JP2003051306A - Negative electrode for lead-acid battery - Google Patents

Negative electrode for lead-acid battery

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Publication number
JP2003051306A
JP2003051306A JP2001239310A JP2001239310A JP2003051306A JP 2003051306 A JP2003051306 A JP 2003051306A JP 2001239310 A JP2001239310 A JP 2001239310A JP 2001239310 A JP2001239310 A JP 2001239310A JP 2003051306 A JP2003051306 A JP 2003051306A
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JP
Japan
Prior art keywords
negative electrode
lead
weight
parts
carbon
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
JP2001239310A
Other languages
Japanese (ja)
Other versions
JP4364460B2 (en
Inventor
Atsushi Furukawa
淳 古川
Hikari Sakamoto
光 坂本
Kozo Sogabe
幸蔵 曽我部
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Furukawa Battery Co Ltd
Original Assignee
Furukawa Battery Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Furukawa Battery Co Ltd filed Critical Furukawa Battery Co Ltd
Priority to JP2001239310A priority Critical patent/JP4364460B2/en
Publication of JP2003051306A publication Critical patent/JP2003051306A/en
Application granted granted Critical
Publication of JP4364460B2 publication Critical patent/JP4364460B2/en
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Expired - Lifetime legal-status Critical Current

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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

Abstract

PROBLEM TO BE SOLVED: To provide a negative electrode for a lead-acid battery with improved high-rate discharge characteristic of a lead-acid battery used for an electric vehicle or the like. SOLUTION: A lead-alloy porous base substance is filled with active material mix paste obtained by adding 1-5 pts.wt. of conductive carbon and 1-5 pts.wt. of activated carbon to 100 pts.wt. of a negative electrode active material within 2-8 pts.wt. of the total addition quantity of the two kinds of carbon materials, and a chemically-unconverted negative electrode thereby obtained is subjected to a formation treatment.

