WO2011077640A1 - 制御弁式鉛蓄電池 - Google Patents

制御弁式鉛蓄電池 Download PDF

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Publication number
WO2011077640A1
WO2011077640A1 PCT/JP2010/006892 JP2010006892W WO2011077640A1 WO 2011077640 A1 WO2011077640 A1 WO 2011077640A1 JP 2010006892 W JP2010006892 W JP 2010006892W WO 2011077640 A1 WO2011077640 A1 WO 2011077640A1
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WO
WIPO (PCT)
Prior art keywords
positive electrode
active material
electrode active
separator
control valve
Prior art date
Application number
PCT/JP2010/006892
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English (en)
French (fr)
Japanese (ja)
Inventor
佐々木健浩
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パナソニック株式会社
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Priority to JP2011517546A priority Critical patent/JPWO2011077640A1/ja
Priority to CN2010800035829A priority patent/CN102246344A/zh
Publication of WO2011077640A1 publication Critical patent/WO2011077640A1/ja

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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
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/06—Lead-acid accumulators
    • H01M10/12—Construction or manufacture
    • H01M10/121—Valve regulated lead acid batteries [VRLA]
    • 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
    • H01M10/06—Lead-acid accumulators
    • H01M10/12—Construction or manufacture
    • H01M10/16—Suspending or supporting electrodes or groups of electrodes in the case
    • 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
    • H01M10/06—Lead-acid accumulators
    • H01M10/18—Lead-acid accumulators with bipolar electrodes
    • 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 control valve type lead acid battery (hereinafter, simply referred to as “battery”).
  • Control valve type lead-acid batteries are broadly divided into trickle and cycle applications.
  • trickle applications the battery is always charged and discharged only during a power failure, as represented by an uninterruptible power supply.
  • the cycle application as represented by a power source for an electric vehicle, a charge / discharge cycle in which the battery is fully charged after receiving a deep discharge is repeated.
  • control valve-type lead-acid batteries have been mainly used for trickle applications.
  • the demand for a control valve type lead storage battery as a power source for electric vehicles has increased, and there is a demand for extending the life of the control valve type lead storage battery during cycle use.
  • Patent Document 1 a specific surface area of the cathode active material and 5.0m 2 /g ⁇ 8.0m 2 / g, and a specific surface area of the anode active material and 0.8m 2 /g ⁇ 1.4m 2 / g Moreover, it is shown that a lead-acid battery having excellent cycle life characteristics can be obtained by pressurizing at a group pressure of 50 kg / dm 2 or more in a state where the electrode group is housed in the battery case.
  • the present invention provides a control valve type lead storage battery having excellent cycle life characteristics.
  • the specific surface area of the positive electrode active material is 1.5 m 2 / g or more and 4.5 m 2 / g or less, and the average pore diameter of the separator is 1.5 ⁇ m or more and 2.5 ⁇ m or less. .
  • the specific surface area of the positive electrode active material is 2.0 m 2 / g or more and 3.5 m 2 / g or less, further excellent cycle life characteristics can be obtained.
  • the “specific surface area” is a specific surface area in a fully charged state, that is, a specific surface area of the active material after chemical conversion, and is measured according to the BET (Brunauer-Emmett-Teller) method.
  • the “average pore diameter” means the separator pore diameter when the separator is assembled to the battery, that is, the dimension of the separator when the dimension between the positive electrode plate and the negative electrode plate is reduced to the state assembled to the battery. It is a pore diameter and is a median diameter measured by a liquid injection method.
  • a known liquid for example, a liquid having a specific gravity similar to that of water
  • the cycle life characteristics are improved.
  • FIG. 1 is a cross-sectional view of a control valve type lead storage battery according to an embodiment of the present invention.
  • FIG. 2 is a table showing values of the specific surface area of the positive electrode active material and the average pore diameter of the separator in the battery produced in the example.
  • FIG. 3 is a table showing the value of the specific surface area of the positive electrode active material and the average pore diameter of the separator in the battery produced in the example.
  • FIG. 4 is a table showing the results of the cycle life test for the battery shown in FIG.
  • FIG. 5 is a table showing the results of the cycle life test for the battery shown in FIG.
  • FIG. 6 is a graph showing the results shown in FIG. 4 and FIG.
  • FIG. 1 is a cross-sectional view of a control valve type lead storage battery according to an embodiment of the present invention.
  • the control valve type lead storage battery 10 is configured such that a positive electrode plate 2 and a negative electrode plate 3 are accommodated in a battery case 1 via a separator 4.
  • the battery case 1 may be a battery case known as a battery case of a control valve type lead-acid battery, and is closed with a lid 5.
  • the lid 5 includes a control valve 8 composed of a valve cylinder 5a, a valve body 6 and a valve pressing plate 7.
  • the valve cylinder 5 a is provided on the lid 5 and extends in the longitudinal direction of the battery case 1.
