Vakadzidza huwandu hwezvinonyungudutsa zvehupenyu (methanol, ethanol, isopropanol, acetone, DMF, DMSO) uye vakaratidza kuti sonication exfoliation inzira iri nyore yekuwana mabhoron flakes makuru uye akaonda.Pamusoro pezvo, vakaratidza kuti nzira yakagadziridzwa yeHummers inogona zvakare kushandiswa kuburitsa boron.Liquid stratification yakaratidzwa nevamwe: Lin et al.7 yakashandisa crystalline boron sesosi yekugadzira yakaderera-layer β12-borene mapepa uye yakawedzera kuishandisa mu borene-based lithium-sulfur mabhatiri, uye Li et al.8 yakaratidza pasi-layer boronene mapepa..Inogona kuwanikwa ne sonochemical synthesis uye inoshandiswa se supercapacitor electrode.Nekudaro, atomic layer deposition (ALD) zvakare imwe yepasi-kumusoro synthesis nzira dzeboron.Mannix et al.9 vakaisa maatomu eboron pane atomu yakachena sirivha inotsigira.Iyi nzira inoita kuti zvikwanise kuwana mashizha e-ultra-pure boronene, zvisinei kuti laboratory-scale kugadzirwa kweboronene inogumira zvakanyanya pamusana pemamiriro ezvinhu akaoma (ultra-high vacuum).Nokudaro, zvakakosha kukudziridza mazano matsva ekugadzirwa kweboronene, kutsanangura nzira yekukura / stratification, uyezve kuita tsvakurudzo yakarurama yezvinyorwa zvayo, zvakadai sepolymorphism, magetsi uye kupisa kupisa.H. Liu nevamwe.10 yakakurukura uye yakatsanangura nzira yekukura kweboron paCu(111) substrates.Zvakazoitika kuti maatomu eboron anowanzo kuumba 2D dense masumbu akavakirwa pamativi matatu, uye simba rekugadzira rinodzikira zvishoma nezvishoma nekukura kwemasumbu, zvichiratidza kuti masumbu e2D boron pamhangura substrates anogona kukura nekusingaperi.Ongororo yakadzama yemapepa maviri-dimensional boron inoratidzwa naD. Li et al.11, uko kwakasiyana ma substrates anotsanangurwa uye zvinogona kushandiswa zvinokurukurwa.Zvinonyatso kuratidzwa kuti pane kumwe kusawirirana pakati pemasvomhu ekuverenga nemhedzisiro yekuedza.Naizvozvo, kuverenga kwe theoretical kunodiwa kuti unzwisise zvizere zvivakwa uye maitiro ekukura kweboron.Imwe nzira yekuzadzisa chinangwa ichi ndeyekushandisa yakapfava tepi yekunamira kubvisa boron, asi ichi chichiri chidiki kuti uongorore zvakakosha zvivakwa uye shandura iyo inoshanda application12.
Nzira inovimbisa yeinjiniya kupemburudza kwe2D zvinhu kubva kune zvakawanda zvinhu ndeye electrochemical peeling.Pano imwe ye electrode ine zvinhu zvakawanda.Kazhinji, makomisheni ayo anowanzo exfoliated ne electrochemical nzira anoitisa zvakanyanya.Anowanikwa setsvimbo dzakamanikidzwa kana mapiritsi.Graphite inogona kubudirira exfoliated nenzira iyi nekuda kwekukwira kwayo kwemagetsi conductivity.Achi nechikwata chake14 vakabudirira kuburitsa graphite nekushandura magraphite rods kuita yakatsikirirwa graphite pamberi pe membrane inoshandiswa kudzivirira kuparara kwezvinhu zvakawanda.Mamwe mazambiringa akakura anonyatso kupepetwa nenzira yakafanana, semuenzaniso, kushandisa Janus15 electrochemical delamination.Saizvozvovo, akaturikidzana phosphorus nhema inoiswa electrochemically stratified, ine acidic electrolyte ions inopararira munzvimbo iri pakati pematanho nekuda kwemagetsi akaiswa.Zvinosuruvarisa, nzira imwechete haigoni kushandiswa chete kune stratification ye boron mu borophene nekuda kwekuderera kwemagetsi ekugadzirisa kwezvinhu zvakawanda.Asi chii chinoitika kana yakasununguka boron poda inosanganisirwa musimbi mesh (nickel-nickel kana mhangura-mhangura) kuti ishandiswe se electrode?Zvinokwanisika here kufambisa conductivity ye boron, iyo inogona kuwedzera electrochemically kupatsanurwa seye layered system yemagetsi conductors?Ndeipi chikamu cheyakagadzirwa yakaderera-layer boronene?
