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Carbon dioxide kha formic acid ah electrochemical in tlawmternak cu carbon dioxide hmannak tthanchoternak caah ruahchannak a ummi lam a si i hydrogen chiahnak thilri ah hman khawhnak a ngei. Hi rian ah hin, carbon dioxide chungin formic acid direct electrochemical sernak caah zero-gap membrane electrode assembly architecture cu ser a si. A biapi mi thiamnak lei thanchonak cu a cation thlennak membrane a si, cucu, hmailei ah aa merhmi bipolar membrane dirhmun ah hman a si tikah, membrane karlak ah a chuakmi formic acid cu 0.25 M tluk a tlawmmi ah anodic flow field chungin a thlen khawh. le meihol cell le hydrogen electrolysis ah a tlangpi in hmanmi suaisam hna, cu nih cun rang deuh in karhternak le chawlehnak ah thlennak a tuah khawh. cm2 cell ah, a kuaimi cation thlennak membrane dirhmun nih <2 V le 300 mA/cm2 ah formic acid caah >75% Faraday tthatnak a pek. A biapi deuhmi cu, 200 mA/cm2 ah suimilam 55 chung fekmi hneksaknak nih a fekmi Faraday tthatnak le cell voltage a langhter. Techno-economic hlathlainak cu a tu lio formic acid chuah ningcang he man tlukruannak hmuh khawhnak lam langhternak caah hman a si.
A tharchuah khawhmi mei hmangin carbon dioxide kha formic acid ah electrochemical in tlawmternak nih thilchuah man kha 75%1 tiang a zorter ti a si, hlanlio thil hlun hmanmi he tahchunh tikah. Cauk2,3 ah langhtermi bantukin, formic acid nih hmannak phunphun a ngei, hydrogen chiahnak le phurhnak ah a ttha i a man a fawimi lam in chemical industry4,5 asiloah biomass industry6 caah rawlchuannak thilri tiang. Formic acid cu metabolic engineering hmangin a hnu ah a hmunmi vanlawng meihol karlak ah thlennak caah rawlchuannak thilri ah hngalh a si cang7,8. Formic acid sipuazi1,9 tthanchonak he, hlathlainak rian zeimawzat nih catalyst thim khawhnak tthatternak ah an i hngat10,11,12,13,14,15,16. Sihmanhsehlaw, zuamnak tampi nih H-cell hmete asiloah ti a luangmi cell hna kha a tlawmmi current density (<50 mA/cm2) ah rian a ttuanmi ah an i hngat peng. Man tlawmternak, chawlehnak hmuh khawhnak le a hnu ah chawlehnak luh khawhnak karhternak caah, electrochemical carbon dioxide zorternak (CO2R) cu a sangmi current density (≥200 mA/cm2) le Faraday tthatnak (FE)17 ah tuah a hau, cu lio ah thilri hmannak tamter le Technology fuel cells in battery thilri pawl hmannak le electrolysis CO2R thilri hna lak khawhnak ding caah sipuazi tthatnak18. Cun, thilchuah khawhnak tthatnak karhter awk le a dang a tanglei thilri sernak hrial awkah, formic acid kha formate salts nakin a donghnak thilchuak ah hman ding a si19.
Hi lei ah, naite ah riantuannak he aa pehtlaimi CO2R formate/formic acid hrambunhmi gas diffusion electrode (GDE) thilri sernak caah zuamnak an tuah. Fernandez-Caso le a hawile nih an tuahmi a tlingmi zohfelnak nih CO2 kha formic acid/formate ah pehzulh tein zorternak caah electrochemical cell sining vialte kha a tawinak in a langhter. A tlangpi in, a um cangmi sining vialte cu phun thum ah ṭhen khawh an si: 1. A luangmi catholytes19,21,22,23,24,25,26,27, 2. Membrane pakhat lawng (cation exchange membrane (CEM)28 asiloah anion exchange membrane (AEM)29 le 3. Sandwich configuration, Simplified, 3313,33. hi tthencheunak hna cu hmanthlak 1a ah langhter an si. Catholyte i a luannak tthencheunak caah, GDE i membrane le cathode karlak ah electrolyte khaan pakhat ser a si. SnO2 cathode hmangin 1.27 mm a thukmi catholyte tthen he carbon substrate hmangin, 500 mA/cm2 ah 90% FE 35 tiang hmuh khawh a si. 15%. Thazaang tthatnak tthanchoter awkah, Li le a hawile nih, CEM pakhat lawng hmangin, 51.7 mA/cm2 tluk a tlawmmi FE 29 an hmuh. duh deuhmi thilri, formic acid si loin. CEM dirhmun ah, KCOOH tibantuk format pawl cu GDE le flow field ah rang tein an i pum kho, cu nih cun phorh khawhnak khamnak le a donghnak ah cell rawhnak a chuahter.
A lang bikmi CO2R pathum le formate/formic acid thlennak thilri sining le hi hlathlainak ah ruahnak cheuhmi suaisam ning tahchunhnak. b Catholyte dirhmun, sandwich dirhmun, cauk chung i CEM dirhmun pakhat lawng (Supplementary Table S1 ah langhtermi) le kan riantuannak caah a dihlak in a tu lio le formate/formic acid chuahmi tahchunhnak. A ongmi hmelchunhnak nih formate cawhmi chuahnak a langhter, cun a fekmi hmelchunhnak nih formic acid chuahnak a langhter. *Anode ah hydrogen hmangin langhtermi sining. c Zero-gap MEA dirhmun cu hmailei ah a ummi cation i thlennak tthen he aa fonhmi bipolar membrane hmangin a si.
Formate sernak khamnak caah, Proietto et al. 32 nih a tthen lomi filter press dirhmun a hman i cu ah cun deionized ti cu a karlak ah a luang. Mah system nih hin 50-80 mA/cm2 karlak ah >70% CE a phan kho. Cu bantuk cun, Yang le a hawile. 14 nih CEM le AEM karlak ah formic acid sernak bawmhchanh awkah a fekmi electrolyte interlayer hman ding in ruahnak a chuahpi. Yang et al.31,36 nih 200 mA/cm2 ah 5 cm2 cell ah 91.3% FE an hmuh, 6.35 wt% formic acid cawhmi an chuah. Xia le a dangdang. Aa lo ngaimi dirhmun hmangin, 200 mA/cm2 ah carbon dioxide (CO2) in formic acid FE ah 83% thlennak tuah khawh a si, cun suimilam 100 minutes 30 chung system fek tein hneksaknak tuah a si. A hmete in hmuhmi cu ruahchannak a um ko nain, porous ion exchange resins man a karhmi le a harmi nih interlayer configuration kha a ngan deuhmi system (eg, 1000 cm2) ah thlen a harter.