  • the valve body 6 is attached to the valve cylinder 5a.
  • the valve pressing plate 7 is provided on the outer side of the lid 5 with respect to the valve body 6, and prevents the valve body 6 from dropping from the valve cylinder 5 a and applies an appropriate valve opening pressure to the control valve 8.
  • control valve 8 is not limited to the above configuration and the configuration shown in FIG.
  • the battery 10 may have a strap for connecting the same polar plates, and the battery case 1 preferably has a positive terminal and a negative terminal. Moreover, when the battery 10 is a monoblock type control valve type lead acid battery, it is preferable that the single cells are connected to each other via an inter-cell connector or the like.
  • a positive electrode current collector (not shown) is filled with a positive electrode active material (not shown).
  • the negative electrode current collector (not shown) is filled with a negative electrode active material (not shown). Z).
  • the current collector may be a known current collector as a current collector of a control valve type lead storage battery, and may be made of a Pb alloy.
  • the positive electrode current collector is made of a Pb alloy containing 1.0% by mass or more and 2.2% by mass or less of Sn and 0.05% by mass or more and 0.15% by mass or less of Ca.
  • a Pb alloy containing 0 mass% or more and 1.0 mass% or less of Sn and 0.05 mass% of Ca may be a grid (casting grid) made by casting, a grid made of expanded metal (expanded grid), or a grid (punching grid) made by punching.
  • a foil in which through holes are formed may be used.
  • the positive electrode active material is lead dioxide.
  • This positive electrode active material has a specific surface area of 1.5 m 2 / g or more and 4.5 m 2 / g or less, and a specific surface area of 2.0 m 2 / g or more and 3.5 m 2 / g or less. Preferably it is.
  • the positive electrode plate 2 is manufactured according to the following method. Water and dilute sulfuric acid are added and kneaded to a lead powder (mixture of metallic lead and lead oxide) obtained by a known technique. Thereby, a paste-like positive electrode active material is obtained. After filling the paste-like positive electrode active material into the positive electrode current collector, aging, drying, and chemical conversion are performed according to a known method. Thereby, the positive electrode 2 is obtained.
  • the amount of water or dilute sulfuric acid relative to the lead powder may be adjusted, or the sulfuric acid concentration in the dilute sulfuric acid may be adjusted.
  • Carbon may be added to the paste-like positive electrode active material. When carbon is added to the paste-like positive electrode active material, the carbon is oxidized during the formation, and vacancies are formed in the positive electrode active material. Further, tin sulfate, tin oxide, phosphate, or the like may be added to the paste-like positive electrode active material.
  • the negative electrode active material is metallic lead, and the specific surface area may be a value known as the specific surface area of the negative electrode active material of the control valve type lead-acid battery, for example, 0.7 m 2 / g or more and 2.0 m 2 / g. It is as follows.
  • the negative electrode plate 3 can be manufactured according to a known manufacturing method as a manufacturing method of the negative electrode plate 3 of the control valve type lead-acid battery.
  • capacitance of a negative electrode active material is larger than the capacity
  • the capacity difference may be a capacity difference known as a capacity difference of the control valve type lead storage battery.
  • the group pressure may be set so that the positive electrode plate 2 and the negative electrode plate 3 are in close contact with the separator 4.
  • the group pressure may be a known value as the group pressure of the control valve type lead storage battery, and may be, for example, 11.0 kPa or more and 40.0 kPa or less. If the group pressure is less than 11.0 kPa, the positive electrode plate 2 or the negative electrode plate 3 may not adhere to the separator 4. On the other hand, if the group pressure exceeds 40.0 kPa, the battery case 1 may need to be strengthened.
  • the separator 4 only needs to be chemically stable with respect to the electrolytic solution (dilute sulfuric acid), can hold a predetermined amount of the electrolytic solution, and can prevent a short circuit between the positive electrode plate 2 and the negative electrode plate 3. good.
  • the electrolytic solution dilute sulfuric acid
  • An example of a material that satisfies all of these requirements is a glass mat.
  • the separator 4 has an average pore diameter of 1.5 ⁇ m or more and 2.5 ⁇ m or less.
  • the diameter of the glass fiber, the basis weight of the glass fiber (the mass of the glass fiber), the content of the binder and the compression amount (before the electrode group is put in the battery case 1) At least one of the degree of compression in the group compression step may be changed, or silica or the like may be added to the separator 4.
  • the electrolytic solution (not shown) is impregnated and held in the pores formed in the positive electrode active material, the negative electrode active material, and the separator 4, and has a known composition as the composition of the electrolytic solution in the control valve type lead storage battery. If you do.
  • the battery case 1 may contain an amount of free electrolyte that does not interfere with the oxygen gas absorption reaction by the negative electrode plate 3.
  • the free electrolytic solution is an electrolytic solution that is not impregnated in any of the positive electrode active material, the negative electrode active material, and the separator 4.
