JPWO2019093313A1 - 正極、非水電解質蓄電素子、正極の製造方法、及び非水電解質蓄電素子の製造方法 - Google Patents
正極、非水電解質蓄電素子、正極の製造方法、及び非水電解質蓄電素子の製造方法 Download PDFInfo
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- JPWO2019093313A1 JPWO2019093313A1 JP2019552800A JP2019552800A JPWO2019093313A1 JP WO2019093313 A1 JPWO2019093313 A1 JP WO2019093313A1 JP 2019552800 A JP2019552800 A JP 2019552800A JP 2019552800 A JP2019552800 A JP 2019552800A JP WO2019093313 A1 JPWO2019093313 A1 JP WO2019093313A1
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Images
Classifications
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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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
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- H—ELECTRICITY
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- H01G11/22—Electrodes
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Abstract
Description
本発明の一実施形態に係る正極は、導電性の基材と、この基材に積層された正極合剤層とを有する。
上記正極基材は、導電性を有する。基材の材質としては、アルミニウム、チタン、タンタル、ステンレス鋼等の金属又はそれらの合金が用いられる。これらの中でも、耐電位性、導電性の高さ及びコストのバランスからアルミニウム及びアルミニウム合金が好ましい。また、正極基材の形成形態としては、箔、蒸着膜等が挙げられ、コストの面から箔が好ましい。つまり、正極基材としてはアルミニウム箔が好ましい。なお、アルミニウム又はアルミニウム合金としては、JIS−H−4000(2014年)に規定されるA1085P、A3003P等が例示できる。なお、本明細書において、「導電性」を有するとは、JIS−H−0505(1975年)に準拠して測定される体積抵抗率が107Ω・cm以下であることを意味する。
上記正極合剤層は、正極合剤から形成される層である。正極合剤は、ニッケルを含む正極活物質及び還元性有機酸を含有する。正極合剤は、その他必要に応じて、導電剤、バインダー(結着剤)、増粘剤、フィラー等の任意成分を含むことができる。
本発明の一実施形態に係る蓄電素子は、正極、負極及び非水電解質を有する。以下、蓄電素子の一例として、二次電池について説明する。上記正極及び負極は、通常、セパレータを介して積層又は巻回された電極体を形成する。この電極体はケースに収納され、このケース内に上記非水電解質が充填される。上記非水電解質は、正極と負極との間に介在する。また、上記ケースとしては、二次電池のケースとして通常用いられる公知の金属ケース、樹脂ケース等を用いることができる。
当該二次電池に備わる正極は、上述した本発明の一実施形態に係る正極である。
上記負極は、負極基材、及びこの負極基材に直接又は中間層を介して配される負極合剤層を有する。
上記セパレータは、正極と負極とを隔離し、かつ非水電解質を保持する役割を担う。セパレータの材質としては、例えば織布、不織布、多孔質樹脂フィルム等が用いられる。これらの中でも多孔質樹脂フィルムが好ましい。多孔質樹脂フィルムの主成分としては、強度の観点から例えばポリエチレン、ポリプロピレン等のポリオレフィンが好ましい。また、これらの樹脂とアラミドやポリイミド等の樹脂とを複合した多孔質樹脂フィルムを用いてもよい。