Design phunphun hna i an net effect hmuh khawhnak ding caah, a hlan deuh ah kan langhtermi system vialte caah kWh pakhat ah formate/formic acid chuahmi kha kan suai i Figure 1b ah kan suai. Hika ah hin catholyte asiloah interlayer aa telmi zeibantuk system paoh nih a tlawmmi current density ah a riantuan ning a sang bik lai i a sangmi current density ah a tlau lai ti cu a fiang ko, cuka ahcun ohmic ri nih cell voltage a khiah khawh. Cun, thazaang ttha tein hman khawhmi CEM dirhmun nih kWh pakhat ah molar formic acid chuahnak a sang bik a pek ko nain, chiti a karhmi nih a sangmi current density ah riantuan ning rawhnak rang tukin a chuahter khawh.
A hlan ah kan i ruahmi tlamtlin lonak phun pawl zorternak caah, a cation thlennak membrane (PCEM) he aa fonhmi hmailei ah aa merhmi BPM aa telmi membrane electrode assembly (MEA) kan ser. A sining cu hmanthlak 1c ah hmuh khawh a si. Hydrogen (H2) cu anode chungah hydrogen oxidation reaction (HOR) hmangin proton chuahter awkah luhter a si. BPM system chungah PCEM tthen cu cathode ah a chuakmi formate ions pawl kha AEM chungin a kal khawh nakhnga, protons he fonh in BPM interface le CEM karlak pores ah formic acid a ser khawh nakhnga an luhter, cun GDE anode le flow field in an chuak. . Hi dirhmun hmangin, 25 cm2 cell area caah <2 V le 300 mA/cm2 ah formic acid >75% FE kan hmuh. A biapi bikmi cu, suaisam nih chawlehnak ah hmuh khawhmi thilri le thilri suaisamnak hna kha fuel cell le ti electrolysis sehzung caah a hman, cu nih cun a rang deuhmi caan a pek. Catholyte dirhmun ah catholyte luannak khaan a um i cu nih cun gas le ti karlak ah hneknak aa tluk lonak a chuahter khawh, a hlei in cell dirhmun ngan deuh ah. Ti a luangmi a tlongmi tthen a ngeimi sandwich sining hna caah, a tlongmi a karlak tthen kha a ttha bik in sersiam awkah fakpi in i zuam a hau i cu nih cun a karlak tthen chung ah hneknak a zorter i carbon dioxide a khonmi a zorter. Mah pahnih nih hin cellular pehtlaihnak a hrawh khawh. Cun, a nganmi ah a dir khomi a tlawmmi a tlawmmi tthen pawl chuah zong a har. Cu he aa dang in, ruahnak cheuhnak thar cu a luannak khaan asiloah a karlak tthen aa tel lomi zero-gap MEA dirhmun a si. A um cangmi electrochemical cell dang hna he tahchunh ahcun, an chuahpimi dirhmun cu a dang tein a um, zeicahtiah a tthangcho khomi, thazaang a tlawmmi, aa tthencheu lomi dirhmun ah formic acid direct in ser khawhnak a tuah.
Hydrogen thlennak kha kham awkah, CO2 zorternak riantuannak nganpi nih MEA le AEM membrane sining hna kha a sangmi molar concentration electrolytes (tahchunhnak ah, 1-10 M KOH) he fonh in cathode ah alkaline dirhmun ser awkah an hman (Figure 2a ah langhter bantuk in). Hi dirhmun ah, cathode ah a chuakmi formate ions pawl cu a ttha lomi charge a ngeimi phun bantukin membrane chungin an kal, cun KCOOH a chuak i anodic KOH stream in system chungin a chuak. Formate FE le cell voltage cu a hramthawk ahcun Figure 2b ah langhtermi bantuk in a ttha ko nain, fekmi hneksaknak nih 10 h chung lawng ah FE 30% hrawng a zorter (Figure S1a–c). M KOH anolyte hmannak cu alkaline oxygen evolution reaction (OER) system37 ah anodic overvoltage tlawmternak le cathode catalyst bed33 chung i ion luh khawhnak hmuh khawhnak caah a biapi tukmi a si ti kha hngalh a herh. Anolyte tlawmtam cu 0.1 M KOH tiang a zor tikah, cell voltage le formic acid oxidation (formic acid tlau) pahnih an karh (Figure S1d), zero-sum trade-off a langhter. Formate oxidation tlukruannak cu a dihlak in ritnak tlukruannak hmangin tah a si; a konglam tam deuh theih na duh ahcun, “Lam” timi ṭhen kha zoh. MEA le CEM membrane pakhat lawng hmannak hmangin riantuan ning zong hlathlainak tuah a si, cun a phichuak cu Figure S1f,g ah langhter a si. Cathode chungin lakmi FE formate cu hneksaknak thawk ah 200 mA/cm2 ah >60% a si, asinain a hlan ah kan i ruahmi cathode chiti khonnak ruangah suimilam pahnih chungah rang tukin a rawk (Figure S11).
Cathode ah CO2R, anode ah hydrogen oxidation reaction (HOR) asiloah OER, le a karlak ah AEM membrane pakhat he zero-gap MEA hmanthlak. b FE le cell voltage caah hi dirhmun caah 1 M KOH le OER cu anode ah a luang. Palhnak hri nih tahnak phun thum i aa dangmi thleidannak kha a langhter. FE le system cell voltage ah H2 le HOR he anode ah. Formate le formic acid chuahternak thleidan khawhnak ding caah rong phunphun an hman. d MEA hmanthlak cu BPM cu a laifang ah hmailei ah aa thlen. FE le battery voltage le caan 200 mA/cm2 ah hi dirhmun hmangin. f Hneksaknak tawite tuah hnu ah hmailei ah aa merhmi BPM MEA hmanthlak.