Muchidzidzo ichi, tinopindura mibvunzo iyi uye tinoratidza kuti iri nyore zano rinopa nzira nyowani yekugadzira mabura matete, sezvakaratidzwa mumufananidzo 1.
Lithium chloride (LiCl, 99.0%, CAS: 7447-41-8) uye boron powder (B, CAS: 7440-42-8) yakatengwa kubva kuSigma Aldrich (USA).Sodium sulfate (Na2SO4, ≥ 99.0%, CAS: 7757-82-6) inopiwa kubva kuChempur (Poland).Dimethyl sulfoxide (DMSO, CAS: 67-68-5) kubva kuKarpinex (Poland) yakashandiswa.
Atomic force microscopy (AFM MultiMode 8 (Bruker)) inopa ruzivo pane ukobvu uye saizi yelatisi yezvinhu zvakaiswa.High resolution transmission electron microscopy (HR-TEM) yakaitwa pachishandiswa maikorosikopu yeFEI Tecnai F20 pamhepo inomhanya ye200 kV.Atomic absorption spectroscopy (AAS) ongororo yakaitwa pachishandiswa Hitachi Zeeman polarized atomic absorption spectrophotometer uye murazvo nebulizer kuona kutama kweioni dzesimbi kupinda mumhinduro panguva ye electrochemical exfoliation.Kugona kwezeta kweboron yakawanda kwakayerwa ndokuitwa paZeta Sizer (ZS Nano ZEN 3600, Malvern) kuona kugona kwepamusoro kweboron yakawanda.Kuumbwa kwekemikari uye hukama hweatomu muzana hwepamusoro pemasampuli zvakadzidzwa neX-ray photoelectron spectroscopy (XPS).Zviyero zvacho zvakaitwa pachishandiswa Mg Ka radiation (hν = 1253.6 eV) muPREVAC system (Poland) yakashongedzerwa neScienta SES 2002 electron energy analyzer (Sweden) inoshanda pamhepo inogara ichifambiswa (Ep = 50 eV).Imba yekuongorora inobviswa kune kumanikidzwa pazasi 5 × 10-9 mbar.
Kazhinji, 0.1 g yemahara-inoyerera boron poda inotanga kudzvanywa musimbi mesh disk (nickel kana mhangura) uchishandisa hydraulic press.Iyo dhisiki ine dhayamita ye15 mm.Madhisiki akagadzirirwa anoshandiswa se electrode.Mhando mbiri dze electrolytes dzakashandiswa: (i) 1 M LiCl muDMSO uye (ii) 1 M Na2SO4 mumvura yakasvibiswa.Waya yeplatinamu yakashandiswa seyetsigiro yemagetsi.Iyo schematic diagraph yeworkstation inoratidzwa muMufananidzo 1. Mu electrochemical stripping, yakapihwa ikozvino (1 A, 0.5 A, kana 0.1 A) inoshandiswa pakati pecathode uye anode.Nguva yechiedzwa chega chega iawa imwe.Mushure maizvozvi, iyo supernatant yakaunganidzwa, centrifuged pa 5000 rpm uye yakashambidzwa kakawanda (3-5 nguva) nemvura yakasvibiswa.
Yakasiyana-siyana paramita, senge nguva uye chinhambwe pakati pemagetsi, zvinokanganisa morphology yechigadzirwa chekupedzisira chekuparadzaniswa kwe electrochemical.Pano tinoongorora maitiro e electrolyte, kushandiswa ikozvino (1 A, 0.5 A uye 0.1 A; voltage 30 V) uye rudzi rwesimbi grid (Ni zvichienderana nehukuru hwekuita).Electrolyte mbiri dzakasiyana dzakaedzwa: (i) 1 M lithium chloride (LiCl) mu dimethyl sulfoxide (DMSO) uye (ii) 1 M sodium sulfate (Na2SO4) mumvura deionized (DI).Mukutanga, lithium cations (Li +) ichapindirana mu boron, iyo inobatanidzwa nechaji yakaipa mukuita.Muchiitiko chekupedzisira, iyo sulfate anion (SO42-) ichapindirana kuita boron yakanaka.
