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摘 要: 本文對(duì)鋰離子電池中硅碳負(fù)極材料的納米結(jié)構(gòu)、摻雜改性以及三元復(fù)合材料的電化學(xué)性能及相關(guān)機(jī)理進(jìn)行了總結(jié)，目的是研究不同改性方法對(duì)硅碳負(fù)極材料的電化學(xué)性能的影響，以找到較為優(yōu)異的硅碳負(fù)極改性方法.經(jīng)過(guò)對(duì)比我們發(fā)現(xiàn)，在已被研究的各種硅碳負(fù)極材料中，通過(guò)采用納米結(jié)構(gòu)、雜原子摻雜以及三元復(fù)合的方法均可顯著提升硅碳負(fù)極材料的電化學(xué)性能.后對(duì)硅碳負(fù)極材料發(fā)展現(xiàn)狀進(jìn)行了簡(jiǎn)要分析，并對(duì)其研究前景進(jìn)行了展望.

目錄：

1 硅碳負(fù)極材料的合成

2 硅碳負(fù)極材料

3 摻雜型硅碳負(fù)極材料

4 展望

隨著能源技術(shù)的更新?lián)Q代，在電子、可再生能源系統(tǒng)和電動(dòng)汽車(chē)等各個(gè)領(lǐng)域，滿(mǎn)足日益增長(zhǎng)的能源需求越來(lái)越迫切.鋰離子電池因其具有較高的容量和穩(wěn)定的循環(huán)壽命，被認(rèn)為是滿(mǎn)足便攜式電子器件、電動(dòng)及混合動(dòng)力汽車(chē)日益增加的能源需求的新型電源[1-4].在不同負(fù)極材料中，硅的理論比容量(高可達(dá)4 200 mA&dot;h g-1)是傳統(tǒng)碳負(fù)極理論比容量(約372 mA&dot;h g-1)的10倍，這吸引了極大的關(guān)注，且硅較低的脫嵌鋰電位(<0.5 V vs. Li/Li+)使得鋰離子電池能獲得更高的功率[5].但是，由于硅負(fù)極材料較低的導(dǎo)電性和嚴(yán)重的體積膨脹(>300%)，硅顆粒發(fā)生開(kāi)裂和粉碎，因?yàn)榛钚圆牧系膿p耗和不良的電接觸導(dǎo)致了緩慢的動(dòng)力學(xué)性能和短暫的循環(huán)壽命，故硅負(fù)極材料在鋰電池中的應(yīng)用并不可觀(guān)[6].納米管、納米線(xiàn)、納米棒、納米片、多孔、中空或帶防護(hù)涂層的封裝硅顆粒等硅納米結(jié)構(gòu)通常應(yīng)用于硅基負(fù)極材料的改善結(jié)構(gòu)和電學(xué)性能結(jié)構(gòu)[7-8].另外，制備這些納米結(jié)構(gòu)的方法(如氣-液-固法，磁控濺射和化學(xué)氣相沉積)都有技術(shù)復(fù)雜和步驟多等缺點(diǎn)[9-10].石墨和多孔碳因在鋰化過(guò)程中體積變化相對(duì)較小(如石墨的體積膨脹率僅為10.6%)且具有良好的循環(huán)穩(wěn)定性和電導(dǎo)率而成為極具潛力的負(fù)極材料.與硅材料相比，碳材料具有與其相似的性質(zhì)，且它們可以緊密結(jié)合，所以碳材料自然地被選為用于分散硅顆粒的襯底材料(即分散載體)[11-12].通過(guò)硅碳復(fù)合，鋰離子電池可獲得更高的比容量、更好的導(dǎo)電性與循環(huán)穩(wěn)定性 [13].

本文主要研究了各種鋰離子電池硅碳復(fù)合負(fù)極材料的合成、結(jié)構(gòu)和電化學(xué)性能，綜述了硅碳負(fù)極材料的研究現(xiàn)狀.