  • the positive electrode active material in the present embodiment has a specific surface area of 1.5 m 2 / g or more and 4.5 m 2 / g or less.
  • the specific surface area of the positive electrode active material in this embodiment is smaller than the specific surface area of the conventional positive electrode active material (for example, the specific surface area in Patent Document 1), softening of the positive electrode active material due to repeated charge and discharge is prevented. Is done.
  • the reaction area of the positive electrode active material is reduced and the reaction efficiency is reduced.
  • the average pore diameter of the separator 4 is set to 1.5 ⁇ m or more and 2.5 ⁇ m or less to ensure the amount of the electrolyte solution in contact with the positive electrode active material.
  • the specific surface area of the positive electrode active material is 2.0 m 2 / g or more and 3.5 m 2 / g or less when the average pore size of the separator 4 is 1.5 ⁇ m or more and 2.5 ⁇ m or less, the cycle life characteristics are further improved. improves. This will be specifically described below.
  • the specific surface area of the positive electrode active material is less than 1.5 m 2 / g, the reason why the cycle life characteristics are deteriorated cannot be stated, but the following may be considered.
  • lead sulfate is deposited on the positive electrode plate 2 side, so that the reaction area of the positive electrode active material is reduced by the discharge.
  • the specific surface area of a positive electrode active material is less than 1.5 m ⁇ 2 > / g, it is thought that the reaction area of the positive electrode active material after discharge becomes remarkably small. For this reason, charging after discharging becomes extremely difficult, resulting in a decrease in charge acceptability. Therefore, it reaches the lifetime.
  • the following can be considered as the reason why the cycle life characteristics are lowered when the specific surface area of the positive electrode active material exceeds 4.5 m 2 / g.
  • the positive electrode active material is coarsened, thereby softening the positive electrode active material. Then, the bond strength between the positive electrode active materials is reduced, and the positive electrode active materials are dropped off.
  • the diameter of a positive electrode active material will become small when the specific surface area of a positive electrode active material exceeds 4.5 m ⁇ 2 > / g, the fall of the contact area of positive electrode active materials will be caused. Therefore, it is considered that the bonding force between the positive electrode active materials is weak even before repeated charging and discharging.
  • the bonding force between the positive electrode active materials is remarkably reduced, and therefore, the positive electrode active material is easily dropped or the timing at which the positive electrode active material is dropped is accelerated. .
  • the average pore diameter of the separator 4 When the average pore diameter of the separator 4 is less than 1.5 ⁇ m, the amount of electrolyte solution that can be held by the separator 4 increases. Therefore, at least half or more of the electrolytic solution supplied into the battery case 1 is absorbed by the separator 4, thereby reducing the amount of the electrolytic solution present on the surface of the positive electrode active material or the negative electrode active material. Therefore, the discharge reaction is difficult to occur.
  • the control valve 8 opens and causes liquid leakage. Thereby, since the water
  • the negative electrode plate 3 cannot absorb the oxygen gas generated in the positive electrode plate 2. Therefore, oxygen gas continues to be generated from the positive electrode plate 2, hydrogen gas continues to be generated from the negative electrode plate 3 (the control valve 8 continues to open), and the electrolytic solution decreases at an accelerated rate. Therefore, the lifetime is reached.
  • the average pore diameter of the separator 4 exceeds 2.5 ⁇ m, the amount of electrolyte solution that can be held by the separator 4 decreases. Therefore, the amount of electrolyte that can be supplied to the battery case 1 is reduced. Therefore, even in this case, the amount of the electrolytic solution present on the surface of the positive electrode active material or the negative electrode active material is reduced, so that the discharge reaction is less likely to occur.
  • the mechanical strength of the separator 4 is reduced. As long as the separator 4 has a predetermined mechanical strength, the separator 4 can prevent the positive electrode active material from having a decreased bonding force between the particles. However, if the mechanical strength of the separator 4 is low, it is difficult for the separator 4 to prevent the positive electrode active material from dropping with a reduced bonding force between the particles.
  • the average pore diameter of the separator 4 when the average pore diameter of the separator 4 is 1.5 ⁇ m or more and 2.5 ⁇ m or less, the amount of the electrolyte present in the vicinity of the surface of the positive electrode active material or the like can be ensured. Furthermore, if the specific surface area of the positive electrode active material is 2.0 m 2 / g or more and 3.5 m 2 / g or less, softening of the positive electrode active material due to repeated charge and discharge is prevented while ensuring a sufficient reaction area of the positive electrode active material. it can. Therefore, it is considered that the effect obtained by optimizing the average pore diameter of the separator 4 is sufficiently exhibited.