Formic acid chuah khawhnak ding caah, hydrogen cu anode ah Pt-on-carbon (Pt/C) catalyst ah pek a si. Figure 2d ah hmuh khawhmi bantuk in, hmailei ah aa merhmi BPM nih anode ah proton a chuahtermi cu formic acid chuah khawhnak ding caah a hlan ah hlathlainak tuah a si cang. BPM tuning unit cu 200 mA/cm2 current ah minutes 40 chung riantuan hnu ah a rawk, 5 V nak tam voltage a kai (Fig. 2e). Hneksaknak tuah hnu ah, CEM/AEM karlak ah a fiangmi tthencheunak hmuh a si. Formate lengah, carbonate, bicarbonate le hydroxide tibantuk anion pawl zong AEM membrane chungin an kal khawh i CEM/AEM karlak ah protons he an i pehtlaih khawh i CO2 gas le ti ti an chuahter khawh, cu nih cun BPM delamination (Fig. 2f) a chuahter i, a donghnak ah cell rawhralnak a chuahter.
A cunglei dirhmun riantuan ning le tlamtlin lonak mechanism cung ah hram bunh in, MEA sining thar cu hmanthlak 1c ah langhtermi le hmanthlak 3a38 ah fiang tein langhter a si. Hika ah, PCEM tthen nih CEM/AEM pehtlaihnak in formic acid le anions pawl an i ṭhialnak lam a pek hna, cucaah thilri pawl an i khonnak kha a zorter. Cu caan te ah cun, PCEM karlak lam nih formic acid cu a karhnak hmun le a luannak hmun ah a hruai, cu nih cun formic acid oxidation a zorter. 80, 40 le 25 mm a chahmi AEMs hmangin polarization hmuhmi cu hmanthlak 3b ah hmuh khawh a si. Ruahning bantuk in, AEM a thuhnak a karh tikah a dihlak in cell voltage a karh ko nain, a thuh deuhmi AEM hmannak nih formic acid a hnulei ah a karh lonak ding caah a kham, cucaah cathode pH a karhter i H2 chuahternak a zorter (Fig. 3c–e).
a AEM le perforated CEM le formic acid kalnak lam phunphun he MEA sining langhternak. b Cell voltage cu aa dangmi current density le aa dangmi AEM thickness ah. EE ah AEM 80 μm (d) 40 μm, e) 25 μm a thuhnak he aa dangmi current density ah. Palhnak tthencheunak nih a dang tein sample pathum in tahmi tlukruannak a langhter. f AEM a tlawm le tam aa dangmi CEM/AEM karlak ah formic acid tlawmtam le pH man zohchunhnak hmuhmi. f PC le pH cu AEM film a chahmi aa dangmi catalyst cathode tthen ah a um. g CEM/AEM pehtlaihnak le khuhnak he formic acid tlawmtam tthencheunak pahnih.
Figure S2 nih Poisson-Nernst-Planck finite element modeling hmangin MEA a thuhnak chung ah formic acid tlawmtam le pH i phawtzamhnak a langhter. Formic acid a tam bik, 0.23 mol/L, cu CEM/AEM karlak ah hmuh a si cu khuaruahhar awk a si lo, zeicahtiah hi pehtlaihnak ah hin formic acid a chuak. AEM chungin formic acid a tlawm deuhdeuh tikah AEM a thuhnak a karh deuhdeuh tikah a zor deuhdeuh, cu nih cun thilri thlennak doh khawhnak a ngan deuhdeuh i hnulei tthennak ruangah formic acid a tlawm deuhdeuh ti a langhter. Hmanthlak 3 f le g nih cathode catalyst ihkhun chung i pH le formic acid man kha hnulei tthencheunak le formic acid tlawmtam tthencheunak nih a chuahtermi an langhter. AEM membrane a tlawm deuhdeuh tikah, cathode pawng ah formic acid a tam deuhdeuh i, cathode pH cu acidic ah a cang. Cucaah, a thuk deuhmi AEM membrane nih ohmic sunghnak a sang deuhmi a chuahter ko nain, cathode ah formic acid a kir tthannak khamnak le FE formic acid system a thianhlimnak sang bik khamnak caah a biapi tukmi an si. A donghnak ah, AEM thuhnak kha 80 μm tiang karhternak nih <2 V ah formic acid caah FE >75% le 25 cm2 cell area caah 300 mA/cm2 a chuahter.
Hi PECM-based architecture a fekmi hneksaknak caah, battery current cu 200 mA/cm2 ah suimilam 55 chung chiah a si. A dihlak in hmuhmi cu hmanthlak 4 ah langhter a si, a hmasa suimilam 3 chungin hmuhmi cu hmanthlak S3 ah langhter a si. Pt/C anodic catalyst hman tikah, cell voltage cu a hmasa 30 min chungah fakpi in a karh (Figure S3a). Caan sau deuh chung ah, cell voltage cu aa thleng bal lo, 0.6 mV/h (Fig. 4a) rawhnak rate a pek. Hneksaknak thawk ah, anode ah lakmi formic acid PV cu 76.5% a si i cathode ah lakmi hydrogen PV cu 19.2% a si. Hneksaknak suimilam pakhatnak hnu ah, hydrogen FE cu 13.8% tiang a tla, cu nih cun formate thim khawhnak a tthanchoter ti a langhter. Sihmanhsehlaw, system chung i formic acid oxidation rate cu suimilam 1 chungah 62.7% tiang a tla, cun anodic formic acid oxidation rate cu hneksaknak hramthawk ah zero hrawng in 17.0% tiang a kai. Cu hnu ah, H2, CO, formic acid FE le formic acid anodic oxidation rate cu hneksaknak chung ah aa thleng lo. Suimilam pakhatnak chung ah formic acid oxidation a karhmi cu PCEM/AEM karlak ah formic acid a karh caah a si kho men. Formic acid a karh tikah, membrane a kuhnak in a chuak lawng si loin, FEM chungin a karh i Pt/C anode tthen ah a lut. Formic acid cu 60°C ah ti bantuk a si caah, a khonmi nih thilri thlennak kongah harnak a chuahter khawh i hydrogen nakin a ttha deuhmi oxidation a chuahter khawh.
a Cell voltage le caan (200 mA/cm2, 60 °C). A chunglei nih cun MEA pakhat i a tthencheunak EM he aa tthenmi optical microscope hmanthlak a langhter. Tahnak: 300 μm. b Pt/C anode hmangin 200 mA/cm2 ah caan he aa pehtlaimi PE le formic acid thianhlimnak.
