JP6697838B2 - 蓄電デバイス用Si系合金負極材料の製造方法 - Google Patents
蓄電デバイス用Si系合金負極材料の製造方法 Download PDFInfo
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- JP6697838B2 JP6697838B2 JP2014107687A JP2014107687A JP6697838B2 JP 6697838 B2 JP6697838 B2 JP 6697838B2 JP 2014107687 A JP2014107687 A JP 2014107687A JP 2014107687 A JP2014107687 A JP 2014107687A JP 6697838 B2 JP6697838 B2 JP 6697838B2
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- 238000004519 manufacturing process Methods 0.000 title claims description 28
- 229910045601 alloy Inorganic materials 0.000 title claims description 13
- 239000000956 alloy Substances 0.000 title claims description 13
- 238000003860 storage Methods 0.000 title claims description 10
- 239000007773 negative electrode material Substances 0.000 title claims description 9
- 239000000843 powder Substances 0.000 claims description 74
- 239000002245 particle Substances 0.000 claims description 40
- 239000002994 raw material Substances 0.000 claims description 24
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 20
- 239000007789 gas Substances 0.000 claims description 19
- 238000001816 cooling Methods 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 11
- 229910052786 argon Inorganic materials 0.000 claims description 10
- 238000010298 pulverizing process Methods 0.000 claims description 9
- 150000001875 compounds Chemical class 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 5
- 239000011324 bead Substances 0.000 claims description 5
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- 229910052787 antimony Inorganic materials 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- 230000001186 cumulative effect Effects 0.000 claims description 3
- 229910052733 gallium Inorganic materials 0.000 claims description 3
- 229910052732 germanium Inorganic materials 0.000 claims description 3
- 229910052738 indium Inorganic materials 0.000 claims description 3
- 229910052746 lanthanum Inorganic materials 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 229910052748 manganese Inorganic materials 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 229910052758 niobium Inorganic materials 0.000 claims description 3
- 229910052698 phosphorus Inorganic materials 0.000 claims description 3
- 229910052718 tin Inorganic materials 0.000 claims description 3
- 229910052720 vanadium Inorganic materials 0.000 claims description 3
- 229910052727 yttrium Inorganic materials 0.000 claims description 3
- 229910052725 zinc Inorganic materials 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- 238000010791 quenching Methods 0.000 claims 1
- 230000000171 quenching effect Effects 0.000 claims 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 26
- 229910001416 lithium ion Inorganic materials 0.000 description 26
- 238000000034 method Methods 0.000 description 19
- 239000011149 active material Substances 0.000 description 14
- 238000003801 milling Methods 0.000 description 14
- 239000008151 electrolyte solution Substances 0.000 description 13
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 12
- 238000009826 distribution Methods 0.000 description 8
- 238000000227 grinding Methods 0.000 description 6
- 239000011148 porous material Substances 0.000 description 6
- 238000007599 discharging Methods 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000009689 gas atomisation Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 3
- 239000003990 capacitor Substances 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 239000011889 copper foil Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 230000006698 induction Effects 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 229910021332 silicide Inorganic materials 0.000 description 3