1 硅碳負(fù)極材料的合成

1.1氣相沉積法

氣相沉積法包括化學(xué)氣相沉積法(CVD)和物理氣相沉積法(PVD).CVD是一種用于生產(chǎn)高質(zhì)量、高性能的固體材料的化學(xué)過(guò)程，這個(gè)方法通常應(yīng)用于半導(dǎo)體領(lǐng)域的薄膜制造.PVD是一種真空沉積法，可以用來(lái)制作薄膜和涂層.PVD是材料從凝聚態(tài)轉(zhuǎn)變?yōu)闅鈶B(tài)，然后再轉(zhuǎn)變?yōu)槟�聚態(tài)薄膜的一個(gè)過(guò)程.常見(jiàn)的PVD過(guò)程是濺射和蒸發(fā).PVD常用于制造具有機(jī)械、光學(xué)、化學(xué)或電學(xué)性能的薄膜 [14].

1.2高溫固相合成

高溫固相合成是一種在高溫(1 000～1 500 ℃ )下，通過(guò)固體界面之間的接觸、反應(yīng)、成核和晶體生長(zhǎng)反應(yīng)生成大量的復(fù)合氧化物的方法.高溫固相合成應(yīng)是制備硅碳復(fù)合材料一種常用方法，為了防止惰性相硅碳的生成，反應(yīng)溫度通�？刂圃�1200 ℃ [15].在反應(yīng)過(guò)程中，溫升速率、反應(yīng)前驅(qū)物的選擇和反應(yīng)溫度的高低將直接影響材料的結(jié)構(gòu)和性能.高溫固相合成技術(shù)因工藝簡(jiǎn)單，工藝參數(shù)易于控制，重現(xiàn)性好而被廣泛應(yīng)用.

1.3機(jī)械合金化

與高溫固相合成法相反，機(jī)械合金化法制備的材料通常具有更小的粒度，更大的比表面積和更均勻的組織[16].機(jī)械合金化是一種固態(tài)粉末加工技術(shù)，涉及重復(fù)冷焊、壓裂和在高能球磨機(jī)中重新焊接混合粉末粒子，從而獲得均勻材料的方法，已被證明能夠從混合元素或預(yù)合金粉末中合成各種平衡和非平衡合金相[17].

1.4靜電紡絲

靜電紡絲是一種利用靜電來(lái)噴射聚合物溶液或聚合物的帶電細(xì)絲的纖維生產(chǎn)方法，其直徑一般為幾百納米.靜電紡絲技術(shù)融合了電噴涂和傳統(tǒng)的溶液干法紡絲纖維的優(yōu)點(diǎn)[18].該過(guò)程不需要使用化學(xué)凝固或高溫來(lái)從溶液中產(chǎn)生紡絲，這使得該工藝特別適用于大而復(fù)雜的微粒生產(chǎn)纖維 [19-20].靜電紡絲技術(shù)是可利用各種材料制備納米纖維的一種低成本、工藝簡(jiǎn)單的通用方法，改進(jìn)工藝后的同軸靜電紡絲技術(shù)可制備納米管和核殼結(jié)構(gòu)納米纖維[21].

2 硅碳負(fù)極材料

碳納米材料因其獨(dú)特的性能而有著許多技術(shù)應(yīng)用，包括輕量化構(gòu)造、電子、能源、環(huán)保、醫(yī)藥等領(lǐng)域[22-23].納米材料的物理和化學(xué)性能不同于普通材料甚至更優(yōu)于普通材料，這些優(yōu)異的性能通常由材料組織的微結(jié)構(gòu)決定[24-25].碳材料因其良好的機(jī)械特性，高導(dǎo)電性和化學(xué)穩(wěn)定性，在無(wú)黏結(jié)劑電極和輕質(zhì)電極研究領(lǐng)域備受關(guān)注.近年來(lái)，納米線(xiàn)、納米纖維、納米管、納米球等硅碳納米結(jié)構(gòu)經(jīng)常被應(yīng)用于鋰離子電池中.

