JP2023039387A - リチウム含有珪素酸化物複合負極材料、その調製方法及びリチウムイオン電池 - Google Patents
リチウム含有珪素酸化物複合負極材料、その調製方法及びリチウムイオン電池 Download PDFInfo
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- JP2023039387A JP2023039387A JP2022000550A JP2022000550A JP2023039387A JP 2023039387 A JP2023039387 A JP 2023039387A JP 2022000550 A JP2022000550 A JP 2022000550A JP 2022000550 A JP2022000550 A JP 2022000550A JP 2023039387 A JP2023039387 A JP 2023039387A
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- lithium
- silicon oxide
- negative electrode
- containing silicon
- oxide composite
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 110
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 109
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 109
- 229910052814 silicon oxide Inorganic materials 0.000 title claims abstract description 109
- 239000002131 composite material Substances 0.000 title claims abstract description 78
- 238000000034 method Methods 0.000 title claims abstract description 27
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 14
- 239000010405 anode material Substances 0.000 title claims abstract description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 47
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 46
- 239000010410 layer Substances 0.000 claims abstract description 16
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 14
- 229910001556 Li2Si2O5 Inorganic materials 0.000 claims abstract description 12
- 229910007562 Li2SiO3 Inorganic materials 0.000 claims abstract description 10
- 239000012792 core layer Substances 0.000 claims abstract description 8
- 239000011258 core-shell material Substances 0.000 claims abstract description 4
- 239000007773 negative electrode material Substances 0.000 claims description 72
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 claims description 59
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 238000002441 X-ray diffraction Methods 0.000 claims description 20
- 239000000243 solution Substances 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000007787 solid Substances 0.000 claims description 15
- 238000000576 coating method Methods 0.000 claims description 13
- 239000002904 solvent Substances 0.000 claims description 12
- 239000011248 coating agent Substances 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 11
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 10
- 230000004048 modification Effects 0.000 claims description 8
- 238000012986 modification Methods 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 7
- 238000000926 separation method Methods 0.000 claims description 7
- 239000007790 solid phase Substances 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 230000001590 oxidative effect Effects 0.000 claims description 6
- 239000002243 precursor Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 238000007654 immersion Methods 0.000 claims description 4
- 239000012808 vapor phase Substances 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 150000001412 amines Chemical class 0.000 claims description 3
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 claims description 3
