JP2016106370A - 新しい高表面伝導率電極材料 - Google Patents
新しい高表面伝導率電極材料 Download PDFInfo
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- JP2016106370A JP2016106370A JP2016028381A JP2016028381A JP2016106370A JP 2016106370 A JP2016106370 A JP 2016106370A JP 2016028381 A JP2016028381 A JP 2016028381A JP 2016028381 A JP2016028381 A JP 2016028381A JP 2016106370 A JP2016106370 A JP 2016106370A
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- Prior art keywords
- carbon
- electrode
- lithium
- polymer
- carbonaceous
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- 239000000463 material Substances 0.000 abstract description 59
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- 239000002245 particle Substances 0.000 abstract description 30
- 229910052760 oxygen Inorganic materials 0.000 abstract description 28
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 27
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 26
- 239000001301 oxygen Substances 0.000 abstract description 26
- 239000003792 electrolyte Substances 0.000 abstract description 23
- 239000003575 carbonaceous material Substances 0.000 abstract description 22
- 150000002500 ions Chemical class 0.000 abstract description 14
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- 239000002184 metal Substances 0.000 abstract description 10
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- 238000009826 distribution Methods 0.000 abstract description 6
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- HNCXPJFPCAYUGJ-UHFFFAOYSA-N dilithium bis(trifluoromethylsulfonyl)azanide Chemical compound [Li+].[Li+].FC(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)F.FC(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)F HNCXPJFPCAYUGJ-UHFFFAOYSA-N 0.000 description 14
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- TZIHFWKZFHZASV-UHFFFAOYSA-N methyl formate Chemical compound COC=O TZIHFWKZFHZASV-UHFFFAOYSA-N 0.000 description 4
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- CSHWQDPOILHKBI-UHFFFAOYSA-N peryrene Natural products C1=CC(C2=CC=CC=3C2=C2C=CC=3)=C3C2=CC=CC3=C1 CSHWQDPOILHKBI-UHFFFAOYSA-N 0.000 description 4
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
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Images