Description

【発明の詳細な説明】 【０００１】 【発明の属する技術分野】本発明は、特に、アイドル・
ストップ、加速アシスト等高率放電を繰り返す電気自動
車(HEV)に適用し得る鉛蓄電池用負極に関する。 【０００２】 【従来の技術】最近、自動車用蓄電池を従来の12Ｖから
36Ｖに高電圧化する動きが活発化している。これは当
初、利便性や低コスト化を目的とした自動車搭載機器の
電動化に伴う電力需要急増への対応やワイヤーハーネス
重量抑制を目的として進められていた。しかしその後、
環境対策や低燃費化が大きな関心事となると共に、高効
率スタータ・ジェネレータが開発されたことで、36Ｖの
高電圧でもアイドル・ストップ機能は勿論、スタート・
アシストやブレーキ時のエネルギー回生が可能となり、
従来のHEV並の過酷な使われ方が予想される。ところ
で、これらの機能のうち、アイドル・ストップやスター
ト・アシストは蓄電池に低音での高率放電性能を要求す
るため、特に、鉛蓄電池が適していると見られていた。
しかし、アイドル・ストップ機能が求める放電性能は、
20Ah程度の電池であってもSOC70％、-15℃で10kw以上で
ある等非常に厳しく、従来の鉛蓄電池では大型化は避け
られない。特に負極は正極と比較して表面積が小さく、
急放電時は電解液の拡散が律速となり、分極が増大す
る。更にPSOCで利用されるために硫酸鉛が導電性を低下
させ、分極は益々増大することになる。この問題を解決
するために、従来の鉛蓄電池用負極板としてリグニンを
添加し、海綿状鉛の微細構造を形成することが知られて
いる。しかし、ここで形成される微細孔は0.1μｍオー
ダーで、比表面積も1ｍ2 ／ｇ程度と決して充分な細か
さを有するとは言えない。また、鉛蓄電池用負極板の導
電剤として粒状のカーボン粉末を例えば0.5％以上添加
することが提案されている。（特開平6-349486、特開平
7-6767、特開平7-201331参照）また、同様の目的で添加
する導電性カーボンを微細な繊維状にしたり、これを粒
粉と組み合わせたりすることも提案されている。（特開
平2-177260、特許2729644号、特許第2847761号参照）し
かし、このように負極の導電性のみの改善に注目して
も、所詮カーボンの導電性は金属鉛よりも低く、硫酸鉛
が多く存在するPSOCの導電性を改善するにとゞまる。 【０００３】 【発明が解決しようとする課題】上記のように、従来の
技術では、鉛蓄電池の負極に導電性を改善するべく導電
性カーボンを添加し、PSOCの導電性を改善はなされた
が、従来の上記の負極を用いる限り、鉛蓄電池に要求さ
れるアイドル・ストップ、スタート・アシスト等の低温
での高率放電性能を満足するなど、PSOC状態で適用され
る優れた鉛蓄電池は得られなかった。 【０００４】 【課題を解決するための手段】本発明は、上記従来の技
術の課題を解決し、上記の要求を満足する鉛蓄電池をも
たらす負極を提供するもので、負極活物質を主体とし導
電性カーボンを混練して成る活物質合剤ペーストを調製
するに当たり、負極活物質100重量部に対し、導電性カ
ーボンを1〜5重量部、活性炭を1〜5重量部の範囲で、且
つこれら両種の炭素材の合計量を2〜8重量部添加して活
物質合剤ペーストを調製することを特徴とし、これを鉛
合金多孔体に充填して得られる未化成の負極を化成して
成る。 【０００５】 【作用】本発明は、上記の構成において負極活物質に特
定量の導電性カーボンと活性炭を併せ添加することによ
り、その導電性カーボンによりPSOC状態で硫酸鉛が多く
存在する負極の分極を減少させると同時に、活性炭の導
電性を補うことができる。一方、活性炭により、導電性
カーボンと共に負極の電気二重層容量を増大し、放電直
後、0.1〜0.5秒目の電池電圧を高く維持することができ
る。導電性カーボンと活性炭の添加量は夫々1〜5重量部
の範囲であり、且つこれら両種の炭素材の合計が負極用
活物質100重量部に対し、8重量部を超えると、負極の海
綿状金属鉛の成長を阻害し、著しく放電性能を損ない、
放電直後、0.1〜0.5秒目の電池電圧を高く維持すること
ができない。 【０００６】 【発明の実施の形態】次に本発明の実施例を比較例と共
に詳述する。 (1)負極活物質合剤ペーストの調製と未化成の負極板の
製造：負極活物質として、鉛粉、酸化鉛、即ち、リサー
ジ(PbO)、四三酸化鉛(Pb3 O4 )などの各種酸化鉛からそ
の単独又は混合物を選択使用できるが、例えば、酸化鉛
(PbO)を用い、これを主体とし、該酸化鉛各100重量部に
対し、導電性カーボンとして比表面積70ｍ2 ／ｇ、粒径
35ｎｍのアセチレンブラック粉末を、活性炭として比表
面積2000ｍ2 ／ｇ、繊維径20μｍ、長さ100μｍ、平均
細孔径2〜5ｎｍのフェノール系活性炭繊維を、表１に示
すような夫々異なる添加量で且つ両種の炭素材、即ち、
導電性カーボンであるアセチレンブラックと活性炭であ
るフェノール系活性炭繊維との合計量が表１に示すよう
な夫々異なる添加量で添加し混合し、このとき、導電性
カーボンと同量の硫酸バリウムの粉末を同時に添加混合
した。次にこれにリグニンを水溶液として加え、続いて
イオン交換水を該酸化鉛各100重量部に対し10重量部と
比重1.36の希硫酸を10重量部を添加、混練して、表１に
示す各種の活物質合剤ペーストを調製した。その夫々の
負極活物質合剤ペーストのカップ密度は約135ｇ／2in3
であった。このように調製した各活物質合剤ペースト
を、夫々の鉛−カルシウム系合金から成る鋳造格子基板
に充填した後、40℃、湿度95％の雰囲気で24時間熟成
し、次で乾燥して各種の未化成の負極板を製造した。 (2)正極活物質合剤ペーストの調製と未化成の正極板の
製造：正極活物質として、酸化鉛(PbO)100重量部にイオ
ン交換水10重量部、続いて比重1.27の希硫酸10重量部を
加え乍ら混練して正極用活物質合剤ペーストを製造し
た。このペーストのカップ密度は約140ｇ／2in3であっ
た。このペーストを同様の鉛−カルシウム系合金から成
る鋳造格子基板に充填した後、40℃、湿度95％の雰囲気
で24時間熟成し、次で乾燥して多数の未化成の正極板を
製造した。 (3)本発明の負極を具備した鉛蓄電池と比較用の負極を
具備した鉛蓄電池の製造：上記に製造した各種の未化成
の負極板の夫々と上記に製造した１種類の未化成の正極
板との所望枚数を、微細なガラス繊維に約10重量部のシ
リカ粉末を混在結着して成る20kPa加圧時の厚みが0.8ｍ
ｍのリテーナーマットセパレータを介して積層し、且つ
同極性同志の耳列を溶接して成る各種の極板群を組み立
て、その夫々を各PP製の電槽に入れ、ヒートシールによ
りPP製の電槽蓋を施し、次で、放電状態での短絡防止用
に硫酸ナトリウムを20ｇ／ｌ添加溶解した比重1.20の硫
酸電解液を夫々の電池内に所定量注入し、その全量を極
板群に含浸せしめた。この電解液の注入は、極板群の理
論空間体積の100％を注入した。これらの電池を40℃の
水槽において、理論容量の200％過充電して電槽化成を
行い、2Ｖのシール型鉛蓄電池を夫々製造した。夫々の
電池の電解液の比重は1.260であった。化成後に行った
各電池の容量試験で5時間率容量は20Ahであった。 (4)低温高率放電性能の評価：このように製造した上記
の各種の電池の夫々を25℃、5時間率電流で完全充電し
た後、5時間率電流でSOCを70％に調整した。即ち、6Ah
分の放電を行った。次に、-15℃で16時間放置した後、3
00Ａで放電し、0.5秒目のセル電圧を測定した。低温高
率放電性能は、0.5秒目電圧が1.67Ｖ／セル(30Ｖ／36Ｖ
電池)以上必要が望ましい。上記性能試験の測定結果
は、下記表１に示す通りであった。 【０００７】 【表１】 【０００８】負極用活物質に導電性カーボンと活性炭を
添加し、負極に生成する硫酸鉛の結晶粒子間に導電性カ
ーボンと活性炭の両者が混在することにより、導電性を
付与すると同時に負極全体に電気二重層容量をもたら
す。導電性カーボンも、アセチレンブラックの他、炭素
繊維、粉状又は繊維状グラファイトなど所望の材料を選
択使用できる、その寸法は、ｎｍのオーダーが好まし
い。 【０００９】上記の２種類の炭素材を使用する場合、導
電性カーボンの添加量及び活性炭の添加量共に負極用活
物質100重量部に対し1〜5重量部であり、導電性カーボ
ンの添加量が1重量部未満では導電性が不充分であり、5
重量部を超えると導電材としての効果が飽和し、活物質
が減り容量が低下する。また、活性炭の添加量が1重量
部未満では電気二重層容量の増加が不充分であり、5重
量部を超えると効果が飽和し、活物質が減り容量が低下
する。而もこの上記の夫々の炭素材の添加量の範囲にお