Pakutanga, chiito che electrolytes pamusoro apa chakaratidzwa pane ikozvino ye 1 A. Iyo nzira yakatora 1 awa nemhando mbiri dzesimbi grids (Ni uye Cu), maererano.Mufananidzo 2 unoratidza atomic force microscopy (AFM) mufananidzo wezvakabuda, uye hurefu hunoenderana hunoratidzwa muFigure S1.Mukuwedzera, kureba uye zviyero zvezvipembenene zvakaitwa mukuedza kwega kwega zvinoratidzwa muTebhu 1. Sezviri pachena, kana uchishandisa Na2SO4 se electrolyte, hupamhi hwehuputi hushoma zvikuru kana uchishandisa girafu yemhangura.Kuenzaniswa nemaflakes akasvunurwa pamberi pemutakuri we nickel, ukobvu hunoderera kanenge ka5.Sezvineiwo, kugoverwa kwehukuru hwezvikero kwakafanana.Zvisinei, LiCl/DMSO yaibudirira mukuita exfoliation ichishandisa mameshes ese esimbi, zvichiita kuti 5-15 zvidimbu zveborocene, zvakafanana nemamwe maexfoliating fluids, zvichiita kuti pave nezvikamu zvakawanda zveborocene7,8.Naizvozvo, zvimwe zvidzidzo zvicharatidza chimiro chakadzama chemasampuli akaiswa mune iyi electrolyte.
AFM mifananidzo yeborocene sheets mushure me electrochemical delamination into A Cu_Li+_1 A, B Cu_SO42−_1 A, C Ni_Li+_1 A, uye D Ni_SO42−_1 A.
Kuongorora kwakaitwa pachishandiswa transmission electron microscopy (TEM).Sezvinoratidzwa muMufananidzo 3, chimiro chakawanda cheboron chine crystalline, sezvinoratidzwa nemifananidzo yeTEM yeboron uye boron yakaturikidzana, pamwe chete neFast Fourier Transform (FFT) inoenderana neSelected Area Electron Diffraction (SAED) inotevera.Misiyano mikuru pakati pemasamples mushure meiyo delamination process inoonekwa zviri nyore mumifananidzo yeTEM, uko d-spacings yakapinza uye madaro ari mapfupi kwazvo (0.35-0.9 nm; Tafura S2).Nepo masamples akagadzirwa pamambure emhangura aienderana ne-β-rhombohedral chimiro cheboron8, samples dzakagadzirwa pachishandiswa nickel.meshinofananidzwa nefungidziro yekufungidzira kweiyo lattice paramita: β12 uye χ317.Izvi zvakaratidza kuti chimiro cheborocene chaive chekristaro, asi ukobvu uye chimiro chekristaro chakachinja pakubuda.Zvisinei, zvinonyatsoratidza kutsamira kwegidhi rinoshandiswa (Cu kana Ni) pane crystallinity yezvakaita borene.Kune Cu kana Ni, inogona kuva imwe-crystal kana polycrystalline, zvichiteerana.Kugadziriswa kweCrystal kwakawanikwawo mune mamwe maitiro e exfoliation18,19.Muchiitiko chedu, danho d uye chimiro chekupedzisira chinoenderana nemhando yegridi inoshandiswa (Ni, Cu).Kusiyana kwakasiyana-siyana kunogona kuwanikwa muSAED mapatani, zvichiratidza kuti nzira yedu inotungamirira pakuumbwa kwemamwe maitiro ekristal akafanana.Mukuwedzera, elemental mepu (EDX) uye STEM imaging yakaratidza kuti yakagadzirwa 2D zvinhu zvinosanganisira chinhu boron (Fig. S5).Zvisinei, kuitira kunzwisisa kwakadzama kwechimiro, zvimwe zvidzidzo zvezvinhu zvekugadzira borophenes zvinodiwa.Kunyanya, kuongororwa kweborene edges kunofanirwa kuenderera mberi, sezvo vachiita basa rakakosha mukugadzikana kwechinhu uye kuita kwayo kunobatsira20,21,22.