- 150000002576 ketones Chemical class 0.000 claims description 3
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 3
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 3
- 239000012046 mixed solvent Substances 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- 239000012071 phase Substances 0.000 claims description 2
- 230000002441 reversible effect Effects 0.000 abstract description 13
- 239000000463 material Substances 0.000 description 47
- 239000007789 gas Substances 0.000 description 20
- 239000000843 powder Substances 0.000 description 17
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 16
- PAZHGORSDKKUPI-UHFFFAOYSA-N lithium metasilicate Chemical compound [Li+].[Li+].[O-][Si]([O-])=O PAZHGORSDKKUPI-UHFFFAOYSA-N 0.000 description 11
- 229910052912 lithium silicate Inorganic materials 0.000 description 11
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 9
- 229910001873 dinitrogen Inorganic materials 0.000 description 9
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 8
- 229910052786 argon Inorganic materials 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 7
- 238000007599 discharging Methods 0.000 description 7
- 229910000103 lithium hydride Inorganic materials 0.000 description 7
- 229910052710 silicon Inorganic materials 0.000 description 7
- 239000010703 silicon Substances 0.000 description 7
- 238000001816 cooling Methods 0.000 description 6
- 230000001681 protective effect Effects 0.000 description 6
- 239000002002 slurry Substances 0.000 description 6
- 229910018068 Li 2 O Inorganic materials 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 238000003763 carbonization Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 230000002427 irreversible effect Effects 0.000 description 3
- -1 lithium silicates Chemical class 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
- 239000005977 Ethylene Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 2
- 238000007664 blowing Methods 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 229910052743 krypton Inorganic materials 0.000 description 2
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 description 2
- AFRJJFRNGGLMDW-UHFFFAOYSA-N lithium amide Chemical compound [Li+].[NH2-] AFRJJFRNGGLMDW-UHFFFAOYSA-N 0.000 description 2
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 229910052919 magnesium silicate Inorganic materials 0.000 description 2
- 239000000391 magnesium silicate Substances 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052754 neon Inorganic materials 0.000 description 2
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000011856 silicon-based particle Substances 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- 239000012448 Lithium borohydride Substances 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 229910000676 Si alloy Inorganic materials 0.000 description 1
- 229910004283 SiO 4 Inorganic materials 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- YJSAVIWBELEHDD-UHFFFAOYSA-N [Li].[Si]=O Chemical compound [Li].[Si]=O YJSAVIWBELEHDD-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- TXLQIRALKZAWHN-UHFFFAOYSA-N dilithium carbanide Chemical compound [Li+].[Li+].[CH3-].[CH3-] TXLQIRALKZAWHN-UHFFFAOYSA-N 0.000 description 1
- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical compound [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000012280 lithium aluminium hydride Substances 0.000 description 1
- IDBFBDSKYCUNPW-UHFFFAOYSA-N lithium nitride Chemical compound [Li]N([Li])[Li] IDBFBDSKYCUNPW-UHFFFAOYSA-N 0.000 description 1
- 229910001947 lithium oxide Inorganic materials 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 235000019792 magnesium silicate Nutrition 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 239000011295 pitch Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000011085 pressure filtration Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 229910021332 silicide Inorganic materials 0.000 description 1
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 235000000346 sugar Nutrition 0.000 description 1
- 150000008163 sugars Chemical class 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Images
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- C—CHEMISTRY; METALLURGY
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- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/02—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/32—Alkali metal silicates
-
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- C01B32/00—Carbon; Compounds thereof
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Abstract
Description
リチウム含有珪素酸化物複合負極材料であって、コア層と、シェル層とを備えたコアシェル構造であり、前記コア層がナノケイ素、Li2SiO3及びLi2Si2O5を含み、前記シェル層が被覆されている導電性炭素層であることを特徴とする、リチウム含有珪素酸化物複合負極材料。
(1)炭素被覆珪素酸化物SiOxとリチウム源を固相混合法で混合して、プレリチウム前駆体を形成する工程、
(2)プレリチウム前駆体を真空又は非酸化性雰囲気下で熱処理を施してから分散してふるい分け、物相と構造の調整を実現して複合物を形成する工程、
(3)前記工程(2)で形成された複合物に表面改質処理を施して表面処理したリチウム含有珪素酸化物複合負極材料を得る工程。
(1)炭素被覆珪素酸化物SiOxとリチウム源を固相混合法で混合して、プレリチウム前駆体を形成する工程
(2)プレリチウム前駆体を真空又は非酸化性雰囲気下で熱処理を施してから分散してふるい分け、物相と構造の調整を実現して複合物を形成する工程
(3)工程(2)で形成された複合物に表面改質処理を施して表面処理したリチウム含有珪素酸化物複合負極材料を得る工程。
2kgのSiO0.8粉末をCVD回転炉に量り入れ、炭素源としてアセチレンを吹き込み、保護雰囲気として窒素ガスを吹き込み、700℃で2.5時間沈着させ、冷却して払い出して炭素被覆珪素酸化物材料を得た。
2kgのSiO0.8粉末をCVD回転炉に量り入れ、炭素源としてエチレンを吹き込み、保護雰囲気として窒素ガスを吹き込み、900℃で3時間沈着させ、冷却して払い出して炭素被覆珪素酸化物材料を得た。
2kgのSiO0.8粉末をCVD回転炉に量り入れ、炭素源としてメタンを吹き込み、保護雰囲気として窒素ガスを吹き込み、1000℃で7時間沈着させ、冷却して払い出して炭素被覆珪素酸化物材料を得た。
2kgのSiO粉末と800gのスクロースを量りとり、VC混合機内で均一に混合してから箱型炉に入れ、窒素ガス保護雰囲気下で800℃にて3時間焼結し、冷却して払い出して炭素被覆珪素酸化物材料を得た。
(1)比較例1で調製した炭素被覆珪素酸化物材料を取り、リチウム源とした水素化リチウムとVC混合し、混合は窒素ガス雰囲気下で実施し、水素化リチウムの質量は、この炭素被覆珪素酸化物材料の5%を占め、
(2)工程(1)で均一に混合した材料を箱型炉に入れ、アルゴンガス雰囲気下で焙煎し、焙煎温度が700℃、昇温速度が1℃/分、温度保持時間が4時間で、冷却して払い出した後、分散してふるい分け、
(3)工程(2)で調製した材料を水に浸漬させ、ここで、水の質量と固体粉末材料の質量比は3:1で、500rpmで2時間浸漬して撹拌した後、吸引ろ過し、次にイソプロパノールを加えて洗浄し、ここでイソプロパノールの質量と固体粉末の質量比は1:1であり、500rpmで1時間撹拌し、吸引ろ過し、そして真空乾燥させ、ふるい分け、リチウム含有珪素酸化物複合負極材料を得た。
(1)比較例1で調製した炭素被覆珪素酸化物材料を取り、リチウム源とした水素化リチウムとVC混合し、混合は窒素ガス雰囲気下で実施し、水素化リチウムの質量は、この炭素被覆珪素酸化物材料の10%を占め、
(2)工程(1)で均一に混合した材料を箱型炉に入れ、アルゴンガス雰囲気下で焙煎し、焙煎温度が650℃、昇温速度が1℃/分、温度保持時間が4時間で、冷却して払い出した後、分散してふるい分け、
(3)工程(2)で調製した材料をエタノールと水の混合溶液に浸漬させ、ここで、エタノールと水の質量比は1:1で、溶液の総質量と固体粉末材料の質量比が3:1で、500rpmで2時間浸漬して撹拌した後、吸引ろ過し、次にアセトンを加えて洗浄し、ここでアセトンの質量と固体粉末の質量比は1:1であり、500rpmで1時間撹拌し、吸引ろ過し、そして真空乾燥させ、ふるい分け、リチウム含有珪素酸化物複合負極材料を得た。
(1)比較例1で調製した炭素被覆珪素酸化物材料を取り、リチウム源とした水素化リチウムとVC混合し、混合は窒素ガス雰囲気下で実施し、窒化リチウムの質量は、この炭素被覆珪素酸化物材料の8%を占め、