いて、両種の炭素材を合わせた添加量は、2〜8重量部の
範囲でなければならない。この範囲を逸脱すると、上記
表１に明らかなように、目標とする低温高率放電性能、
高率放電後0.5秒時のセル電圧1.67Ｖ以上が得られな
い。 【００１０】 【発明の効果】請求項１に係る発明による本発明の負極
を鉛蓄電池に用いることにより、PSOC状態での放電特性
を大幅に改善でき、優れた電気自動車、その他の高率放
電を要求する各種の用途に用いることができる。DETAILED DESCRIPTION OF THE INVENTION [0001] TECHNICAL FIELD The present invention relates to an idle
Electric automatic that repeats high-rate discharge such as stop and acceleration assist
The present invention relates to a negative electrode for a lead storage battery applicable to a vehicle (HEV). [0002] 2. Description of the Related Art Recently, a storage battery for an automobile has been increased from the conventional 12V.
The trend to increase the voltage to 36V is increasing. This is
For the first time, automotive equipment for convenience and cost reduction
Respond to the rapid increase in power demand due to electrification and wire harnesses
It was being pursued to reduce weight. But then
Environmental measures and low fuel consumption are of great interest, and
With the development of the rate starter generator, 36V
The start / stop function as well as the idle / stop function even at high voltage
Energy regeneration during assist and braking becomes possible,
It is expected to be used as severely as conventional HEVs. Place
Among these functions, idle stop and star
Assist requires storage batteries to have high-rate discharge performance at low tones
Therefore, lead storage batteries have been considered to be particularly suitable.
However, the discharge performance required by the idle stop function is
Even with batteries of about 20Ah, SOC 70%, at -15 ° C with 10kw or more
It is very strict, so do not increase the size of conventional lead-acid batteries
I can't. In particular, the negative electrode has a smaller surface area than the positive electrode,
At the time of sudden discharge, diffusion of the electrolyte is rate-limiting and polarization increases.
You. Lead sulphate lowers conductivity for use in PSOC
The polarization will increase further. Solve this problem
Lignin as a conventional negative plate for lead-acid batteries
Known to add and form spongy lead microstructure
I have. However, the micropores formed here are 0.1 μm
With a specific surface area of 1mTwo/ G is enough fine
I can not say that it has. In addition, the introduction of negative electrode plates for lead-acid batteries
Add 0.5% or more of granular carbon powder as electric agent
It has been proposed to. (Japanese Unexamined Patent Publication No. 6-349486,
7-6767, see JP-A-7-201331) Also added for the same purpose
Conductive carbon to be made into fine fibrous
Combinations with flour have also been proposed. (JP
Hei 2-177260, Japanese Patent No. 2729644, Japanese Patent No. 2847721)
However, focusing on improving only the conductivity of the negative electrode,
Even after all, the conductivity of carbon is lower than that of metallic lead,
Only to improve the conductivity of PSOCs, where many are present. [0003] As described above, the conventional
In technology, the negative electrode of lead-acid batteries
Added conductivity carbon to improve the conductivity of PSOC
However, as long as the above-mentioned conventional negative electrode is used,
Low temperature such as idle stop and start assist
Satisfies high-rate discharge performance in
No good lead-acid battery was obtained. [0004] SUMMARY OF THE INVENTION The present invention relates to the above-mentioned conventional technology.
Technology to solve the problems of
It provides a negative electrode that can be used mainly for negative electrode active materials.
Preparation of active material mixture paste by kneading conductive carbon
In doing so, 100 parts by weight of the negative electrode active material
1 to 5 parts by weight of carbon, 1 to 5 parts by weight of activated carbon, and
