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WO2016178509A1 - Matériau actif d'électrode négative pour une batterie rechargeable au lithium - Google Patents

Matériau actif d'électrode négative pour une batterie rechargeable au lithium Download PDF

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Publication number
WO2016178509A1
WO2016178509A1 PCT/KR2016/004697 KR2016004697W WO2016178509A1 WO 2016178509 A1 WO2016178509 A1 WO 2016178509A1 KR 2016004697 W KR2016004697 W KR 2016004697W WO 2016178509 A1 WO2016178509 A1 WO 2016178509A1
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silicon
active material
secondary battery
lithium secondary
negative electrode
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Korean (ko)
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공문규
성재욱
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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
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • 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
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • 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

Definitions

  • the present invention relates to a negative electrode active material for a lithium secondary battery, and more particularly, to a negative electrode active material for a lithium secondary battery having a high charge and discharge capacity and excellent capacity retention.
  • Lithium metal is used as a negative electrode active material of a conventional lithium battery.
  • a carbon-based material is used as a negative electrode active material instead of lithium metal because a short circuit of the battery occurs due to the formation of a dendrite. .
  • Examples of the carbon-based active material include crystalline carbon such as graphite and artificial graphite, and amorphous carbon such as soft carbon and hard carbon.
  • crystalline carbon such as graphite and artificial graphite
  • amorphous carbon such as soft carbon and hard carbon.
  • Graphite is typically used as the crystalline carbon, and has a theoretical limit capacity of 372 mAh / g, which has a high capacity, and is used as a negative electrode active material.
  • the graphite or carbon-based active material has a rather high theoretical capacity, it is only about 380 mAh / g, and there is a problem in that the above-described negative electrode cannot be used in the development of a high capacity lithium battery in the future.
  • the currently active research is a negative electrode active material of the metal-based or intermetallic compounds.
  • a negative electrode active material of the metal-based or intermetallic compounds.
  • lithium batteries using metals or semimetals such as aluminum, germanium, silicon, tin, zinc, and lead as negative electrode active materials have been studied.
  • Such a material has a high energy density and high energy density, and can absorb and release more lithium ions than a negative electrode active material using a carbon-based material, thereby manufacturing a battery having a high capacity and a high energy density.
  • Pure silicon for example, is known to have a high theoretical capacity of 4017 mAh / g.
  • the cycle characteristics are deteriorated, which is still an obstacle to practical use.
  • the silicon is used as a lithium occlusion and release material as a negative electrode active material, it may be difficult to change the volume between the active materials due to the volume change during the charge and discharge process. This is because conductivity decreases or a phenomenon in which the negative electrode active material is peeled off from the negative electrode current collector occurs. That is, the silicon and the like contained in the negative electrode active material expands to about 300 to 400% by occluding lithium by charging, and when the lithium is discharged, the inorganic particles contract.
  • Japanese Laid-Open Patent Publication No. 2006-286312 discloses a lithium secondary battery using a silicon thin film formed by a dry process as a negative electrode active material.
  • the silicon thin film has the structure isolate
  • Patent document 1 attempts to mitigate expansion and contraction of silicon by the physical shape of a silicon thin film, but productivity of a thin film falls significantly, and therefore it is difficult to apply it to actual battery mass production.
  • the present invention is to provide a negative electrode active material for a lithium secondary battery that the electrical change does not occur because the volume change is small during charging and discharging.
  • the present invention is to provide an alloy composition composition method for suppressing the generation of the silicon coarse region when producing a silicon negative electrode active material using a quench solidification process.
  • the present invention is to provide a porous structure through some etching process of the matrix structure other than silicon through an additional etching process.
  • the present invention is an alloy containing silicon (Si), the alloy is made of the following formula (1),
  • an inert intermetallic compound obtained by quenching and solidifying the alloy in a molten state, an inert intermetallic compound in which a solid region and an amorphous region distributed around the solid state active silicon (Si) microparticles and the silicon (Si) microparticles can be mixed, It provides a negative electrode active material for a lithium secondary battery having a porous feature to remove some of the solid region distributed around the fine particles.