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
-
- 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
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/44—Raw materials therefor, e.g. resins or coal
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/48—Conductive polymers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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Abstract
Description
Aは、アルカリ金属を含み、
Mは、少なくとも1種の遷移金属、及び随意に少なくとも1種の非遷移金属、例えばマグネシウム又はアルミニウム、並びにそれらの混合物を含み、
Zは、少なくとも1種の非金属を含み、
Oは酸素、Nは窒素、且つFはフッ素である。
また、係数a、m、z、o、n、fはそれぞれ0以上であり且つ電気的中性を確実にするように選択する。ここで、伝導性炭質材料は前記材料の表面に均一に堆積させて、この材料の粒子表面において実質的に規則的な電場分布を得る。酸素、フッ素、及び窒素のイオン半径が同様であるので、電気的な中性が維持される限り、これらの元素の相互置換が可能になる。単純化のために及び酸素が最も頻繁に使用される元素であることを考慮して、これらの電極材料は複合酸化物と呼ぶ。好ましい遷移金属は、鉄、マンガン、バナジウム、チタン、モリブデン、ニオブ、タングステン、亜鉛、及びそれらの混合物を含む。好ましい非遷移金属は、マグネシウム及びアルミニウムを含む。好ましい非金属は、硫黄、セレン、リン、ヒ素、シリコン、ゲルマニウム、ホウ素、及びそれらの混合物を含む。
Aは、Li、Na、又はKのようなアルカリ金属を含み、
Mは、少なくとも1種の遷移金属、及び随意に、マグネシウム又はアルミニウムのような少なくとも1種の非遷移金属、又はそれらの混合物を含み、
Zは、S、Se、P、As、Si、Ge、Bのような少なくとも1種の非金属を含み、
Oは酸素であり、
Nは窒素であり、そしてFはフッ素であり、ここで、これらの元素は、F−、O2−、及びN3−のイオン半径が同様であるので、複合酸化物中の酸素を置換することができ、また
それぞれの係数a、m、z、o、n、及びfはそれぞれ独立に0以上で、この材料の電気的中性を確実にする。
C+O2 ←→ CO2
InP(O2)=InP(CO2)=94050/{R(273.2+θ)}
ここで、Rは理想気体定数(1,987cal・mol−1・K−1)であり、
θは温度(℃)である。
2CO ←→ C+CO2
Aa’MmZzOoNnFf + Aa−a’CcOoR’
→ AaMmZzOoNnFf
ここで、R’は有機ラジカルであり、ポリマー鎖の一部である
CY−CY + 2e− → −C=C− + 2Y−
ここで、Yはハロゲン又は疑似(pseudo−)ハロゲンを示している。ここでこの疑似ハロゲンという用語は、イオンY− の形で存在することができる有機又は無機ラジカルであって、対応するプロトン化化合物HYを作ることができるものを意味している。ハロゲン及び疑似ハロゲンの例としては、F、Cl、Br、I、CN、SCN、CNO、OH、N3、RCO2、RSO3を挙げることができ、ここでRはH又は有機ラジカルである。CY結合の還元による形成は、還元元素の存在下で行うことが好ましい。この還元元素としては、水素、亜鉛、マグネシウム、Ti3+イオン、Ti2+イオン、Sm2+イオン、Cr2+イオン、V2+イオン、テトラキス(ジアルキルアミノエチレン)、又はホスフィン類を挙げることができる。これらの試薬は、電気化学的に再生すること又は得ることができる。更に、還元速度を増加させる触媒を使用することも有利である。パラジウム又はニッケルの誘導体類は、特に2,2’−ビピリジンのような窒素化合物類又はリン化合物類との錯体の形で、効果的である。同様に、これらの化合物は、上述のような還元剤の存在下で活性な形で化学的に又は電気化学的にもたらすことができる。還元によってカーボンをもたらすことができる化合物類としては、ペルハロゲン化炭素類、特にポリマーの形のペルハロゲン化炭素類、ヘキサクロロブタジエン、及びヘキサクロロシクロペンタジエンを挙げることができる。
−CH−CY− + B → −C=C− + BHY
この例は、炭質堆積物でコーティングされた挿入材料を直接にもたらす本発明の材料の合成を説明する。
Fe3(PO4)2・8H2O + Li3PO4
→ 3LiFePO4
調製した材料を、室温及び80℃においてCR2032タイプのボタン電池で試験した。