(2)工程(1)で均一に混合した材料を箱型炉に入れ、アルゴンガス雰囲気下で焙煎し、焙煎温度が850℃、昇温速度が1℃/分、温度保持時間が3時間で、冷却して払い出した後、分散してふるい分け、
(3)工程(2)で調製した材料を酢酸と水の混合溶液に浸漬させ、ここで、酢酸と水の質量比は1:10で、溶液の総質量と固体粉末材料の質量比が3:1で、500rpmで2時間浸漬して撹拌した後、吸引ろ過し、次にエタノールを加えて洗浄し、ここでエタノールの質量と固体粉末の質量比は1:1であり、500rpmで1時間撹拌し、吸引ろ過し、そして真空乾燥させ、ふるい分け、リチウム含有珪素酸化物複合負極材料を得た。
(1)比較例1で調製した炭素被覆珪素酸化物材料を取り、リチウム源とした金属リチウムとの機械的融合処理を行い、融合はアルゴンガス雰囲気下で実施し、融合温度が180~250℃で、金属リチウムの質量はこの炭素被覆珪素酸化物材料の10%を占め、
(2)工程(1)で均一に混合した材料を箱型炉に入れ、アルゴンガス雰囲気下で焙煎し、焙煎温度が500℃、昇温速度が1℃/分、温度保持時間が2時間で、冷却して払い出した後、分散してふるい分け、
(3)工程(2)で調製した材料を酢酸と水に浸漬させ、ここで、エタノールと水の質量比は5:1で、溶液の総質量と固体粉末材料の質量比が3:1で、500rpmで2時間浸漬して撹拌した後、吸引ろ過し、次にエーテルを加えて洗浄し、ここでエーテルの質量と固体粉末の質量比は1:1であり、500rpmで1時間撹拌し、吸引ろ過し、そして真空乾燥させ、ふるい分け、リチウム含有珪素酸化物複合負極材料を得た。
(1)比較例1で調製した炭素被覆珪素酸化物材料を取り、リチウム源としたリチウムアミドとVC混合し、混合はアルゴンガス雰囲気下で実施し、チウムアミドの質量は、この炭素被覆珪素酸化物材料の12%を占め、
(2)工程(1)で均一に混合した材料を箱型炉に入れ、アルゴンガス雰囲気下で焙煎し、焙煎温度が600℃、昇温速度が1℃/分、温度保持時間が4時間で、冷却して払い出した後、分散してふるい分け、
(3)工程(2)で調製した材料を炭酸水に浸漬させ、ここで、炭酸水の質量と固体粉末材料の質量比は3:1で、500rpmで2時間浸漬して撹拌した後、吸引ろ過し、次にイソプロパノールを加えて洗浄し、ここでイソプロパノールの質量と固体粉末の質量比は1:1であり、500rpmで1時間撹拌し、吸引ろ過し、そして真空乾燥させ、ふるい分け、リチウム含有珪素酸化物複合負極材料を得た。
1、結晶構造のキャラクタリゼーション:実施例及び比較例で調製されたリチウム含有珪素酸化物複合負極材料について結晶構造のキャラクタリゼーションを実施した。XRDテストは、オランダのパナリティカル(PANalytical)社製粉末X線回折装置Xpert3 Powderを用い、テスト電圧40KV、テスト電流40mA、スキャン範囲10°~90°、スキャンステップ長さ0.008°、1 ステップあたりのスキャン時間12秒となった。
Claims (10)
- リチウム含有珪素酸化物複合負極材料であって、コア層と、シェル層とを備えたコアシェル構造であり、前記コア層がナノケイ素、Li2SiO3及びLi2Si2O5を含み、前記シェル層が被覆されている導電性炭素層であることを特徴とする、リチウム含有珪素酸化物複合負極材料。
- ナノケイ素の平均結晶粒サイズ≦20nmであることを特徴とする、請求項1に記載のリチウム含有珪素酸化物複合負極材料。
- 前記導電性炭素層の厚さは、2~500nmであることを特徴とする、請求項1に記載のリチウム含有珪素酸化物複合負極材料。
- リチウム含有珪素酸化物複合負極材料のX線回折パターンにおける2θが26.90±0.3°のLi2SiO3(111)回折ピーク面積は、A1で、X線回折パターンにおける2θが28.40±0.3°のSi(111)回折ピーク面積がA2であり、A2/A1≧1.0であることを特徴とする、請求項1に記載のリチウム含有珪素酸化物複合負極材料。
- リチウム含有珪素酸化物複合負極材料のX線回折パターンにおける2θが24.75±0.2°のLi2Si2O5(111)回折ピーク強度は、I1で、X線回折パターンにおける2θが26.90±0.3°のLi2SiO3(111)回折ピーク強度はI2であり、0.25≦I1/I2≦1.0であることを特徴とする、請求項1に記載のリチウム含有珪素酸化物複合負極材料。
- (1)炭素被覆珪素酸化物SiOxとリチウム源を固相混合法で混合して、プレリチウム前駆体を形成する工程と、
(2)プレリチウム前駆体を真空又は非酸化性雰囲気下で熱処理を施してから分散してふるい分け、物相と構造の調整を実現して複合物を形成する工程と、
(3)前記工程(2)で形成された複合物に表面改質処理を施して表面処理したリチウム含有珪素酸化物複合負極材料を得る工程と
含むことを特徴とする、リチウム含有珪素酸化物複合負極材料の調製方法。 - 前記炭素被覆珪素酸化物SiOxの中に、0.5≦x≦1.6であることを特徴とする、請求項6に記載のリチウム含有珪素酸化物複合負極材料の調製方法。
- 前記炭素被覆珪素酸化物SiOxの中の炭素被覆方法は、気相法被覆又は固相法被覆のいずれか1種であることを特徴とする、請求項6に記載のリチウム含有珪素酸化物複合負極材料の調製方法。
- 前記工程(3)の表面改質処理が洗浄であり、前記洗浄の具体的工程は、前記工程(2)で調製された複合物を溶液Aに入れて浸漬処理を施し、溶液Aに浸漬した後、固液分離を行い、固液分離後に得られた固形物を溶液Bで洗い流し続け、分離した固形物に乾燥処理を施すことであり、前記溶液Aはアルコール、炭酸リチウムを溶解したアルカリ水、弱酸、水、又はそれらの混合溶液のうちの1種であり、前記溶液Bはエーテル類溶媒、ケトン類溶媒、エステル類溶媒、アルコール類溶媒、アミン類溶媒又はそれらの混合溶媒のうちの1種であることを特徴とする、請求項6に記載のリチウム含有珪素酸化物複合負極材料の調製方法。
- 請求項1に記載のリチウム含有珪素酸化物複合負極材料を備えることを特徴とする、リチウムイオン電池。
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JP2016192385A (ja) * | 2015-03-31 | 2016-11-10 | ソニー株式会社 | 負極活物質およびその製造方法、負極、ならびに電池 |
WO2017038320A1 (ja) * | 2015-08-28 | 2017-03-09 | 株式会社大阪チタニウムテクノロジーズ | Li含有酸化珪素粉末及びその製造方法 |
JP2021103691A (ja) * | 2016-05-30 | 2021-07-15 | 信越化学工業株式会社 | リチウムイオン二次電池用負極活物質、リチウムイオン二次電池用混合負極活物質材料、リチウムイオン二次電池用負極、リチウムイオン二次電池、リチウムイオン二次電池用負極活物質の製造方法、リチウムイオン二次電池用負極の製造方法、及びリチウムイオン二次電池の製造方法 |
WO2019189747A1 (ja) * | 2018-03-30 | 2019-10-03 | 株式会社大阪チタニウムテクノロジーズ | 酸化珪素粉末の製造方法及び負極材 |
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