  • the present invention provides a negative electrode active material for a lithium secondary battery to suppress the volume growth of the solid phase when the inert intermetallic compound changes the state of the silicon alloy from the high-temperature liquid state to a solid phase.
  • the present invention provides a negative electrode active material for a lithium secondary battery wherein the transition metal is one or more selected from the group consisting of Al, Ni, Cu, Ti and Fe.
  • the present invention provides a negative electrode active material for a lithium secondary battery that the inert intermetallic compound may include Al 3 Ni, NiSi 2 and Al phase.
  • the present invention provides a negative electrode active material for a lithium secondary battery is further coated with a metal element or a carbon-based material on the porous structure surface.
  • the present invention provides a negative electrode active material for a lithium secondary battery, characterized in that the ratio of the X-Ray Dirrractometer (XRD) peak area of the silicon (Si) microparticles and the silicon compound (SiM) phase is 1 to 1.
  • XRD X-Ray Dirrractometer
  • the negative electrode active material significantly improves the performance and stability of the battery, and has excellent capacity and cycle characteristics of the lithium secondary battery including the negative electrode active material.
  • Fig. 1 is a diagram of a melt-spinning process, which is a type of quench solidification process.
  • Figure 2 is a schematic diagram showing the state change process of the liquid phase to a solid state through the quench solidification process of the silicon alloy.
  • TEM 3 is a result drawing of a transmission electron microscope (TEM) of the silicon alloy of Example 1;
  • 6, 8, 10 and 12 is a view showing the result after the coin-shaped secondary battery using a negative electrode active material prepared in Examples 1 to 3 and Comparative Example 1, and subjected to charge and discharge evaluation.
  • the present invention relates to a negative electrode active material for a lithium secondary battery and a lithium secondary battery comprising the same, wherein the negative electrode active material for a lithium secondary battery includes active silicon (Si) fine particles and an inert intermetallic compound distributed around the active fine particles. It is a porous structure.
  • the present invention suppresses the occurrence of the silicon coarse region when the molten silicon alloy is made into a solid phase by using a quench solidification process to produce the negative electrode active material.
  • a quench solidification process to produce the negative electrode active material.
  • an additional etching process it can effectively suppress the expansion problem of the silicon-based negative electrode active material due to the lithium insertion.
  • intermetallic compounds should be formed in a composite structure made of silicon and an intermetallic compound. Some of the two metals are to facilitate the selective removal even in weakly acidic material. In addition, the metal remaining by the etching may serve to maintain electrical conductivity between the silicon particles.
  • silicon has attracted attention as a negative electrode active material of a lithium secondary battery that requires continuous high capacity, but has a disadvantage in that its life is sharply reduced due to severe volume expansion during charge and discharge.
  • attention has been paid to composite particles composed of active silicon microparticles and inert intermetallic compounds distributed around the active silicon microparticles.
  • Fig. 1 is a diagram of a melt-spinning process, which is a type of quench solidification process.
  • the liquid silicon alloy is sent to the cooling wheel 40 through the nozzle 20 using the inert gas 30.
  • phase transformation by rapid cooling is possible at a rate of 10 4 to 10 6 K / sec.
  • the high temperature metal solution coated in a wide and thin direction in the rotational direction in contact with the cooling wheel 40 rotating at high speed is deprived of heat by the cooling wheel 40 having excellent thermal conductivity, so that the phase transformation occurs from the high temperature metal solution to the metal plate material at room temperature.
  • the phase transformation is terminated by forming a plurality of solid phase nuclei rather than growing solid phase nuclei. That is, by minimizing the phase transformation time to increase the nucleus of the solid phase it is possible to finely form the size of the silicon and intermetallic compound.
  • the present invention is quench solidified using a silicon (Si) alloy composed of the following formula.
  • the transition metal may be one or more selected from the group consisting of Al, Ni, Cu, Ti, and Fe.
  • Figure 2 is a schematic diagram showing the state change process of the liquid phase to a solid state through the quench solidification process of the silicon alloy.
  • (a) is a schematic diagram showing the process of the phase change from the liquid phase to the solid phase of the conventional silicon alloy
  • (b) is a schematic diagram of the phase change of the silicon alloy of the present invention composition.