TEM mifananidzo yehuwandu hweboron A, B Cu_Li+_1 A neC Ni_Li+_1 A uye inoenderana SAED mapatani (A', B', C');nekukurumidza Fourier shandura (FFT) kuisa kumufananidzo weTEM.
X-ray photoelectron spectroscopy (XPS) yakaitwa kuti ione dhigirii ye oxidation yemasamples eborene.Munguva yekupisa kwemuenzaniso weborophene, chiyero cheboron-boron chakawedzera kubva pa6.97% kusvika pa28.13% (Table S3).Zvichakadaro, kuderedzwa kwebhoron suboxide (BO) zvisungo kunoitika kunyanya nekuda kwekuparadzaniswa kwepamusoro oxides uye kutendeuka kweboron suboxide kuB2O3, sezvinoratidzwa nehuwandu hweB2O3 mumasampuli.Pamusoro pemuonde.S8 inoratidza shanduko muyero yekubatanidza ye boron uye oxide zvinhu pakudziya.Iyo yakazara spectrum inoratidzwa mufig.S7.Miedzo yakaratidza kuti boronene yakasvibiswa pamusoro pe boron: oxide ratio ye1: 1 isati yapisa uye 1.5: 1 mushure mekupisa.Kuti uwane tsananguro yakadzama yeXPS, ona Supplementary Ruzivo.
Miedzo yakatevera yakaitwa kuti iedze mhedzisiro yezvino yakashandiswa pakati pema electrode panguva yekuparadzaniswa kwe electrochemical.Iwo maedzo akaitwa panguva dze0.5 A uye 0.1 A muLiCl/DMSO, zvichiteerana.Migumisiro yezvidzidzo zveAFM inoratidzwa muFig. 4, uye mapeji ekukwirira akaenzana anoratidzwa muFig.S2 uye S3.Tichifunga kuti kukora kwe borophene monolayer inenge 0.4 nm, 12,23 mukuedza pa 0.5 A uye kuvapo kwegridi yemhangura, iyo thinnest flakes inoenderana ne5-11 borophene layers ine lateral dimensions inenge 0.6-2.5 μm.Mukuwedzera, mukuedza nenickelmagridi, maflakes ane kudiki kwazvo kugovera ukobvu (4.82-5.27 nm) akawanikwa.Sezvineiwo, boron flakes inowanikwa ne sonochemical nzira dzine zvakafanana flake saizi muhuwandu hwe1.32-2.32 nm7 kana 1.8-4.7 nm8.Mukuwedzera, iyo electrochemical exfoliation yegraphene inokurudzirwa naAchi et al.14 yakakonzera maflakes akakura (> 30 µm), angave ane hukama nehukuru hwechinhu chekutanga.Nekudaro, magraphene flakes ane 2-7 nm gobvu.Mafuraki ehukuru hwakafanana uye hurefu hunogona kuwanikwa nekuderedza kushandiswa ikozvino kubva ku1 A kusvika ku0.Izvo zvinofanirwa kucherechedzwa kuti zviedzo zvakaitwa pane nickel grid ine ikozvino ye0.1 A hazvina kubudirira.Izvi zvinokonzerwa nekuderera kwemagetsi ekugadzirisa nickel kana ichienzaniswa nemhangura uye simba risina kukwana rinodiwa kugadzira borophene24.TEM kuongororwa kweCu_Li+_0.5 A, Cu_Li+_0.1 A, Cu_SO42-_1 A, Ni_Li-_0.5 A uye Ni_SO42-__1 A inoratidzwa muFigure S3 uye Figure S4, maererano.
Electrochemical ablation inoteverwa neAFM imaging.(A) Cu_Li+_1A, (B) Cu_Li+_0.5A, (C) Cu_Li+_0.1A, (D) Ni_Li+_1A, (E) Ni_Li+_0.5A.