Hneksaknak hramthawknak (BOT) ah timhtuahnak lio le hneksaknak donghnak (EOT) ah 55 h ttha tein hneksaknak tuah hnu ah sample pawl an muisam cu nano-X-ray computed tomography (nano-CT) hmangin langhter a si, hmanthlak 5 a ah hmuh khawh a si. EOT sample cu BOT caah 930 nm he tahchunh tikah 1207 nm a kauhnak he catalyst particle ngan deuh a ngei. High-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) hmanthlak le thazaang-tthennak X-ray spectroscopy (EDS) hmuhmi hna cu Figure 5b ah langhter an si. BOT catalyst tthen nih hin a hme deuhmi catalyst particles tam deuh le a ngan deuhmi agglomerates cheukhat a ngeih lio ah, EOT dirhmun ah catalyst layer cu a dang tein hmun hnih ah tthen khawh a si: pakhat cu a ngan deuhmi solid particles he a dang pakhat cu a porous deuhmi hmun he. A hme deuhmi thil hme tete an zat. EDS hmanthlak nih a langhter mi cu a nganmi a fekmi thil hme tete hna cu Bi in an khat, thir Bi a si kho men, cun a tlongmi hmun hna cu oxygen in an khat. Cell cu 200 mA/cm2 ah rian a ttuan tikah, cathode i a ttha lomi thilti khawhnak nih Bi2O3 a zorter lai, a tanglei ah kan i ruahmi in situ X-ray laknak spectroscopy hmuhmi nih a langhter. HAADF-STEM le EDS mapping nih a langhter mi cu Bi2O3 nih tlawmternak a tuah, cu nih cun oxygen a sunghter hna i thir tlawmpal ngan deuh ah a fonh hna. BOT le EOT cathode hna i X-ray diffraction pattern nih EDS data fianternak kha a fehter (Fig. 5c): BOT cathode ah crystalline Bi2O3 lawng hmuh a si, cun EOT cathode ah crystalline bimetal hmuh a si. Bi2O3 cathode catalyst oxidation dirhmun cung ah cathode thazaang nih a chuahpimi thil hngalhthiam awkah, lumnak cu a ongmi circuit thazaang (+0.3 V vs RHE) in -1.5 V (vs RHE) tiang thlen a si. Bi2O3 tthen cu RHE he tahchunh tikah -0.85 V ah a zor hram aa thawk ti hmuh a si, cun spectrum tthennak hmun ah a rangmi hri a tthawnnak a zor tikah thir Bi cu -1.1 ah RHE 90% tiang a zor ti a langhter. V cu RHE he aa ralchanh (Fig. 5d). A kalning zei a si hmanh ah, cathode ah formate a dihlak in thim khawhnak cu aa thleng lo, H2 le CO FE le formic acid sernak in hmuh khawh a si, cathode sining, catalyst oxidation dirhmun le microcrystalline sining ah thlennak nganpi a um ko nain.
a Nano-X-ray CT hmangin hmuhmi catalyst tthencheunak le catalyst particles tthencheunak a tthenthum in a ummi sining. Tahnak: 10 μm. b A cunglei 2: BOT le EOT catalysts cathode tthen HAADF-STEM hmanthlak hna. Tahnak: 1 μm. A tanglei 2: EOT catalyst cathode tthen i a ngan deuhmi HADF-STEM le EDX hmanthlak hna. Tahnak: 100 nm. c BOT le EOT cathode sample hna i X-ray thlennak sining hna. d 0.1 M KOH chung i Bi2O3 electrode i a hmun ah X-ray laknak spectra cu a tthawnnak (0.8 V in -1.5 V vs. RHE) riantuannak in a si.
Formic acid oxidation khamnak in thazaang tthatnak tthanchoternak caah zeibantuk caantha dah a um ti hngalh khawhnak ding caah, H2 reference electrode cu voltage tlaunak nih a chuahpimi hngalh khawhnak ding caah hman a si39. 500 mA/cm2 nak tlawm deuh a tu lio ah, cathode thazaang cu -1.25 V tang ah a um. Anodic thazaang cu a tlangpi in tthen hnih ah tthen a si: thlennak current tlawmtam HOR le a hlan i tahmi Bulter-Volmer equation nih a chimchungmi theoretical overvoltage HOR 40, cun a tangmi cu oxidation acid caah a si. HOR41 he tahchunh tikah a tlawm deuhmi thlennak kinetics ruangah, anode ah formic acid oxidation thlennak tlawmte nih anodic thilti khawhnak a karhter khawh. A phichuak nih a langhter mi cu formic acid anodic oxidation tling tein khamnak nih 500 mV overvoltage hrawng a hloh khawh.
Hi tuaktannak hneksaknak caah, anode luhnak ah deionized ti (DI) a luan ning kha a chuakmi formic acid tlawmternak caah thlen a si. Hmanthlak 6b le c nih FE, formic acid tlawmtam, le cell voltage kha 200 mA/cm2 ah anode ah DI flux riantuannak in an langhter. Deionized ti luannak rate cu 3.3 mL/min in 25 mL/min tiang a karh tikah, anode ah formic acid tlawmtam cu 0.27 mol/L in 0.08 mol/L tiang a zor. Tahchunhnak ah, Xia le a hawile nih an chuahpimi sandwich sining hmangin. 30 a formic acid 1.8 mol/L cu 200 mA/cm2 ah hmuh a si. A tlawmternak nih formic acid a dihlak in FE a tthanter i H2 FE a zorter, zeicahtiah cathode pH cu formic acid a hnulei a karhnak a zor caah alkaline deuh a si. A tam bik DI luannak ah a zormi formic acid tlawmternak nih formic acid oxidation zong a hloh dih, cu nih cun 200 mA/cm2 ah 1.7 V tang lawng a simi cell voltage dihlak a chuahter. Battery lumnak zong nih riantuan ning dihlak a hnorsuan, cun a phichuak cu Figure S10 ah hmuh khawh a si. Sihmanhsehlaw, PCEM-based architectures nih formic acid oxidation khamnak ah thazaang ttha tein hman khawhnak kha a tthanchoter khawh, formic acid lei ah hydrogen thim khawhnak a tthanchotermi anodic catalysts hmannak in siseh, thilri riantuannak in siseh.