Two to eight parts by weight of the total amount of these two types of carbon materials
It is characterized by preparing a material mixture paste,
Chemical formation of unformed negative electrode obtained by filling in porous alloy
Become. [0005] According to the present invention, there is provided a negative electrode active material having the above structure.
By adding a certain amount of conductive carbon and activated carbon together
Lead carbon in the PSOC state due to the conductive carbon
At the same time as reducing the polarization of the existing negative electrode,
It can supplement the electrical properties. On the other hand, conductive carbon
Increases the electric double layer capacity of the negative electrode together with carbon,
After 0.1-0.5 seconds, the battery voltage can be kept high
You. 1 to 5 parts by weight each of conductive carbon and activated carbon
And the sum of these two types of carbon materials is
If the amount exceeds 8 parts by weight with respect to 100 parts by weight of the active material,
Inhibits the growth of flocculent metal lead, significantly impairing discharge performance,
Immediately after discharging, keep the battery voltage high for 0.1 to 0.5 seconds.
Can not. [0006] Next, an example of the present invention will be described together with a comparative example.
Will be described in detail. (1) Preparation of negative electrode active material mixture paste and unformed negative electrode plate
Manufacture: Lead powder, lead oxide, ie, Risa
Di (PbO), Lead trioxide (PbThreeOFour ) Etc.
Can be used alone or as a mixture, for example, lead oxide
(PbO), which is mainly used, and 100 parts by weight of the lead oxide
On the other hand, specific surface area 70m as conductive carbonTwo/ G, particle size
35nm acetylene black powder as activated carbon
Area 2000mTwo/ G, fiber diameter 20μm, length 100μm, average
The phenolic activated carbon fibers having a pore diameter of 2 to 5 nm are shown in Table 1.
Such different addition amounts and both types of carbon materials, namely,
Acetylene black, which is conductive carbon, and activated carbon
As shown in Table 1
Each with a different amount of addition and mixing.
Simultaneously add and mix the same amount of barium sulfate powder as carbon
did. Then add lignin as an aqueous solution to this, followed by
10 parts by weight of ion-exchanged water for each 100 parts by weight of the lead oxide
10 parts by weight of diluted sulfuric acid having a specific gravity of 1.36 was added and kneaded, and
The various active material mixture pastes shown below were prepared. Their respective
The cup density of the negative electrode active material mixture paste is about 135g / 2in3
Met. Each active material mixture paste thus prepared
A cast lattice substrate made of each lead-calcium alloy
After filling, aged for 24 hours in an atmosphere of 40 ° C and 95% humidity
Then, it was dried to produce various unformed negative electrode plates. (2) Preparation of positive electrode active material mixture paste and unformed positive electrode plate
Production: 100 parts by weight of lead oxide (PbO)
10 parts by weight of exchange water and 10 parts by weight of dilute sulfuric acid with a specific gravity of 1.27
And kneading the mixture to produce a positive electrode active material mixture paste.
Was. The cup density of this paste is about 140g / 2in3.
Was. This paste was made from a similar lead-calcium alloy.
After filling the casting lattice substrate, the atmosphere at 40 ° C and 95% humidity
For 24 hours, and then dried to form a large number of unformed cathode plates.
Manufactured. (3) a lead-acid battery provided with the negative electrode of the present invention and a negative electrode for comparison