  • a control valve type lead-acid battery was prepared by variously changing the specific surface area of the positive electrode active material and the average pore diameter of the separator, and a cycle life test was performed on the battery.
  • a current collector was prepared.
  • a sheet made of a Pb alloy containing 1.6% by mass of Sn and 0.06% by mass of Ca was prepared, and this sheet was expanded. In this way, a positive electrode current collector was obtained.
  • seat which consists of a Pb alloy containing 0.25 mass% Sn and 0.07 mass% Ca was prepared, and the expansion process was performed with respect to this sheet
  • a paste-like active material was prepared. Water was added to and kneaded with lead powder (lead powder is composed of 30% by mass of Pb and 70% by mass of PbO), and further, kneaded while dropping dilute sulfuric acid having a sulfuric acid concentration of 40% by mass. In this way, a paste-like positive electrode active material was obtained.
  • carbon (conducting aid), barium sulfate (shrinking agent) and lignin sulfonic acid sodium salt (shrinking agent) are added to and mixed with the above lead powder, water is added and kneaded, and further dilute sulfuric acid is added dropwise While kneading. In this way, a paste-like negative electrode active material was obtained. Each kneading was performed using a ball mill.
  • the unformed positive electrode plate had a height (up and down direction of FIG. 1) of 67.0 mm, a width of 44.5 mm, and a thickness (left and right direction of FIG. 1) of 3.00 mm.
  • the unformed negative electrode plate had a height (up and down direction of FIG. 1) of 68.0 mm, a width of 44.5 mm, and a thickness (left and right direction of FIG. 1) of 1.90 mm.
  • a single cell was produced using 6 unformed positive plates and 7 unformed negative plates. At this time, a separator made of glass fiber was disposed between the unformed positive electrode plate and the unformed negative electrode plate. In this way, three single cells were produced. Each single cell was accommodated in the cell chamber of the battery case, the single cells were connected in series, and a predetermined single cell was connected to the terminal of the battery case. Then, after inject
  • the specific surface area of the negative electrode active material was 1.0 m 2 / g in any battery.
  • the specific surface area of the positive electrode active material was as shown in FIGS. Note that when the amount of water and dilute sulfuric acid added to the lead powder was increased to produce a paste-like positive electrode active material, the specific surface area of the positive electrode active material increased.
  • the average pore diameter of the separator was as shown in FIGS.
  • the diameter of the glass fiber and the basis weight of the glass fiber were changed to change the average pore diameter of the separator.
  • the group pressure applied to the separator was 14.7 kPa (20 kgf / dm 2 when converted to a non-SI unit system).
  • Cycle life test (1) Test method The following cycle life test was performed on each battery shown in FIGS. After performing high rate discharge (constant current discharge at 5.00 A, discharge end voltage is 5.25 V) in an atmosphere at 25 ° C. for 2 hours, constant current and constant voltage charge (charge voltage is 7.35 V, initial charge current) Was 4.50 A) for 12 hours. This was defined as one cycle, and the life was reached when the discharge capacity at high rate discharge reached 60%.
  • the average pore diameter of the separator is It was higher than the maximum value of the number of cycles (for example, the number of cycles of the battery D6) when it was outside the range of 1.5 ⁇ m to 2.5 ⁇ m.
  • the average pore size of the separator is 1.5 ⁇ m or more and 2.5 ⁇ m or less
  • the specific surface area of the positive electrode active material is 2.0 m 2 / g or more and 3.5 m 2 / g or less.
  • the specific surface area of the positive electrode active material is changed from 1.2 m 2 / g to 1.5 m 2 / g. Even if it was changed or the specific surface area of the positive electrode active material was changed from 4.5 m 2 / g to 5.0 m 2 / g, the cycle life characteristics were only slightly improved.
  • the specific surface area of the positive electrode active material is changed from 1.2 m 2 / g to 1.5 m 2 / g, or the ratio of the positive electrode active material
  • the cycle life characteristics were remarkably improved (the number of cycles became about 1.5 times or more). This is what the present inventor has discovered for the first time, and far exceeds the range that the inventor had originally anticipated. As a reason why such a result is obtained, the present inventor believes that there is a synergistic effect by optimization of the specific surface area of the positive electrode active material and optimization of the average pore diameter of the separator.
  • the present inventor confirmed that the same results as those shown in FIGS. 4 to 6 can be obtained if the specific surface area of the negative electrode active material is 0.7 m 2 / g or more and 2.0 m 2 / g or less. ing. That is, the results shown in FIGS. 4 to 6 are not limited to the case where the specific surface area of the negative electrode active material is 1.0 m 2 / g.
  • the present inventor has confirmed that the same results as those shown in FIGS. 4 to 6 can be obtained when the group pressure applied to the separator is 11.0 kPa or more and 40.0 kPa or less. That is, the results shown in FIGS. 4 to 6 are not limited to the case where the group pressure is 14.7 kPa.
  • the present invention is useful for a control valve type lead-acid battery and is suitable for cycle applications such as a power source for an electric vehicle.

