JP2022501292A - 酸素の存在下で多孔質炭素中に固定化されたセレン、および二次電池中の固定化セレンの使用 - Google Patents
酸素の存在下で多孔質炭素中に固定化されたセレン、および二次電池中の固定化セレンの使用 Download PDFInfo
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- JP2022501292A JP2022501292A JP2020538795A JP2020538795A JP2022501292A JP 2022501292 A JP2022501292 A JP 2022501292A JP 2020538795 A JP2020538795 A JP 2020538795A JP 2020538795 A JP2020538795 A JP 2020538795A JP 2022501292 A JP2022501292 A JP 2022501292A
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- Prior art keywords
- selenium
- carbon
- immobilized
- oxygen
- lithium
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- 239000011669 selenium Substances 0.000 title claims abstract description 645
- 229910052711 selenium Inorganic materials 0.000 title claims abstract description 637
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 title claims abstract description 635
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims description 445
- 229910052799 carbon Inorganic materials 0.000 title claims description 325
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims description 98
- 229910052760 oxygen Inorganic materials 0.000 title claims description 96
- 239000001301 oxygen Substances 0.000 title claims description 96
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- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims 1
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims 1
- 238000010000 carbonizing Methods 0.000 claims 1
- 239000000834 fixative Substances 0.000 claims 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims 1
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims 1
- XTLOJJNLKXLMMJ-UHFFFAOYSA-N [Se].[C].[O] Chemical compound [Se].[C].[O] XTLOJJNLKXLMMJ-UHFFFAOYSA-N 0.000 abstract 1
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Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/002—Compounds containing, besides selenium or tellurium, more than one other element, with -O- and -OH not being considered as anions
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
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Abstract
Description
さらに、硫黄は絶縁体であり、導電性の最小レベルを達成するために高レベルの炭素材料の負荷レベルを必要とする。Li/Na−S二次電池は、硫黄の電気伝導率が極めて低いため、急速に放電または充電することが非常に困難である。
(A)セレン−炭素複合材料の調製
粉砕および製粉後、適当量のクエン酸カリウムを、不活性雰囲気下において800℃で5時間焼成し、室温まで冷却した。希塩酸で洗浄して中性pHにした。濾過して乾燥させ、二次元炭素ナノ材料(図1)を得た。50:50の質量比となるように、二次元炭素材料とセレンとを秤量し、次に、セレンのエタノール溶液と均一に撹拌および混合した。溶媒を蒸発させた後、乾燥オーブンで混合物を乾燥した。乾燥した混合物を240℃まで5℃/分で加熱し、そして、3時間均熱処理した。続いて、450℃まで5℃/分で昇温し続け、20時間均熱処理した。室温まで冷却して、セレン−炭素複合材料を得た。