Manufacture of equipped lead storage batteries: Various types of non-chemical products manufactured above
Each of the negative electrode plates and one type of unformed positive electrode manufactured above
Apply the desired number of sheets to a glass fiber with about 10 parts by weight
0.8m thickness when pressurized at 20kPa and mixed with Rica powder
m via a retainer mat separator, and
Assembling various electrode groups by welding ear rows of same polarity
Each of them into each PP battery case and heat seal them.
Cover with a battery case made of PP, and then for short-circuit prevention in the discharge state
20 g / l of sodium sulfate was added to and dissolved in sulfuric acid with a specific gravity of 1.20.
A predetermined amount of the acid electrolyte is injected into each battery, and the entire amount is
The plate group was impregnated. The injection of this electrolyte is
100% of the theoretical volume was injected. Keep these batteries at 40 ° C
In a water tank, overcharge 200% of the theoretical capacity to form a battery case.
As a result, 2 V sealed lead-acid batteries were manufactured. Each
The specific gravity of the battery electrolyte was 1.260. Went after chemical formation
In the capacity test of each battery, the 5-hour rate capacity was 20 Ah. (4) Evaluation of low-temperature high-rate discharge performance:
Fully charged at 25 ° C, 5 hour rate current
After that, the SOC was adjusted to 70% with a 5-hour rate current. That is, 6Ah
Minutes of discharge. Next, after leaving at -15 ° C for 16 hours, 3
Discharge was performed at 00 A, and the cell voltage at 0.5 seconds was measured. Low temperature high
As for the rate discharge performance, the voltage at 0.5 second is 1.67V / cell (30V / 36V
Battery) is necessary. Measurement results of the above performance test
Was as shown in Table 1 below. [0007] [Table 1] [0008] Conductive carbon and activated carbon are used as the negative electrode active material.
The conductive powder is added between the lead sulfate crystal particles formed on the negative electrode.
Carbon and activated carbon are mixed to improve conductivity.
At the same time, the electric double layer capacity is brought to the whole negative electrode
You. Conductive carbon is not only acetylene black, but also carbon.
Select desired material such as fiber, powdery or fibrous graphite
Can be used selectively, its dimensions are preferably on the order of nm
No. When the above two types of carbon materials are used,
Both the amount of conductive carbon added and the amount of activated carbon added
1 to 5 parts by weight based on 100 parts by weight of the substance,
If the added amount of the component is less than 1 part by weight, the conductivity is insufficient, and 5
Exceeding parts by weight saturates the effect as a conductive material,
And the capacity decreases. Also, the amount of activated carbon added is 1 weight
Less than 5 parts, the increase of the electric double layer capacity is insufficient,
Exceeding the parts, the effect is saturated, the active material decreases and the capacity decreases
I do. Also, the range of addition of each of the above carbon materials is within the range.
The combined amount of both types of carbon materials is 2 to 8 parts by weight.
Must be in range. If you deviate from this range,
As apparent from Table 1, the target low-temperature high-rate discharge performance,
A cell voltage of 1.67 V at 0.5 seconds after high-rate discharge cannot be obtained.
No. [0010] The negative electrode according to the present invention according to the first aspect of the present invention.
Discharge characteristics in the PSOC state by using
Can significantly improve the performance of excellent electric vehicles and other high emission rates
It can be used for various applications that require electricity.