  • (a) After the silicon solid core 50 is formed in the metal solution 60, the silicon core grows. At this time, a solid core of an intermetallic compound having a lower melting point than silicon is formed. After that, the nucleus of silicon and the nucleus of the intermetallic compound continue to grow, and the phase transformation is terminated when both liquid phases change into solid phase.
  • (b) is a schematic diagram of solid-state transformation in the presence of silicon and two or more intermetallic compounds. Initially, the solid core 50 of the high melting point silicon is formed and starts to grow. Thereafter, a plurality of nuclei 70 of two or more intermetallic compounds are formed, and the nucleus 70 of the intermetallic compound suppresses the growth of the solid silicon 50. Silicon whose phase transformation from liquid phase to solid phase is suppressed forms new solid silicon rather than growth of solid silicon to complete phase transformation.
  • the formed intermetallic compound may help the nucleus of the silicon solid phase to be easily formed.
  • the solid silicon nucleus is formed on the surface of the intermetallic compound present in the liquid phase 60, it serves to reduce the surface energy, thereby helping to form a silicon solid phase nucleus, thereby achieving a fine tissue formation .
  • the present invention which is rapidly solidified, is composed of a large number of solid state active silicon (Si) microparticles with minimized coarsening region and an inert intermetallic compound distributed around the silicon (Si) microparticles.
  • the crystalline region and the amorphous region exist in a mixed state.
  • a porous structure is formed by directly etching silicon using hydrofluoric acid, but in the present invention, a method of etching an intermetallic compound other than silicon is selected to enable commercial etching process.
  • the intermetallic oxide may be composed of Al 3 Ni so as not to be removed in an etching process as opposed to Al and NiSi 2 , which are easily etched to easily form a porous structure using a common acid.
  • the Al 3 Ni is an intermetallic compound that cannot be etched in a weak acid and is not removed even in various etching processes. Through such an etching process, a porous silicon alloy can be manufactured.
  • a silicon (Si) alloy was prepared by an arc dissolving method under argon gas to have a composition of Si 50%, Ni 9.5%, and Al 40.5%, and the prepared Si alloy was formed of Ni 3 and Al 3 Ni and NiSi using a melt spinning method.
  • a silicon (Si) alloy was prepared such that silicon (Si) microparticles were located between matrix phases (inactive intermetallic compounds) composed of 2 and Al.
  • the quenching speed rotational speed of the cooling wheel
  • the method applied in the present invention is not limited to the above method, and in addition to the melt spinning method, if a sufficient quenching speed can be obtained, the fine powder production technique (gas atomizer method, centrifugal gas atomizer method, plasma method) as described above can be obtained. It can also be manufactured by the atomizer method, the rotating electrode method, the mechanical etching method and the like.
  • an inactive intermetallic compound was etched around silicon particles to prepare a negative active material for a lithium secondary battery of a silicon alloy having a porous structure.
  • a silicon (Si) alloy was formed in the same manner as in Example 1 except that the composition was made of Si 40%, Ni 11.4%, and Al 48.6%.
  • the silicon (Si) alloy was formed in the same manner as in Example 1 except that the composition was made of Si 30%, Ni 13.3%, and Al 56.7%.
  • the silicon (Si) alloy was carried out in the same manner as in Example 1 except that the composition was made of Si 60%, Ni 15%, and Al 25%.
  • SEM Scanning Electron Microscopy
  • Examples of the anode active material before etching (a) can be confirmed that there is no coarse region and the silicon crystal of a uniform fine structure, the cathode active material after the etching (b) can be confirmed that the empty space is formed around the silicon particles. .
  • Comparative Example 1 can observe the microstructure (a) according to the thickness of the quench solidified plate and the silicon coarse region (b) as the distance from the cooling wheel.
  • Coin-shaped secondary batteries were prepared using the negative electrode active materials prepared in Examples 1 to 3 and Comparative Example 1, and after the charge and discharge evaluations, the results are shown in FIGS. 6, 8, 10, and 12.
  • the mixing ratio of the active material, the conductive agent (Super P-based conductive agent), and the binder (PI-based binder) is 77: 15: 2: 6 (active material: additive: conductive agent: binder). It was prepared as possible.
  • Example 1 it can be seen that the charge before etching (a) has a maximum capacity of 900mAh / g, and as a result of the continuous charge and discharge, the capacity is gradually reduced to fall below 250mAh / g. However, after the etching (b) it can be seen that the charge capacity of 1500 ⁇ 1800mAh / g.
  • Example 2 As in Example 1, it can be seen that the charging capacity after etching is increased by at least two times, and Example 1, which has the largest content of silicon (Si), is larger than other examples. .
  • Comparative Example 1 the charge capacity was about 1445.5 mAh / g, similar to the charge capacity after etching in Example 2, but it can be seen that the capacity decreases rapidly after several charge and discharge cycles.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Composite Materials (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Silicon Compounds (AREA)