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Secondary Cells (AREA)
  • Cell Separators (AREA)
PCT/JP2010/006892 2009-12-25 2010-11-25 制御弁式鉛蓄電池 WO2011077640A1 (ja)

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JP2011517546A JPWO2011077640A1 (ja) 2009-12-25 2010-11-25 制御弁式鉛蓄電池
CN2010800035829A CN102246344A (zh) 2009-12-25 2010-11-25 控制阀式铅蓄电池

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JP2009294166 2009-12-25

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2018018801A (ja) * 2016-07-29 2018-02-01 株式会社Ｇｓユアサ 鉛蓄電池
WO2018148484A1 (en) 2017-02-10 2018-08-16 Daramic, Llc Improved separators with fibrous mat, lead acid batteries using the same, and methods and systems associated therewith
US10522837B2 (en) 2013-11-29 2019-12-31 Gs Yuasa International Ltd. Lead-acid battery

Citations (5)

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Publication number Priority date Publication date Assignee Title
JPH07122266A (ja) * 1993-08-30 1995-05-12 Shin Kobe Electric Mach Co Ltd 鉛蓄電池用正極板及びその製造方法
JP2000030696A (ja) * 1998-07-09 2000-01-28 Shin Kobe Electric Mach Co Ltd 密閉形鉛蓄電池
JP2000133253A (ja) * 1998-10-28 2000-05-12 Shin Kobe Electric Mach Co Ltd 鉛蓄電池および鉛蓄電池の製造方法
JP2005216741A (ja) * 2004-01-30 2005-08-11 Furukawa Battery Co Ltd:The 密閉型鉛蓄電池用正極板および前記正極板を用いた密閉型鉛蓄電池
JP2006331755A (ja) * 2005-05-25 2006-12-07 Furukawa Battery Co Ltd:The 制御弁式鉛蓄電池

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JPS6091572A (ja) * 1983-10-24 1985-05-22 Yuasa Battery Co Ltd 密閉形鉛蓄電池
JPH10106526A (ja) * 1996-09-26 1998-04-24 G S Kasei Kogyo Kk 鉛電池用セパレータ及びその製造方法
JPH10189029A (ja) * 1996-12-24 1998-07-21 Japan Storage Battery Co Ltd 密閉形鉛蓄電池の製造方法

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Publication number Priority date Publication date Assignee Title
JPH07122266A (ja) * 1993-08-30 1995-05-12 Shin Kobe Electric Mach Co Ltd 鉛蓄電池用正極板及びその製造方法
JP2000030696A (ja) * 1998-07-09 2000-01-28 Shin Kobe Electric Mach Co Ltd 密閉形鉛蓄電池
JP2000133253A (ja) * 1998-10-28 2000-05-12 Shin Kobe Electric Mach Co Ltd 鉛蓄電池および鉛蓄電池の製造方法
JP2005216741A (ja) * 2004-01-30 2005-08-11 Furukawa Battery Co Ltd:The 密閉型鉛蓄電池用正極板および前記正極板を用いた密閉型鉛蓄電池
JP2006331755A (ja) * 2005-05-25 2006-12-07 Furukawa Battery Co Ltd:The 制御弁式鉛蓄電池

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10522837B2 (en) 2013-11-29 2019-12-31 Gs Yuasa International Ltd. Lead-acid battery
JP2018018801A (ja) * 2016-07-29 2018-02-01 株式会社Ｇｓユアサ 鉛蓄電池
WO2018148484A1 (en) 2017-02-10 2018-08-16 Daramic, Llc Improved separators with fibrous mat, lead acid batteries using the same, and methods and systems associated therewith

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CN102246344A (zh) 2011-11-16

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