上記非水電解質は、非水溶媒と、この非水溶媒に溶解する電解質塩とを含む。上記非水電解質には、その他の添加剤が含有されていてもよい。
<正極の製造方法>
本発明の一実施形態に係る正極の製造方法は、正極合剤ペーストにより、密度が3.1g/cm3以上である正極合剤を形成することを備え、上記正極合剤ペーストが、ニッケルを含む正極活物質及び還元性有機酸を含有する非水電解質蓄電素子用の正極の製造方法である。
本発明の一実施形態に係る非水電解質蓄電素子の製造方法は、上述の正極の製造方法を含む非水電解質蓄電素子の製造方法である。
本発明は上記実施形態に限定されるものではなく、上記態様の他、種々の変更、改良を施した態様で実施することができる。例えば、上記正極又は負極において、中間層を設けなくてもよい。また、当該正極において、正極合剤は明確な層を形成していなくてもよい。例えば上記正極は、メッシュ状の正極基材に正極合剤が担持された構造などであってもよい。
(正極)
正極活物質であるLiNi1/3Mn1/3Co1/3O2と、還元性有機酸であるクエン酸と、導電剤であるアセチレンブラック(AB)と、結着剤であるポリフッ化ビニリデン(PVDF)と、分散媒であるN−メチルピロリドン(NMP)とを用いて正極合剤ペーストを作製した。正極活物質、結着剤及び導電剤の質量比率は90.5:4.5:5.0(固形分換算)とした。また、クエン酸の含有量は、正極活物質100質量部に対して、0.04質量部とした。この正極合剤ペーストを正極基材としてのアルミニウム箔(厚さ16μm)の両面に、正極合剤層非形成部を残して間欠塗工し、乾燥させることで正極合剤層を作製した。その後、正極合剤層表面をロールプレスし、正極を得た。得られた正極の厚さは140μm、正極合剤(正極合剤層)の密度は3.1g/cm3であった。
有機酸(還元性有機酸又はその他の有機酸)の種類及びその含有量、並びに正極合剤の密度を表1、2に示した通りとしたこと以外は、実施例1と同様にして、実施例2〜5及び比較例1〜6の各正極を得た。なお、正極合剤層表面のプレス圧力を適宜変更して、正極合剤の密度を調整した。また、表2中のマレイン酸は、還元性を有さない有機酸である。
(保管前の表面抵抗測定)
上記のようにして作製された各正極について、表面抵抗計(三菱化学社の「ロレスタFP」、プローブは4探針のMCP−TESTERを使用)にて、25℃、露点0℃以下の環境で合剤層表面の抵抗を測定した。
上記保管前の表面抵抗を測定した実施例1〜2及び比較例1〜4の各正極について、温度30℃、相対湿度55%の環境下に二週間保管した。保管後の各正極について、上記「保管前の表面抵抗測定」と同様の方法にて、表面抵抗を測定した。保管前の表面抵抗値に対する保管後の表面抵抗値の百分率を表面抵抗増加率(%)として表1に示す。
上記保管前の表面抵抗を測定した実施例3〜5及び比較例5〜6の各正極について、温度50℃、相対湿度75%の環境下に二週間保管した。保管後の各正極について、上記「保管前の表面抵抗測定」と同様の方法にて、表面抵抗を測定した。保管前の表面抵抗値に対する保管後の表面抵抗値の百分率を表面抵抗増加率(%)として表2に示す。
2 電極体
3 電池容器
4 正極端子
4’ 正極リード
5 負極端子
5’ 負極リード
20 蓄電ユニット
30 蓄電装置
Claims (8)
- 密度が3.1g/cm3以上である正極合剤を備え、
上記正極合剤が、ニッケルを含む正極活物質及び還元性有機酸を含有する非水電解質蓄電素子用の正極。 - 上記還元性有機酸が、カルボン酸である請求項1の正極。
- 上記カルボン酸が、ギ酸、シュウ酸、クエン酸、マロン酸、乳酸、酒石酸、及び没食子酸からなる群より選ばれる少なくとも1種である請求項2の正極。
- 上記正極活物質における遷移金属に占めるニッケルの含有量が33モル%以上である請求項1、請求項2又は請求項3の正極。
- 上記還元性有機酸の含有量が、上記正極活物質100質量部に対して0.01質量部以上0.1質量部以下である請求項1から請求項4のいずれか1項の正極。
- 請求項1から請求項5のいずれか1項の正極を備える非水電解質蓄電素子。
- 正極合剤ペーストにより、密度が3.1g/cm3以上である正極合剤を形成することを備え、
上記正極合剤ペーストが、ニッケルを含む正極活物質及び還元性有機酸を含有する非水電解質蓄電素子用の正極の製造方法。 - 請求項7の正極の製造方法を含む非水電解質蓄電素子の製造方法。
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