Abstract

La présente invention concerne un matériau actif d'électrode négative pour une batterie rechargeable au lithium. Le matériau actif d'électrode négative est un alliage contenant du silicium composé de la formule chimique (1) de SixMyNz, où 30 ≤ x ≤ 60, 1 ≤ y ≤ 20, 30 ≤ z ≤ 60, x + y + z = 100 ; x, y et z représentent chacun un % atomique ; et M et N représentent chacun un métal de transition, et est caractérisé en ce qu'il présente une structure poreuse qui peut être obtenue par solidification rapide de l'alliage dans un état fondu et est composé de fines particules de silicium actives solides et d'un composé intermétallique inactif qui est réparti autour des fines particules de silicium et peut comporter une région solide et une région amorphe, certaines parties de la région solide réparties autour des fines particules étant enlevées.
PCT/KR2016/004697 2015-05-06 2016-05-04 Matériau actif d'électrode négative pour une batterie rechargeable au lithium Ceased WO2016178509A1 (fr)

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KR1020150063063A KR101762773B1 (ko) 2015-05-06 2015-05-06 리튬 이차 전지용 음극 활물질
KR10-2015-0063063 2015-05-06

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018225971A1 (fr) * 2017-06-07 2018-12-13 한국생산기술연구원 Matériau actif d'anode destiné à une batterie secondaire au lithium, anode destinée à une batterie secondaire au lithium, et batterie secondaire au lithium comprenant une telle anode

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KR102087134B1 (ko) * 2017-06-07 2020-03-11 한국생산기술연구원 리튬이차전지용 음극활물질, 리튬이차전지용 음극 및 이를 포함하는 리튬이차전지
KR102309817B1 (ko) * 2018-08-06 2021-10-07 충남대학교산학협력단 리튬 이차전지용 음극 활물질 및 그의 제조방법
KR102166559B1 (ko) * 2018-08-06 2020-10-16 충남대학교산학협력단 리튬 이차전지용 음극 활물질 및 그의 제조방법
KR102254126B1 (ko) * 2018-09-12 2021-05-20 연세대학교 산학협력단 다공성 실리콘 구조체, 이를 포함하는 2차전지용 음극 활물질 및 이의 제조방법
KR102218030B1 (ko) * 2018-11-26 2021-02-22 한국생산기술연구원 리튬이차전지용 음극활물질 제조방법, 리튬이차전지용 음극활물질, 리튬이차전지용 음극 및 이를 포함하는 리튬이차전지
KR102218033B1 (ko) * 2018-11-27 2021-02-22 한국생산기술연구원 리튬이차전지용 음극활물질 제조방법, 리튬이차전지용 음극활물질, 리튬이차전지용 음극 및 이를 포함하는 리튬이차전지
KR20230038938A (ko) 2021-09-13 2023-03-21 현대자동차주식회사 리튬이차전지용 복합음극 및 이의 제조방법
KR102527633B1 (ko) * 2023-03-17 2023-04-28 성재욱 리튬 이차전지용 음극 활물질, 이의 제조방법 및 상기 음극 활물질을 포함하는 리튬 이차전지

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KR20050020571A (ko) * 2003-08-22 2005-03-04 삼성에스디아이 주식회사 리튬 이차 전지용 음극 활물질, 이의 제조 방법 및 이를포함하는 리튬 이차 전지
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018225971A1 (fr) * 2017-06-07 2018-12-13 한국생산기술연구원 Matériau actif d'anode destiné à une batterie secondaire au lithium, anode destinée à une batterie secondaire au lithium, et batterie secondaire au lithium comprenant une telle anode

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KR101762773B1 (ko) 2017-07-28
KR20160131208A (ko) 2016-11-16

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