上記調製されたSe−炭素複合材料を水と共にカーボンブラックSuperP(TIMCAL)およびバインダ(CMC/SBR(質量比1:1))と混合し、その後、パルプ化、コーティング、乾燥、およびその他の手順による定型の方式によって、セレン炭素複合材料カソードを得た。
上記で調製したSe−炭素複合材料カソード、アノードとしてのリチウム箔、セパレータとしてのセルガードダイヤフラム、電解質としての1MのLiPF6を含むEC/DMCにより、リチウムセレンコイン電池およびリチウムセレンパウチ電池(図4)が組み立てられた。
充放電装置を用いて、リチウムセレンコイン電池およびリチウムセレンパウチ電池の定電流充放電試験を行った。試験電圧範囲は1.0〜3.0Vであり、試験温度は25℃である。放電比容量および充放電電流のレベルは、セレンの質量に基づいて標準的に計算される。充放電電流は0.1Cまたは0.05Cである。リチウムセレンコイン充放電曲線は図2に示されており、具体的な試験結果は表1に示されている。リチウムセレンパウチ電池の試験結果は図5に示されている。
二次元炭素材料のために炭化される原材料としてクエン酸ナトリウムを用いたことを除いては、条件は実施例1と同様である。電池試験結果は以下の表1に示されている。
二次元炭素材料のために炭化される原材料としてグルコン酸カリウムを用いたことを除いては、条件は実施例1と同様である。電池試験結果は以下の表1に示されている。
炭素材料の高温炭化温度を650℃としたことを除いては、条件は実施例1と同様である。電池試験結果は以下の表1に示されている。
乾燥した混合物を5℃/分の加熱速度で300℃まで加熱し、この温度で3時間均熱処理したことを除いては、条件は実施例1と同様である。電池試験結果は以下の表1に示されている。
乾燥した混合物を5℃/分の加熱速度で240℃まで加熱し、この温度で3時間均熱処理した後、600℃まで加熱を続け、この一定温度で20時間均熱処理したことを除いては、条件は実施例1と同様である。電池試験結果は以下の表1に示されている。
リチウムセレン電池が、リチウムアノードシートに代え、リチウム化グラファイトアノードを組み込んでいることを除いては、条件は実施例1と同様である。電池試験結果は以下の表1に示されている。
リチウムセレン電池が、リチウムアノードシートに代え、リチウム化ケイ素炭素アノードを組み込んでいることを除いては、条件は実施例1と同様である。電池試験結果は以下の表1に示されている。
原材料としてポリアクリルニトリルを用いたことを除いては、条件は実施例1と同様である。電池試験結果は以下の表1に示されている。
セレンと炭素との複合材料を調製するために一段階の複合方法を使用したことを除いては、条件は実施例1と同様である。本例では、乾燥されたセレン炭素混合物を5℃/分の加熱速度で500℃まで加熱し、この温度で23時間均熱処理した。これにより、Se−炭素複合材料を得た。このようにして得たSe−炭素複合材料から作製した電池の充放電曲線は図3に示されている。電池試験結果は以下の表1に示されている。
走査電子顕微鏡(SEM)像を、エネルギー分散分析X線(EDX)検出器を備えたTescanVega走査電子顕微鏡で収集した。
第一の残渣を形成するために、260gのクエン酸カリウム充填物をるつぼに入れ、該るつぼを管状炉内の石英管に入れた。アルゴンガス流を炉に流し、炉を室温(〜20−22℃)から600℃まで5℃/分で昇温した。炉をその温度で60分間保持した後、炉を停止して炉が冷めてから管から充填物を取り出し、174.10gの処理された残渣を得た。第2処理残渣および第3処理残渣を形成するために、第1残渣に関わる記載と同じ工程を、420gおよび974gのクエン酸カリウムの充填物について、別々に繰り返した。得られた第2および第3の処理残渣は、それぞれ282.83gおよび651.93gであった。
0.1206グラムのセレン(セレンのバルク特性を示す)を一組のメノウ製乳鉢および乳棒に加れ、実施例9に従って調製された炭素骨格0.1206グラムを同じメノウ製乳鉢および乳棒に加えた。セレンと炭素骨格の混合物を手動で約30分間で粉砕し、セレンと炭素骨格との粉砕した混合物をステンレス鋼の金型(直径10mm)に移した。金型中の混合物を約10MPaの圧力でプレスし、混合物のペレットを形成した。次に、不活性環境(アルゴン)の存在下で密封容器にペレットを充填し、ペレットを含む密封容器をオーブンに入れた。ペレットが入れられた密封容器を入れたオーブンを、例えば12時間にわたり240℃(セレンの融点以上)で加熱する。セレンの融解温度を超え、セレンおよび炭素が部分的または完全に反応する、本出願に記載された特徴の一部または全部を有する固定化セレンを形成させるのに十分な時間および温度の任意の組み合わせが、想定ではあるが、使用された。次に、ペレットを室温に戻した後、容器からペレットを取り出す。取り出されたペレットは、本実施例10の固定化セレンである。
乳鉢および乳棒に、以下の材料が準備された。