a 60 °C ah rian a ttuanmi cell reference H2 electrode, Pt/C anode le 80 μm AEM hmangin cell voltage hrawhnak. b FE le formic acid tlawmtam kha 200 mA/cm2 ah anodic deionized ti a luan ning aa dangmi hmangin an lak. c Anode nih a phunphun in formic acid a lak tikah, cell voltage cu 200 mA/cm2 a si. Palhnak hri nih tahnak phun thum i aa dangmi thleidannak kha a langhter. d Ram pumpi riantuannak ah a tlangpi in mei man US$0.068/kWh le US$4.5/kg hydrogen hmangin deionized ti luannak phunphun ah riantuan ning in tthenmi a niam bik zuar man. (*: Anode ah formic acid a niam bik oxidation dirhmun cu 10 M FA a si lai tiah ruah a si, ram pumpi ah a tlangpi in riantuannak mei man cu $0.068/kWh a si, cun hydrogen cu $4.5/kg a si. **: A niam bik oxidation dirhmun cu formic acid a si lai tiah ruah a si. Anode ah FA a tlawm bik cu 13 M a si, hmailei ah electric man a si lai tiah ruah a si. $0.03/kWh, cun dot line nih 85 wt% FA market man a langhter.
Figure 5d ah langhtermi bantukin, riantuannak dirhmun phunphun tangah meihol fonhmi hna i a niam bik zuar man hmuh khawhnak ding caah techno-economic hlathlainak (TEA) tuah a si. TEA caah hmanmi lam le hnulei konglam hna cu SI ah hmuh khawh a si. Anode chuahnak ah LC tlawmtam a tam deuh tikah, cell voltage a sang deuh ko nain, tthennak man a zor caah meihol fonhnak man dihlak cu a zor. Catalyst sernak asiloah electrode thiamnak in formic acid i anodic oxidation kha tlawmter khawh a si ahcun, a niam deuhmi cell voltage (1.66 V) le a chuakmi ti chung i FA a tam deuhmi (10 M) fonhmi nih electrochemical FA chuahnak man kha 0.74 US dollars/kg (electric mei cung ah hram bunh in) tiang a zorter lai. man) $0.068/kWh le $4.5/kg hydrogen42. Cun, hmailei ah thlen khawhmi mei man $0.03/kWh le hydrogen $2.3/kg he fonh tikah, FA ti thurhnawm tinhmi cu 1.3 million ah a zor, cu nih cun a donghnak ah ruahmi chuah man cu US$0.66/kg43 a si. Mah cu a tu market man he tahchunh khawh a si. Cucaah, hmailei ah electrode thilri le sining hna ah aa hngatmi zuamnak nih anodization kha a zorter chinchin khawh i cu lioah cell voltage niam deuh ah riantuannak kha a sang deuhmi LC tlawmtam chuah khawhnak nawl a pek khawh.
A tawinak in chim ahcun, CO2 kha formic acid ah tlawmternak caah zero-gap MEA sining zeimawzat kan hlathlai i a chuakmi formic acid caah membrane mass transfer interface tuah khawhnak ding caah perforated cation exchange membrane (PECM) aa telmi composite forward-biased bipolar membrane aa telmi sining pakhat kan chuahpi. . Hi dirhmun nih hin 0.25 M tiang (anode DI luannak 3.3 mL/min) ah >96% formic acid a chuahter. DI luannak sang deuh (25 mL/min) ah, hi dirhmun nih 25 cm2 cell area hmangin 1.7 V ah 200 mA/cm2 >80% FE a pek. A tlawm deuhmi anodic DI rate (10 mL/min) ah, PECM dirhmun nih 200 mA/cm2 ah hneksaknak 55 h chung a fekmi voltage le a sangmi formic acid FE levels a kilven. Chawlehnak ah hmuh khawhmi catalysts le polymeric membrane thilri hna nih an hmuh khawhmi a sangmi fekmi le thim khawhnak cu a ttha bikmi electrocatalysts he fonh in a tthanchoter khawh. A hnu riantuannak nih riantuannak dirhmun, anode catalyst thim khawhnak, le MEA sining remh in formic acid oxidation zorternak ah a biapi in a chiah lai, cu nih cun a niam deuhmi cell voltage ah a tlawm deuhmi effluent a chuahter lai. Hika ah langhtermi formic acid caah carbon dioxide hmannak lam sawhsawh nih anolyte le catholyte khaan, sandwich thilri le thilri ttha a herhnak a hloh, cucaah cell thazaang tthatnak a karhter i system a harmi a zorter, cu nih cun a fawiter deuh. Ruahnak cheuhnak nih hin hmailei ah thiamnak le sipuazi lei in a ttha mi CO2 thlennak sehzung sernak caah hmunhma a pek.