2.1硅碳納米線(xiàn)

納米線(xiàn)是納米級(jí)應(yīng)用的一種，產(chǎn)業(yè)化的納米線(xiàn)直徑分布在50～100 nm[26].圖1為碳硅核殼納米線(xiàn)的SEM形貌. 將非晶硅包覆在碳納米線(xiàn)上制備的碳硅核殼納米線(xiàn)材料[27]作為高功率和長(zhǎng)壽命鋰電池負(fù)極的容量可達(dá)2 000 mA&dot;h g-1且具有良好的循環(huán)壽命.

圖1 碳硅核殼納米線(xiàn)的SEM形貌[27]

Fig.1 SEM image of C-Si NWs after 5 cycles [27]

該材料初始庫(kù)倫效率為90%，隨后周期的庫(kù)倫效率仍高達(dá)98%～99.6%.研究發(fā)現(xiàn)，均勻和完整的碳涂層可以緩解硅納米線(xiàn)完全鋰化產(chǎn)生的膨脹. 催化生長(zhǎng)的碳納米纖維(CNFs)的應(yīng)用已經(jīng)有十幾年.碳納米纖維已經(jīng)產(chǎn)業(yè)化，且具有良好的機(jī)械強(qiáng)度，高的導(dǎo)熱性和導(dǎo)電性[28,29].混合納米結(jié)構(gòu)Si/CNFs負(fù)極在比容量和循環(huán)壽命方面表現(xiàn)出優(yōu)越的性能.碳納米纖維不僅提供了良好的應(yīng)變/應(yīng)力松弛層，而且還提供了電子的傳輸途徑[30-31].

2.2 硅碳納米纖維

Shu等[32]利用CVD法研制了空心CNFs/Si復(fù)合材料，所得的負(fù)極材料具有優(yōu)異的倍率特性.在0.6 C下，CNFs/Si電極的初始放/充電容量分別為1 197.8和941.4 mA&dot;h g-1，循環(huán)20周期后的可逆充電容量為733.9 mA&dot;h g-1，其容量保持率高達(dá)77.9%.CNFs/Si負(fù)極材料表現(xiàn)出優(yōu)異的電化學(xué)性能，其不僅提供硅顆粒之間的導(dǎo)電橋和集電器，也作為一個(gè)抑制硅顆粒體積膨脹的緩沖區(qū).

圖2 純硅與CNFs/Si循環(huán)前后電極結(jié)構(gòu)比較[32].

Fig.2 Comparison of pure Si and CNFs/Si electrodes before and after cycling[32].

2.3硅碳納米管

近年，許多研究熱點(diǎn)都集中在基于碳納米管的鋰電池負(fù)極材料的制備上[33].以往關(guān)于含碳納米管的硅負(fù)極材料的研究主要集中在通過(guò)簡(jiǎn)單的機(jī)械混合、碳納米管在硅材料上的生長(zhǎng)、碳納米管表面硅原子的植入或者在碳納米管薄膜上沉積硅以形成Si/CNT薄膜等來(lái)使硅與碳納米管外表面產(chǎn)生電子連接.但是，由于硅顆粒的不均勻分布，碳納米管的約束效應(yīng)并不令人滿(mǎn)意，使硅在納米空間內(nèi)并沒(méi)有收到碳納米管網(wǎng)絡(luò)的足夠約束[34].Zhao等[35]采用CVD法原位合成了一種硅/非晶碳納米管核殼復(fù)合負(fù)極材料(Si/ACNT).在100 mA g-1下，該電極容量可達(dá)1496 mA&dot;h g-1，在300個(gè)循環(huán)周期后仍有80%容量保持率，具有良好的循環(huán)穩(wěn)定性.

圖 3 不同尺寸的Si/ACNT復(fù)合材料的TEM圖[35]

Fig.3 TEM images of different microstructure size of the Si/ACNT composite [35]

2.4 硅碳納米球

碳納米球由石墨結(jié)構(gòu)中分布不連續(xù)的玻璃態(tài)石墨層組成[36].由于碳納米球具有高比表面積，良好的化學(xué)穩(wěn)定性和熱穩(wěn)定性等特性，其可以用于制備高強(qiáng)度高密度的碳/碳復(fù)合材料、液相色譜柱、高比表面積活性炭材料、鋰電池負(fù)極材料以及一系列高性能碳材料.碳微球具有很強(qiáng)的吸附能力，可以重復(fù)利用[37-38].