実施例10に従って調製した固定化セレン56mg、SuperP7.04mg、カルボキシメチルセルロース(CMC)溶液182μL(CMC溶液52μLごとに乾燥CMC1mgを含む)、SBRラテックス分散液21.126μL(SBRラテックス分散液6.036μLごとに乾燥SBRラテックス1mgを含む)、および純水200μL。粒子、バインダ、および水を手で30分間撹拌することによりスラリーとし、カソードスラリーが調整された。次いで、カソードスラリーを、導電性基材片、例えば、箔の片側に塗布し、空気乾燥した。一実施形態では、導電性基材または箔は、アルミニウム(Al)箔であってもよい。しかし、これは、任意の形状または形態の任意の適切なおよび/または望ましい導電性材料の使用が想定されるので、限定的な意味で解釈されるべきではない。説明のみを目的として、セレンカソードを形成するためのAl箔の使用を本明細書に記載する。しかし、これは限定的な意味で解釈されるべきではない。
実施例11のカソードディスクを用いて、次の実施例にて説明する図15に示す方法で、リチウム−セレンコイン型セル二次電池を組み立てた。この例では、実施例11の直径10mmのカソードディスク4を、コイン電池の正のケース(図15の「正のケース」)として機能する2032ステンレススチールコイン電池の基部2上に固定化セレンシート5を正のケースの基部2から離して上方に向けて配置し、ベアアルミニウム側を、正のケースの基部2と対向させ接触させた。次に、直径19mm、厚さ25ミクロンの電池セパレータ6を、固定化セレンシート5と接触した状態でカソードディスク4の上に配置した。一実施形態では、電池セパレータ6は、有機セパレータ、無機セパレータ、または固体電解質セパレータであってもよい。有機セパレータは、ポリマー、例えば、ポリエチレン、ポリプロピレン、ポリエステル、ハロゲン化ポリマー、ポリエーテル、ポリケトンなどであり得る。無機セパレータは、ガラスおよび/または石英繊維から作製され得る。
(a)乾燥または湿潤条件下でのセレンと炭素の混合、
(b)工程(a)の混合物の高温での任意の乾燥、
(c)工程(b)の乾燥混合物の任意のペレット化、
(d)固定化セレンを調製するためにセレンを炭素に融解させること。
(a)乾燥または湿潤条件下でのセレンと炭素の混合、
(b)工程(a)の混合物の高温での任意の乾燥、
(c)工程(b)の乾燥混合物の任意のペレット化、
(d)固定化セレンを調製するためにセレンを炭素に融解させること。
実施例10に記載された原理および手順に従い、セレン5原子%(at%)、セレン20原子%、セレン35原子%、およびセレン50原子%を、以下の表4に詳述する硫黄ドープされた固定化セレンの合成において、それぞれ硫黄で置換した。硫黄がドープされた固定化セレンの試料を、実施例9に記載の原理および手順に従って調製した炭素骨格を用いて合成した。
本明細書に記載される炭素材料は、以下の工程を含む調製方法から得ることができる。
(1)異なる成分(不活性塩、活性化剤、および炭素前駆体)を混合する。本混合工程は、ボールミル粉砕工程または異なる成分の溶液の凍結乾燥工程を含むことができる。
(2)混合物を不活性雰囲気下において高温で炭化する。次いで熱湯で洗浄して無機塩を除去し、そして乾燥して、相互接続した湾曲した薄い炭素層を含む3D多孔質材料を得る。
工程(1)において、不活性塩は、塩化カリウム、塩化ナトリウム、または炭酸ナトリウムから選択され得る。活性化剤は、炭酸カリウム、重炭酸カリウム、またはシュウ酸カリウムから選択することができる。炭素前駆体は、上記の再生可能な炭素源から選択することができる。工程(2)において、高温炭化は、800−900℃、望ましくは800−850℃で行い得、炭化時間は1−8時間、望ましくは1−4時間で行い得る。
Claims (11)
- 固定化セレン体を調製する方法であって、
(a)セレン、炭素、および酸素の混合物を形成すること、
(b)前記工程(a)の前記混合物をセレンの融点よりも高い温度まで加熱すること、および、
(c)前記工程(b)の加熱された前記混合物を周囲温度または室温まで冷却し、それにより固定化セレン体を形成すること、
を含む方法。 - 前記炭素は、自己テンプレート型炭素または外来テンプレート型炭素のいずれかである、請求項1に記載の方法。
- 前記炭素中の50%以下のセレンローディングに対して、前記混合物中の酸素量が0.63ミリモル/グラム以上である、請求項1に記載の方法。
- 前記炭素中の50%(含まない)〜60%(含む)のセレンローディング(すなわち、50%<セレンローディング≦60%)に対して、前記混合物中の酸素量が0.5ミリモル/グラム以上である、請求項1に記載の方法。
- 前記炭素中の60%以上のセレンローディングに対して、前記混合物中の酸素量が0.31ミリモル/グラム以上である、請求項1記載の方法。
- 前記工程(a)の前に前記炭素を活性化し、それにより前記炭素に細孔を形成することをさらに含む、請求項1に記載の方法。
- 前記活性された炭素を、酸化剤と組み合わせることまたは酸化剤と混合すること、をさらに含む、請求項5に記載の方法。
- 前記酸化剤が以下の少なくとも1つを含む、請求項7に記載の方法。
硝酸、
過酸化水素、
有機過酸化物、
酸素、および/または
オゾン。 - 前記酸化剤が、水性環境において以下の少なくとも1つを含む、請求項7に記載の方法。
過硫酸アンモニウム、
過硫酸ナトリウム、
過硫酸カリウム、
マンガンの塩、
バナジウムの塩、および/または
クロムの塩。 - 前記自己テンプレート型炭素が、以下を含むプロセスによって作製される、請求項1に記載の方法。
溶融物中のアニオンの過飽和が溶融物中で結晶化された塩を形成するまで、溶融により塩を炭化すること、
前記溶融物が結晶化塩の結晶子の表面を被覆するまで、前記溶融物の粘度を増加させること、および、
前記結晶子表面上の前記溶融物中の炭素を凝固させること。 - セレン、炭素、および酸素の混合物を含む固定化セレン体。
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