上述のようにして得た材料を、CR2032タイプのボタン電池で試験した。カソードは、活性材料の粉末とカーボンブラック(Ketjenblack(商標))とを混合して得て、電流コレクターとの電子交換を確実にし、分子量400,000のポリエチレンオキシドをバインダー及びイオン伝導体の両方として加える。重量による割合は、35:9:56である。アクリロニトリルを混合物に加えて、エチレンポリオキシドを溶解する。この混合物を均一化し、1.7cm2のステンレス鋼ディスクに注ぐ。カソードは減圧下で乾燥させ、ヘリウムの減圧雰囲気(H2O,O2が1vpm未満)のグローブボックスに輸送する。ニッケル基材に積層されたリチウムシート(27μm)をアノードとして使用する。ポリマー電解質は、分子量5,000,000のポリエチレンオキシド及びLiTFSI(リチウムビス−トリフルオロメタンスルホンイミド)を、オキシエチレン単位の酸素とリチウムとの比が20:1になる量で含む。
炭質堆積物でコーティングしたLiFePO4は室温でも試験した。この場合において、複合材カソードは、85:5:10の比で、活性材料、カーボンブラック、及びEPDM(好ましくはシクロヘキサンに溶解したEPDM)を混合することによって調製する。この混合物は、1.7m2のディスク状にしてステンレス鋼電流コレクター上に拡げ、減圧下で乾燥し、そしてヘリウム雰囲気のグローブボックスに維持する。上述のように、アノードとしてはリチウムを使用する。これら両方の電極は、Celgard(商標)多孔質膜によって分離する。使用した電解質は、γ−ブチロラクトン中のLiTFSIの0.8M溶液である。図6に示されるボルタンペログラム(voltamperograms)は、3〜3.8Vのゆっくりとしたボルタンメトリー(20mV・h−1)で室温において得た。そのような構成では、酸化及び還元の速度は80℃でよりもかなり低速であると考えられる。更に、バッテリーの電力は、サイクルを重ねるとゆっくりと減少する。他方で、理論容量全体が達成可能である。(第1サイクルで97.5%、第5サイクルで99.4%)。すなわち、サイクル(5サイクル)の間の損失なしに、可逆的な交換が可能である。電解質が結合ポリマーをよく濡らさずに、電解質の電極への浸透が不十分であることによって、このバッテリーの電力が小さくなることは除外されない。
この例は、炭化水素ガスからの伝導性炭質堆積物の形成を示している。ポリプロピレン粉末を添加せず、熱処理不活性雰囲気を窒素中の1%プロペンの混合物で置き換えて、リチウム鉄ホスフェートの調製のために例1で説明される合成を繰り返す。熱処理の間に、プロペンは分解して、合成する材料上でカーボンの堆積物を作る。化学解析によれば、得られる試料は2.5%のカーボンを含んでいる。サイクルボルタンメトリーは、例1で説明されるのと同じ条件でこの試料に行い、1回目のサイクルでは重要な活性現象を示す(図6参照)。この場合においてレドックス反応速度の改良は、反復的な交換の容量の増加として達成される。放電工程の間の測定によれば、調製したLiFePO4試料の初期容量は、2.5%の電気化学的に不活性なカーボンを考慮に入れると、理論容量の77%である。5回目のサイクルの後では容量は91.4%に達する。観察される活性化現象は、粒子をコーティングしている多孔質のカーボン層厚さに関連し、またカチオンの拡散を遅らせることがある。
上述のように調製したトリフィライト試料LiFePO4を解析する。その質量分率は、Fe:34.6、Li:4.2%、P:19.2であり、これは化学量論量とは5%異なっている。
セルロースアセテートを、カーボンコーティング先駆物質として、例3のホスフェートLiFePO4に加える。このポリマーは、24%程度の高い炭化率で分解することが知られている。これは200℃〜400℃で分解する。これよりも高い温度では、アモルファスカーボンが転移してグラファイトタイプ構造を与える。このグラファイトタイプ構造は、付着する傾向があり、且つかなり伝導性のカーボン堆積物である。
ペリレン及びその誘導体類は、熱分解によって、グラファイト状タイプカーボンをもたらすことが知られている。これは開始分子中の縮合環の存在に起因している。特に、ペリレン−テトラカルボキン酸無水物は560℃以上で分解して、カーボンコーティングを提供する。しかしながら、この生成物の溶解性は低く、例3のLiFePO4 である複合酸化物との均一な混合は実施することが困難である。この問題を解決するために、エチレンポリオキシド鎖で離したペリレン基を含むポリマーを、第1の工程において調製した。オキシエチレン部分は、通常の有機溶媒類に芳香族基を溶解させる溶解剤として作用するのに十分に長くなるように選択する。従って、商業的な3,4,9,10−ペリレンテトラカルボン酸無水物(Aldrich)は、以下の反応に従って高温で、Jaffamine 600(Hunstmann)と反応させる。
ここで、R=−[CH(CH3)CH2O−]p(CH2CH2O−)q[CH2−CH(CH)3O]p−1CH2−CH(CH)3−
、であり、1≦p≦2、10≦n≦14である。
この例は、本発明の炭質堆積物をもたらすポリマーからの脱離反応の使用を説明している。
この例は、電極材料としての窒素含有化合物の使用を説明している。