圖4 化學(xué)還原后及未進(jìn)行化學(xué)還原的不同尺寸下的Si/C復(fù)合材料的TEM圖[39]

Fig.4 TEM images of different microstructure size of Si/carbon nanospheres composite [39]

Zhou等[39]用簡(jiǎn)單的化學(xué)方法制備了硅/碳納米球.通過(guò)熱處理，硅顆粒被非晶碳包覆，從而抑制了原始硅的集聚，緩解了硅在循環(huán)過(guò)程中巨大的體積膨脹.在200 mA g-1下，該材料的初始可逆容量為888.6 mA&dot;h g-1.在50次循環(huán)后，電極的充電容量仍有610.7 mA&dot;h g-1.在鋰化過(guò)程中，硅碳微球能有效地緩沖硅納米顆粒的體積膨脹/收縮，具有優(yōu)異的電化學(xué)性能和循環(huán)穩(wěn)定性.

3 摻雜型硅碳負(fù)極材料

在摻雜型硅碳負(fù)極材料中，硅和碳緊密地結(jié)合形成了一個(gè)穩(wěn)定均勻的系統(tǒng).在充放電過(guò)程中，硅原子作為電化學(xué)反應(yīng)的活性中心，碳原子作為鋰化的載體.另外，碳載體還可作為電子傳輸通道和支撐結(jié)構(gòu).

3.1氮摻雜型硅/碳負(fù)極材料

由于氮摻雜所造成的缺陷，氮摻雜的碳具有較高的導(dǎo)電性和電化學(xué)活性，并有助于界面中鋰離子的傳輸[40].氮摻雜層可以防止電極材料與電解液的直接接觸且可提高復(fù)合材料和鋰離子在電極和電解液界面上傳輸速率[41].氮摻雜的碳涂層在促進(jìn)和保持穩(wěn)定的SEI層中提供了一個(gè)有效的電子傳輸途徑，促進(jìn)了脫嵌鋰反應(yīng) [42].此外，研究發(fā)現(xiàn)摻雜氮的碳涂層比原始碳涂層有著更高的導(dǎo)電性和鋰離子遷移率[43-44].

Shen等[45]將用離子液體輔助制備的硅@氮摻雜碳(Si@NC)納米顆粒與硅@碳(Si@C)納米顆粒進(jìn)行比較.在420 mA g-1下，經(jīng)過(guò)100次循環(huán)后，所制備的Si@NC復(fù)合材料表現(xiàn)出較高的可逆容量，約為725 mA&dot;h g-1，是同種方法制備的Si@C材料的兩倍(360 mA&dot;h g-1).該材料改進(jìn)的電化學(xué)性能得益于納米復(fù)合材料穩(wěn)定的核殼結(jié)構(gòu)，更重要的是氮元素?fù)诫s到碳?xì)ぶ?包覆的氮摻雜碳層不僅改善了材料的導(dǎo)電性，且緩解了鋰化過(guò)程體積膨脹產(chǎn)生的應(yīng)力.

圖5 不同電流密度下，Si@N-C、Si@C和Si納米顆粒的循環(huán)性能 [45].

Fig.5 Cycling performance and rate capability of Si@N-doped carbon, Si@C and Si nanoparticles at different current density [45]

3.2硅/碳/石墨負(fù)極材料

硅負(fù)極材料大的缺陷是當(dāng)硅大鋰化時(shí)，其體積膨脹率高達(dá)300%[46].減少硅體積膨脹效應(yīng)，并充分利用硅超高可逆容量的一種方法是將石墨與其結(jié)合[47].石墨因其良好穩(wěn)定性、低成本、低工作電壓等優(yōu)點(diǎn)成為了新型復(fù)合負(fù)極材料的理想選擇[48].石墨、碳和硅復(fù)合材料可提供可觀(guān)的可逆容量，并可有效減少負(fù)極材料的體積膨脹[49].