A dang tein langhter a si lo ahcun, chemical phun thilri le cawhnuk vialte cu hmuhmi ning tein hman an si. Bismuth oxide catalyst (Bi2O3, 80 nm) cu US Research Nanomaterials, Inc. in cawk a si. Polymer powder (AP1-CNN8-00-X) cu IONOMR nih a pek. Omnisolv® brand N-propanol (nPA) le ultrapure water (18.2 Ω, Milli–Q® Advantage A10 ti thianhnak system) cu Millipore Sigma in cawk an si. ACS nih fehtermi methanol le acetone cu VWR Chemicals BDH® le Fisher Chemical in cawkmi an si. Polymer powder cu acetone le methanol cawhmi he 1:1 tluk in rit ning in cawh in 6.5 wt.% a tlawmmi polymer tthencheunak hmuh khawh a si. 30ml thawl chungah 20g Bi2O3, ti thiang tuk, nPA le ionomer tthencheunak cawh in catalytic ink kha timhtuah. Mah thilri ah hin 30 wt.% catalyst, ionomer le catalyst rit zat 0.02 le zu le ti rit zat 2:3 (40 wt.% nPA) aa tel. Cawh hlan ah, Glen Mills 5mm zirconia cawhnak thilri 70g cu cawhmi ah an cawh. Sample pawl cu FisherbrandTM digital bottle roller ah 80 rpm in suimilam 26 chung chiah an si. Na thuh hlanah cafang kha minutes 20 chung umter. Bi2O3 ink cu Qualtech automatic applicator (QPI-AFA6800) ah 1/2′′ x 16′′ laboratory wirewound refill (RD Specialties – 60 mil diameter) hmangin 22°C ah an thuh. 5 mL catalytic ink cu 7.5 x 8 inch Sigraacet 39 BB carbon gas diffusion carrier (fuel cell chiahnak) ah rod deposition in 55 mm/sec tluk rang in hman a si. Hi a thuhmi electrode pawl kha oven ah chiah hna law 80 °C ah roter hna. Rod thuhnak kalning le GDE thuhnak hmanthlak hna cu hmanthlak S4a le b ah hmuh khawh a si. X-ray fluorescence (XRF) thilri (Fischerscope® XDV-SDD, Fischer-Technolgy Inc. USA) nih a thuhmi GDE phorhmi cu 3.0 mg Bi2O3/cm2 a si ti kha a fehter.
Anion i thlengnak membrane (AEM) le perforated CEM aa telmi composite membrane dirhmun caah. Nafion NC700 (Chemours, USA) cu 15 μm a thuhnak he CEM tthen ah hman a si. Anodic catalyst cu ionomer le carbon ratio 0.83 le 25 cm2 a khuhnak hmun he FEM cungah direct in an thlet. Anode catalyst ah 0.25 mg Pt/cm2 a ritmi a kau ngaimi (50 wt.% Pt/C, TEC 10E50E, TANAKA thir mansung) he dirhmi platinum kha hman a si. Nafion D2020 (Ion Power, USA) cu catalyst i anode tthen caah ionomer ah hman a si. CEM khuhnak cu CEM zukcawl cung ah 3mm karlak ah aa tlukmi hri pawl tannak in tuah a si. Hmunhma thlennak konglam cu hmanthlak S12b le c ah hmuh khawh a si. X-ray computed tomography hmangin, hmanthlak S12d le e ah langhtermi bantuk in, a kuaimi tthennak cu 32.6 μm a si ti kha fehter a si. Cell fonh lio ah, catalyst-coated perforated CEM membrane cu 25 cm2 Toray cauk (5 wt% PTFE treated, Fuel Cell Store, USA) cung ah chiah a si. AEM membrane (PiperION, Versogen, USA) cu 25, 40 asiloah 80 μm a thuhnak cu CEM cung ah chiah a si i cu hnu ah GDE cathode cung ah chiah a si. AEM membrane cu a luannak hmun dihlak khuh awkah 7.5 × 7.5 cm tthen in an tan i fonh hlanah 1 M potassium hydroxide cawhnuk ah zankhuadei an chiah. Anode le cathode pahnih nih 18% GDE tlawmternak ttha bik hmuh khawhnak dingah a thukmi PTFE spacers an hman. Battery fonhnak konglam cu Figure S12a ah hmuh khawh a si.
Hneksaknak tuah lio ah, fonhmi cell cu 60 °C (30, 60, le 80 °C ah lum le kih aa hngatmi hlathlainak caah) ah chiah a si i 0.8 L/min hydrogen gas cu anode ah pek a si i 2 L/min carbon dioxide cu cathode ah pek a si. Anodic le cathodic thli luannak pahnih cu 100% aa pehtlaimi lumnak le 259 kPa a tlingmi cathodic hneknak ah an lumter hna. Riantuan lio ah, cathode gas stream cu 1 M KOH cawhmi he 2 mL/min in cawh a si i cathode catalyst ihkhun hmannak le ionic hruainak thanchoternak caah a si. Anode chung i formic acid chuah khawhnak ding caah anode gas a luangmi kha deionized ti he 10 ml/min tluk in cawh. Thilri luhternak le chuahnak kongkau cu hmanthlak S5 ah hmuh khawh a si. Cathode chuahmi thli nih CO2 a ngei i CO le H2 a chuahter. Ti lum cu condenser (2°C ah a niammi lumnak thlennak) hmangin chuah a si. A tangmi gas cu gas caan zohfelnak caah lak a si lai. Anode a luannak cu gas le ti thleidan khawhnak ding caah condenser chungin a kal ve lai. Ti thurhnawm cu a thiangmi thawl chungah an khawmh lai i a chuakmi formic acid zat tuak khawhnak dingah liquid chronometry hmangin hlathlainak tuah a si lai. Electrochemical hneksaknak cu Garmy potentiostat (reference number 30K, Gamry, USA) hmangin tuah a si. Polarization curve tah hlanah, cell cu 0 in 250 mA/cm2 karlak ah 2.5 mA/cm2 scan rate he linear voltammetry hmangin voi 4 tiang an thlen. Polarization curves cu galvanostatic mode in cell cu cathode gas le anolyte liquid lak hlan ah minutes 4 chung current density pakhatkhat ah chiah in hmuh an si.
Cathode le anodic potentials thleidan awkah MEA chung i hydrogen reference electrode kan hman. Reference electrode dirhmun cu hmanthlak S6a ah hmuh khawh a si. Nafion membrane (Nafion 211, IonPower, USA) cu MEA membrane le reference electrode pehtlaihnak caah ionic bridge ah hman a si. Nafion strip a donghnak pakhat cu 1 cm2 gas diffusion electrode (GDE) he pehtlaih a si i 0.25 mg Pt/cm2 (50 wt% Pt/C, TEC10E50E, TANAKA Precious Metals) cu 29BC carbon cauk (Fuel Cell Store, USA) ah a thlet. ). Special polyetheretherketone (PEEK) thilri cu gas kharnak le GDE le Nafion strips karlak ah pehtlaihnak tha a um khawhnak hnga le reference electrode kha fuel cell thilri he pehtlaihnak caah hman a si. Nafion strip a dang pakhat cu CEM battery a chuakmi tthen he aa pehtlai. Figure S6b nih MEA he fonhmi zohchunhmi electrode i a tthennak kha a langhter.