「Nasicon」構造のリチウムバナジウム(III)ホスホシリケートLi3.5V2(PO4)2.5(SiO4)0.5を、以下のようにして調製した。
この例は、レドックス材料におけるアルカリ金属含有率の変化を伴う炭質コーティングの形成を説明している。
この例は、レドックス材料におけるアルカリ金属含有率の変化を伴う炭質コーティングの形成を説明している。
化合物LiCo0.75Mn0.25PO4は、空気中において10時間にわたって850℃で焼成することによって、微粉砕したコバルトオキサレート二水和物、マンガンオキサレート二水和物、及び二水素アンモニウムホスフェートから調製した。得られる藤色(mauve)粉末を、炭化タングステンボールと共に遊星ミルで粉砕して、平均粒度を4μmにした。10gのこの複合ホスフェートを、メチルホルメート中の例5のペリレンポリマーの6%溶液10mLと共に、すり鉢ですりつぶした。溶媒は素早く蒸発した。得られる粉末を、酸素を含まない乾燥したアルゴンの流れで、管状炉において740℃で3時間にわたって処理して、黒色の粉末を得た。このセルの電気化学活性は、例6と同様なリチウムイオンセルで試験した。この場合の電解質は、耐酸化性溶媒ジメチルアミノ−トリフルオロエチルスルファメートCF3CH2OSO2N(CH3)2に1Mの濃度で溶解したリチウムビス−フルオロメタンスルホンイミド(Li[FSO2]2N)である。最初に充電する場合、Li+:Li0に対して4.2〜4.95Vの電圧範囲で、セルの容量は145mAhg−1であった。バッテリーは50回の深い放電−充電サイクルでの容量の低下が10%未満であり、このことは高い電位に対する電解質の耐性を示している。
エタノール水の80:20混合物中のリチウムアセテート二水和物、マンガンアセテート四水和物、及びテトラエトキシシランの化学量論量混合物の反応によって得られるゲルをか焼することによって、化合物Li2MnSiO4を得た。ゲルは炉において80℃で48時間にわたって乾燥させ、粉末状にし、そして空気条件において800℃でか焼した。3.28gの得られるシリケート、及び例3からの12.62gのリチウム鉄ホスフェートを、例11と同様な遊星ミルでボールミル粉砕し、そして粉末を、6時間にわたって740℃の管状炉において酸素を含まない乾燥したアルゴン流れ条件で800℃で処理した。冷却の後で得られた複合酸化物の式はLi1.2Fe0.8Mn0.2P0.8Si0.2O4である。粉末は3mLの2%コバルトアセテート溶液で湿らせ、そして乾燥させた。2時間にわたって窒素中の10%の一酸化炭素の1mL/sの流れで、前記管状炉において500℃で、この粉末を処理した。冷却の後で、得られた黒色粉末の電気化学活性を、例1の条件と同じ条件で試験した。80℃のPEO電解質では、サイクリックボルタンメトリー曲線から測定した容量は、Li+:Li0に対して2.8〜3.9Vのカットオフ電圧で185mAhg−1(理論値の88%)であった。同様な条件において試験したコーティングされていない材料は、比容量が105mAhg−1であった。
アルゴン条件において、例3からの3gのリチウム鉄ホスフェートを50mLのアセトニトリル中に懸濁させ、そこに0.5gのヘキサクロロシクロペンタジエン及び10mgのテトラキス(トリフェニルホスフィン)ニッケル(0)を加えた。激しく撹拌しながら、室温において1.4mLのテトラキス(ジメチルアミノ)エチレンを滴状で加えた。溶液は青色に変化し、更に還元剤を加えると黒色になった。添加が完了した後で、反応物を24時間にわたって撹拌し続けた。得られる黒色沈殿物をろ過し、エタノールで洗浄し、そして減圧下で乾燥させた。カーボン堆積物のアニーリングを、3時間にわたって酸素を含まないガス流れ条件において400℃で行った。得られる黒色粉末の電気化学活性を、例1の条件と同じ条件で試験した。Li+:Li0に対して2.9〜3.7Vのカットオフ電圧で測定した容量は、実験にれば160mAhg−1(理論値の91%)であった。コーティングされていない材料の比容量は、同じ実験条件で112mAhg−1であった。
300mLの80:20イソプロパノール−水中のチタンテトラ(イソプロポキシド)(28.42g)、リチウムアセテート二水和物(35.7g)、及びマグネシウムアセテート四水和物(10.7g)を使用して、ゾルーゲル技術によってスピネル化合物Li3.5Mg0.5Ti4O12を調製した。得られる白色のゲルを80℃で炉において乾燥させ、そして空気中で3時間にわたって800℃でか焼し、その後で5時間にわたって850℃でアルゴン中の10%水素条件でか焼した。10gの得られた青色粉末を、アセトン中のセルロースアセテート13wt%溶液12mLと混合した。このペーストを乾燥させ、そして700℃の不活性雰囲気において例4の条件でポリマーをか焼した。
光変調デバイス(エレクトロクロミック窓)を以下の様式で製造した。
ガラス/ITO/WO3/PEO−LiTFSI/LiFePO4複合電極/ITO/ガラス
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