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 239000003115 supporting electrolyte Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 2
- 239000004642 Polyimide Substances 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 230000008602 contraction Effects 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004880 explosion Methods 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 229910021382 natural graphite Inorganic materials 0.000 description 2
- 229920001721 polyimide Polymers 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 1
- 229910013870 LiPF 6 Inorganic materials 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910021383 artificial graphite Inorganic materials 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000009931 harmful effect Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- -1 lithium hexafluorophosphate Chemical compound 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 239000011802 pulverized particle Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000009692 water atomization Methods 0.000 description 1
Images
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Battery Electrode And Active Subsutance (AREA)
Description
(a)Siが主成分であるSi相
及び
(b)Siと、Mg,Al,Ti,V,Cr,Mn,Fe,Co,Ni,Cu,Zn,Ga,Ge,Zr,Nb,Mo,In,Sn,Sb,La,Y,P,Bi,N,及びCの群から選択される1又は2以上の元素とを含む化合物相
を有する蓄電デバイス用Si系合金負極材料が得られる。この製造方法は、
(1)原料を加熱し、前記加熱により溶融した前記原料を100℃/s以上の冷却速度で急冷して、その後の加熱処理を行わずに、一次粉末を得るステップ
及び
(2)上記ステップ(1)における一次粉末を乾式ジェットミル装置にて粉砕し、累積50体積%の粒子径(D50)が0.1μm以上10.0μm以下である二次粉末を得るステップ
を含む。
上記コイン型セルにて、温度が25℃であり、電流密度が0.50mA/cm2である条件で、正極と負極との電位差が0Vとなるまで充電を行った。その後、電位差が1.5Vとなるまで放電を行った。この充電及び放電を、50サイクル繰り返した。初期の放電容量X及び50サイクルの充電及び放電を繰り返した後の放電容量Yを測定した。さらに、放電容量Xに対する放電容量Yの比率(維持率)を算出した。この結果が、下記の表3及び4に示されている。
一次粉末から二次粉末を得るための粉砕工程の作業性を、下記の基準によって格付けした。
A:良い
B:悪い
C:極めて悪い
この結果が、下記の表3及び4に示されている。
6・・・電解液
8・・・セパレータ
10・・・正極
12・・・負極
18・・・集電体
20・・・活物質層
22・・・粒子
Claims (4)
- (a)Siが主成分であるSi相
及び
(b)Siと、Mg,Al,Ti,V,Cr,Mn,Fe,Co,Ni,Cu,Zn,Ga,Ge,Zr,Nb,Mo,In,Sn,Sb,La,Y,P,Bi,N,及びCの群から選択される1又は2以上の元素とを含む化合物相
を有する蓄電デバイス用Si系合金負極材料の製造方法であって、
(1)原料を加熱し、前記加熱により溶融した前記原料を100℃/s以上の冷却速度で急冷して、その後の加熱処理を行わずに、一次粉末を得るステップ
及び
(2)上記ステップ(1)における一次粉末を乾式ジェットミル装置にて粉砕し、累積50体積%の粒子径(D50)が0.1μm以上10.0μm以下である二次粉末を得るステップ
を含むことを特徴とする製造方法。 - 上記ステップ(2)における粉砕に、エアーガス、窒素ガス又はアルゴンガスが用いられる請求項1に記載の製造方法。
- 上記ステップ(2)において用いられる乾式ジェットミル装置のうち、上記粉末と衝突する部分の材質が、ステンレス鋼である請求項1又は2に記載の製造方法。
- 上記ステップ(1)が、前記急冷により凝固した前記原料をボールミル、ビーズミル、遊星ボールミル、アトライタ及び振動ボールミルの群から選択される少なくとも1種の装置にて粉砕して前記一次粉末を得ることを含む、請求項1〜3のいずれか一項に記載の製造方法。
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JP6705302B2 (ja) * | 2016-06-16 | 2020-06-03 | 日産自動車株式会社 | 電気デバイス用負極活物質、およびこれを用いた電気デバイス |
JP2024065690A (ja) * | 2022-10-31 | 2024-05-15 | 大同特殊鋼株式会社 | リチウムイオン電池用の負極材料粉末 |
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JPH10272350A (ja) * | 1997-03-31 | 1998-10-13 | Mitsubishi Chem Corp | 無機物混合フィラーの製造方法 |
JP2001291514A (ja) * | 2000-04-06 | 2001-10-19 | Sumitomo Metal Ind Ltd | 非水電解質二次電池用負極材料とその製造方法 |
WO2013002163A1 (ja) * | 2011-06-27 | 2013-01-03 | 三井金属鉱業株式会社 | 非水電解液二次電池用負極活物質 |
WO2013151047A1 (ja) * | 2012-04-05 | 2013-10-10 | 三井金属鉱業株式会社 | 非水電解液二次電池用負極活物質 |
US9478800B2 (en) * | 2012-05-15 | 2016-10-25 | Mitsui Mining & Smelting Co., Ltd. | Negative electrode active material for nonaqueous electrolyte secondary batteries |
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JP6177652B2 (ja) * | 2012-10-09 | 2017-08-09 | 三井金属鉱業株式会社 | リチウム二次電池の製造方法 |
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