A chuakmi thli cu condenser le gas-liquid tthennak chungin a kal hnu ah, gas sample pawl cu cathode chungin an lak hna. A lakmi gas cu 4900 Micro GC (10 μm molecular sieve, Agilent) hmangin a tlawmbik voithum tiang hlathlainak tuah a si. Sample pawl cu caan khiahmi (second 30) chung inert multi-layer aluminium foil gas sample bags SupelTM (Sigma-Aldrich) ah an lak hna i an lak hnu suimilam pahnih chungah microgas chromatograph chungah kut in an khumh hna. Hnawmhnak lumnak cu 110°C ah chiah a si. Carbon monoxide (CO) le hydrogen (H2) cu a lummi (105 °C) hneknak (28 psi) 10 m MS5A column ah argon (Matheson Gas-Matheson Purity) kha carrier gas ah hmangin tthen an si. Hi pehtlaihnak hna cu a chung ah aa telmi lumternak hngalh khawhnak (TCD) hmangin hmuh khawh an si. GC chromatograms le CO le H2 tahfung hna cu Figure S7 ah hmuh khawh an si. Ti bantuk formic acid sample pawl cu anode chungin caan khiahmi (second 120) chung an lak hna i 0.22 μm PTFE syringe filter hmangin 2 mL vials ah an thlet hna. Vials chung i a ummi ti thilri pawl cu Agilent 1260 Infinity II bioinert high-performance liquid chromatography (HPLC) system hmangin an hlathlai hna, cu chungah 20 μl sample cu autosampler (G5668A) hmangin 4 mM sulfuric acid (H2SO4) aa chawkmi he an thun. ) 0.6 ml/min (quaternary pump G5654A) a luannak rate in. Thilri pawl cu a lummi (35°C, column oven G7116A) Aminex HPX-87H 300 × 7.8 mm (Bio-Rad) ah Micro-Guard Cation H guard column nih a hruai hna. Formic acid cu diode array detector (DAD) hmangin hmuh khawh a si. 210 nm wavelength le 4 nm bandwidth ah. HPL chromatogram le formic acid standard calibration curve cu Figure S7 ah hmuh khawh a si.
Gas chuahmi (CO le H2) FE cu a tanglei equation hmangin tuak a si, cun gas moles dihlak cu ideal gas equation hmangin tuak a si:
Cu hna lakah: \({n}_{i}\): electrochemical thlennak ah electron zat. \(F\): Faraday's constant. \({C}_{i}\): HPLC ti chuahmi tlawmtam. \(V\): caan khiahmi t chung ah lakmi ti sample zat. \(j\): a tu lio a ritmi. \(A\): Electrode i a sining (25 cm2). \(t\): zohchunhnak caan. \(P\): a tlingmi hneknak. \({x}_{i}\): GC nih a khiahmi gas mole zatuak. \(R\): gas aa thleng lomi. \(T\): lumnak.
Anodic cations an tlawmtam ning cu inductively coupled plasma atomic emission spectroscopy (ICP-OES) hmangin tah a si. Anode chungah a luang khomi asiloah a karh khomi cations hna cu Ti, Pt, Bi le K an si. K ti lo ahcun, a dang cations vialte cu hmuh khawhnak ri tang ah an um. Anode kha protons asiloah a dang cations he i fonh dingin chiah in cawhmi chungah ions ser. Cucaah, formic acid a thianghlimnak cu hitihin tuak khawh a si
Formate/FA chuahmi nih hin MEA sining pakhatkhat hmangin hmanmi electric mei kWh pakhat ah chuahmi FA zat kha mol/kWh in a langhter. A hleiin riantuannak thil sining tangah a tu lio a tlawm le tam, cell voltage le Faraday tthatnak cung ah hram bunh in tuakmi a si.
A dihlak in a ritmi tlukruannak cung ah hram bunh in anode ah a chuakmi formic acid zat kha tuak. Cathode ah aa zuammi thil pathum a cang: hydrogen thlennak, CO2 in CO ah thlennak, le CO2 in formic acid ah thlennak. Anton ah formic acid oxidation kan ngeih caah, formic acid FE cu tthen hnih ah tthen khawh a si: formic acid laknak le formic acid oxidation. A dihlak in ritnak tlukruannak cu hitihin tial khawh a si:
HPLC nih a lakmi formic acid, hydrogen le CO zat tahnak caah GC kan hman. Formic acid tam deuh cu Supplementary Figure S5 ah langhtermi timhtuahnak hmangin anode chungin lakmi a si ti kha hngalh a herh. Cathode khaan chungin lakmi formate zat cu a biapi lo, a ngan ning pahnih tluk a tlawm deuh, cun SC dihlak zat 0.5% nak tlawm deuh a si.
Hika ah hmanmi pehzulh tein phorhnak model cu aa lo ngaimi system hna cung i a hlan i riantuannak cungah hram aa bunhmi a si34. Poisson-Nerst-Planck (PNP) tlukruannak aa pehtlaimi system cu electronic le ionic in a kalmi tthennak ah ti tlawmtam le electrostatic thazaang hngalh khawhnak caah hman a si. A tanglei equation le model geometry kong a tlingmi zohfelnak cu SI ah pek a si.
Hi system nih hin ti chung thilri pariat (\({{{{{{\rm{C}}}}}}}{{{{{\rm{O}}}}}}}_{2 \left ({{{{{\rm{aq}}}}}}\right)}\), \({{{{\rm{}}}}}\), \({{{{\rm{}}}}}}}}}}} an tlawmtam kha a khiah ({{{{{\rm{O}}}}}}{{{{{\rm{H}}}}}}{-}\), \({{{ {{{ \rm{ HCO}}}}}}}}_{3}^{-}\), \({{{{{{\rm{CO}}}}}}}_{{{{{\rm{CO}}}}}}}_{{{{{\rm{CO}}}}}}}}_{{{{\rm{CO}}}} ({{{{{\rm{HCOOH}}}}}}}\), \({{{{{{\rm{HCOO}}}}}}}}}^{- }\) le \({{{ {{{\rm{K}}}}}}^{+}\)), ionic conducting phase (\(\{I \{I \}) le anodic) le anodi hruai khawhnak. Electrostatic potentials cu phases (\({\phi }_{A}\) le \({\phi }_{C}\) ciocio ah an um. Cu nakin, hmunhma electric neutrality le charge phawtzamhnak riantuannak hna cu a tling lo, vancung charge region cu Poisson's equation hmangin direct in a phichuak a si; Hi lamthluan nih hin CEM|AEM, CEM|Pore, le AEM|Pore karlak ah Donnan hnuh khawhnak hna kha direct in model tuah khawhnak a kan pek. Cun, porous electrode theory (PET) cu catalyst i anodic le cathodic tthen chung i charge phurhnak kong chim awkah hman a si. Catialtu hna nih an theih khawh tawk ahcun, hi rian nih hin PET hmannak hmasa bik kha vancung charge pengtlang tampi a ngeimi system ah a aiawh.