───────────────────────────────────────────────────── フロントページの続き (72)発明者 曽我部 幸蔵 福島県いわき市常磐下船尾町杭出作23−６ 古河電池株式会社いわき事業所内 Ｆターム(参考） 5H050 AA02 BA09 CA06 CB02 CB15 EA10 FA16 GA10 GA15 GA23 HA01    ────────────────────────────────────────────────── ─── Continuation of front page    (72) Inventor Kozo Sogabe             23-6 Tsukushi, Funabashi-cho, Joban-shi, Iwaki-shi               Furukawa Battery Co., Ltd. Iwaki Office F-term (reference) 5H050 AA02 BA09 CA06 CB02 CB15                       EA10 FA16 GA10 GA15 GA23                       HA01

Claims (1)

【特許請求の範囲】 【請求項１】 負極活物質を主体とし導電性カーボンを
混練して成る活物質合剤ペーストを調製するに当たり、
負極活物質100重量部に対し、導電性カーボンを1〜5重
量部、活性炭を1〜5重量部の範囲で、且つこれら両種の
炭素材の合計量を2〜8重量部添加して活物質合剤ペース
トを調製することを特徴とし、これを鉛合金多孔体に充
填して得られる未化成の負極を化成して成る鉛蓄電池用
負極。Claims 1. In preparing an active material mixture paste composed mainly of a negative electrode active material and kneaded with conductive carbon,
To 100 parts by weight of the negative electrode active material, 1 to 5 parts by weight of conductive carbon, 1 to 5 parts by weight of activated carbon, and 2 to 8 parts by weight of the total amount of both types of carbon materials are added to activate. A negative electrode for a lead storage battery, comprising preparing a material mixture paste, and forming an unformed negative electrode obtained by filling the mixture into a lead alloy porous body.
JP2001239310A 2001-08-07 2001-08-07 Negative electrode for lead acid battery Expired - Lifetime JP4364460B2 (en)

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