Pano isu tinopawo nzira inogoneka ye stratification yeakawanda drill mutete-layer drills (Fig. 5).Pakutanga, iyo yakawanda bur yakatsikirirwa muCu / Ni grid kuti iite conduction mu electrode, iyo yakabudirira kushandisa voltage pakati peaxiliary electrode (Pt wire) uye electrode inoshanda.Izvi zvinobvumira maion kuti afambe kuburikidza ne electrolyte uye ave akaiswa mu cathode / anode zvinhu, zvichienderana ne electrolyte inoshandiswa.Ongororo yeAAS yakaratidza kuti hapana maion akaburitswa kubva musimbi mesh panguva iyi (ona Supplementary Information).yakaratidza kuti ions chete kubva ku electrolyte inogona kupinda mukati mebhoroni.Iyo yakawanda yekutengesa boron inoshandiswa mune iyi nzira inowanzonzi "amorphous boron" nekuda kwekugoverwa kwayo kusina kurongeka kwezvikamu zvekutanga masero, icosahedral B12, iyo inopisa kusvika ku1000 ° C kuti iite yakarongedzerwa β-rhombohedral structure (Fig. S6) 25 .Zvinoenderana nedata, lithium cations inopinzwa nyore muchimiro cheboron padanho rekutanga uye kubvarura zvimedu zvebhatiri reB12, pakupedzisira kugadzira maviri-dimensional boronene dhizaini ine yakarongeka yakarongeka, senge β-rhombohedra, β12 kana χ3 , zvichienderana neyakashandiswa ikozvino uyemeshzvinhu.Kuratidza hukama hweLi + kune boron yakawanda uye basa rayo rinokosha mukugadzirisa delamination, kukwanisa kwayo zeta (ZP) yakayerwa kuva -38 ± 3.5 mV (ona Supplementary Information) .Iyo yakaipa ZP kukosha kweboron yakawanda inoratidza kuti kupindirana kweiyo positive lithium cations kunoshanda kupfuura mamwe maion anoshandiswa muchidzidzo ichi (senge SO42-).Izvi zvinotsanangurawo kupinza kwakanyanya kweLi + muchimiro cheboron, zvichikonzera kubviswa kwakanyatsonaka kwe electrochemical.
Nokudaro, takagadzira nzira itsva yekuwana mabhoroni akadzika-layer ne electrochemical stratification ye boron uchishandisa Cu / Ni grids muLi +/DMSO uye SO42-/H2O mhinduro.Inoitawo seinopa kuburitsa pamatanho akasiyana zvichienderana neyazvino yakashandiswa uye grid inoshandiswa.Iyo nzira yekubvisa exfoliation inotsanangurwa uye inokurukurwa.Zvinogona kugumiswa kuti mhando-inodzorwa yakaderera-layer boronene inogona kugadzirwa nyore nekusarudza yakakodzera simbi mesh semutakuri weboron uye nekugadzirisa iyo inoshandiswa ikozvino, iyo inogona kushandiswa zvakare mukutsvaga kwekutanga kana maapplication anoshanda.Zvinonyanya kukosha, iyi ndiyo yekutanga yakabudirira kuedza pa electrochemical stratification ye boron.Zvinotendwa kuti iyi nzira inowanzo shandiswa kuburitsa zvinhu zvisiri-conductive kuita maviri-dimensional mafomu.Nekudaro, kunzwisiswa kuri nani kwechimiro uye zvivakwa zveakaita yakaderera-layer burs inodiwa, pamwe nekuwedzera kutsvagisa.
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Nickel wire mesh imhando yewaya yeindasitirijirayakagadzirwa kubva kune nickel waya.Iyo inoratidzirwa nekugara kwayo, magetsi conductivity, uye kuramba kune corrosion uye ngura.Nekuda kwehunhu hwayo hwakasiyana, nickel waya mesh inowanzoshandiswa mumashandisirwo akadai sekusefa, sieving, uye kupatsanura mumaindasitiri akadai seaerospace, makemikari, uye kugadzira chikafu.Inowanikwa muhukuru hwema mesh saizi uye waya madhayamita kuti ienderane nezvinodiwa zvakasiyana.