GDE BOT le EOT cathode sample pawl cu Zeiss Xradia 800 Ultra 8.0 keV X-ray source, absorption le wide field modes, le image fusion1 hmangin hneksaknak an tuah hna. -90° in 90° tiang hmanthlak 901 cu second 50 chung langhternak caan he an lak hna. Remhnak cu 64 nm voxel size he hnulei thlennak filter hmangin tuah a si. A hleiin ttialmi code hmangin tthencheunak le particle ngan le hme tthencheunak hlathlainak tuah a si.
Electron microscopic sining langhternak ah hneksaknak MEAs kha epoxy resin ah khumh in diamond namte in a tlawm tukmi tthennak caah timhtuahnak ah aa tel. MEA pakhat cio i a tthencheunak cu 50 in 75 nm tiang a thukmi ah tan a si. Talos F200X transmission electron microscope (Thermo Fisher Scientific) cu scanning transmission electron microscopy (STEM) le energy-dispersive X-ray spectroscopy (EDS) tahnak caah hman a si. Microscope cu EDS Super-X system he aa thuam i windowless SDD hmuh khawhnak 4 a ngei i 200 kV in a rian a ttuan.
Powder X-ray diffraction patterns (PXRD) cu Bruker Advance D8 powder X-ray diffractometer ah Ni-filtered Cu Kα radiation 40 kV le 40 mA ah rian a ttuanmi ah hmuh a si. Hlathlainak cu 10° in 60° tiang a si, kedan ngan cu 0.005° a si, cun data laknak rangnak cu kedan pakhat ah second 1 a si.
Bi2O3 Bi L3 catalyst tthennak ah a ummi RAS spectrum cu inn ah sermi cell hmangin thil ti khawhnak riantuannak ah tah a si. Bi2O3 catalytic ionomer ink cu 26.1 mg Bi2O3 156.3 μL ionomer cawhnuk (6.68%) he cawh in 1 M KOH, ti (157 μL) le isopropyl alcohol (104 μL) in a tlawmter i ionomer ink hmuh khawhnak ding caah timhtuahnak a si. Catalyst coefficient cu 0.4 a si. Bi2O3 catalyst loading 0.5 mg/cm2 a phak tiang ink cu graphene sheets ah a tlarimi hmun (10×4 mm) ah an thuh. Graphene catlap a tangmi cu electrolyte in hi hmun pawl thleidan khawhnak ding caah Kapton in an thuh. Catalyst-coated graphene sheet cu PTFE pahnih karlak ah khumh a si i cell body (PEEK) ah hri in hren a si, Figure S8. Hg/HgO (1 M NaOH) cu zohchunh awk electrode ah a hman, cun carbon cauk cu counter electrode ah a hman. Hg/HgO zohchunhmi electrode cu hydrogen-saturated 0.1 M KOH chungah hnimhmi platinum hri hmangin tahmi thilti khawhnak vialte kha thlen khawhmi hydrogen electrode (RHE) tahfung ah thlen khawhnak ding caah tahfung an ser. XRD spectra cu 0.1 M KOH ah hnimh in 30 °C tiang lumtermi Bi2O3/graphene sheet riantuannak electrode a tthawnnak zohfelnak in hmuh a si. Electrolyte cu battery chungah a kal, electrolyte luhnak cu cell tang ah a um i a chuahnak cu a cunglei ah a um i cu nih cun bubble a chuah tikah electrolyte nih catalyst layer a tawngh khawh nakhnga a tuah. CH Instruments 760e potentiostat cu riantuanmi electrode thazaang uk khawhnak caah hman a si. Potential sequence cu a ongmi circuit potential a si: -100, -200, -300, -400, -500, -800, -850, -900, -1000, -1100, -1500 le +700 mV cu RHE cungah aa hngat. iR thilti khawhnak vialte cu remh an si cang.
Bi L3 edge (~13424 eV for Bi metal) X-ray absorption fine structure (XAFS) spectroscopy cu channel 10-ID, Advanced Photon Source (APS), Argonne National Fluorescence Laboratory ah tuah a si. Ram pumpi Model Tahnak Laboratory. X-ray thazaang thlennak caah nitrogen ti in lumtermi two-crystal Si(111) monochromator hman a si, cun harmonic content zorternak caah rhodium-coated mirror hman a si. Scan thazaang cu 13200 in 14400 eV tiang aa dang, cun ceunak cu 5 × 5 silicon PIN diode array hmangin filter asiloah Soller slits um loin tah a si. A pahnihnak chuahkehnak i a zero tannak thazaang cu Pt foil L2 tthennak in 13271.90 eV ah tah a si. Electrochemical cell a thuhnak ruangah, zohchunhmi tahfung spectrum kha caankhatte ah tah khawh a si lo. Cucaah, tuakmi scan-to-scan thlennak a cangmi X-ray thazaang cu hneksaknak chung vialte tahnak tuah tthanmi cungah hram bunh in ±0.015 eV a si. Bi2O3 tthen a thuhnak nih cun ceunak nih amah tein a lak khawhnak a tlawmter; electrode pawl nih a cangmi ceunak le hmuh khawhnak he pehtlai in a fekmi dirhmun an ngeih, cu nih cun zohfelnak vialte kha aa khat dih. Athena software (version 0.9.26) i linear combination fitting algorithm hmangin Bi le Bi2O3 standards XANES region he tahchunh in bismuth oxidation dirhmun le chemical form hngalh khawhnak ding caah near-field XAFS spectrum hman a si. code IFEFFIT 44 in.
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