Wang等[50]通過(guò)噴霧干燥自組裝法將熱解碳和天然石墨(NG)包覆在亞微米硅片上成功制備了Si/C@NGs復(fù)合材料.該材料的初始昆侖效率高達(dá)82.8%，在0.1 A g-1下循環(huán)100個(gè)周期后仍有1524.0 mAh g-1的容量保留，這種層級(jí)結(jié)構(gòu)的材料與純硅相比有著多層碳涂層和空隙，有效地緩解了硅充放電過(guò)程中的體積膨脹.

圖6 天然石墨顆粒、Si / SAN@NGs、碳化后Si / C@NGs和Si / C@NGs復(fù)合截面的SEM圖 [50].

Fig.6 SEM images of NG particles, Si/SAN@NGs composite, Si/C@NGs composite after carbonization and cross profile of Si/C@NGs composite, respectively[50].

3.3硅/碳/石墨烯負(fù)極材料

近年來(lái)，石墨烯由于具有高導(dǎo)電性、高強(qiáng)度、高化學(xué)穩(wěn)定性、超高的比表面積和開(kāi)放的多孔結(jié)構(gòu)等特性，具有對(duì)鋰電池電極材料體積變化的靈活約束作用，被認(rèn)為是有前景的碳材料[51].由于大比表面積、高導(dǎo)電性和良好的放電能力，石墨烯可以提高硅基復(fù)合電極的電化學(xué)性能，改善了大電流密度下的循環(huán)穩(wěn)定性，是一種極具吸引力的碳材料[52-53].

Pan等[54]采用工業(yè)通用的噴霧干燥法和隨后的煅燒工藝制備了硅@碳@石墨烯球形微結(jié)構(gòu)復(fù)合材料(Si@C@RGO).碳?xì)ず腿嵝允�墨烯的結(jié)合可有效提高復(fù)合材料的電導(dǎo)率，并可適應(yīng)硅在循環(huán)過(guò)程中巨大的體積變化.在100 mA g-1的低電流密度下，該種材料的初始可逆性為1 599 mA&dot;h g-1，當(dāng)在200 mA g-1下循環(huán)多次后的容量保持率高達(dá)94.9%.此外，即使在2 000 mA g-1的高電流密度下，Si@C@RGO負(fù)極也仍有951 mA&dot;h g-1的高可逆比容量.研究證明，石墨烯是一種防止硅在脫嵌鋰過(guò)程中結(jié)構(gòu)變化的有效緩沖元素，且可極大地提高鋰電池的可逆容量、循環(huán)穩(wěn)定性和倍率特性[55].

圖7 Si@C和Si@C@RGO復(fù)合材料電化學(xué)性能比較 [54]

Fig.7 Comparision of the electrochemical performance of Si@C and Si@C@RGO composite[54]

4 展 望

一般來(lái)說(shuō)，對(duì)硅碳負(fù)極材料的研究主要是針對(duì)更高能量密度、更大充放電性能、更高循環(huán)穩(wěn)定性和更高安全性鋰離子電池方面的發(fā)展.表面涂覆改性是電極材料制備的基本工藝，可提高材料加工性能，提高電解質(zhì)的相容性，降低不可逆容量，提高初始庫(kù)侖效率.對(duì)材料的比例和循環(huán)性能的改進(jìn)研究主要集中在用摻雜、改性或噴霧干燥等方法對(duì)材料進(jìn)行納米化，提高電子和離子的傳輸速率以改善材料的導(dǎo)電性和穩(wěn)定性.具有良好的機(jī)械彈性、高電導(dǎo)率和化學(xué)穩(wěn)定性的碳材料在鋰離子電池硅碳負(fù)極材料的發(fā)展中具有巨大的潛力.此外，對(duì)于鋰離子電池硅碳負(fù)極材料脫嵌鋰機(jī)理的研究，以及與硅碳材料更相容的粘結(jié)劑和電解液的探索，也是未來(lái)50年的研究熱點(diǎn).

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原標(biāo)題:鋰離子電池硅碳負(fù)極材料的制備與應(yīng)用