WO2013122132A1 - 鉛蓄電池用正極板及び該極板の製造方法並びにこの正極板を用いた鉛蓄電池 - Google Patents

鉛蓄電池用正極板及び該極板の製造方法並びにこの正極板を用いた鉛蓄電池 Download PDF

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WO2013122132A1
WO2013122132A1 PCT/JP2013/053505 JP2013053505W WO2013122132A1 WO 2013122132 A1 WO2013122132 A1 WO 2013122132A1 JP 2013053505 W JP2013053505 W JP 2013053505W WO 2013122132 A1 WO2013122132 A1 WO 2013122132A1
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Prior art keywords
active material
positive electrode
electrode plate
lead
mass
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PCT/JP2013/053505
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English (en)
French (fr)
Japanese (ja)
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一郎 向谷
剛生 坂本
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新神戸電機株式会社
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Priority to CN201380005144.XA priority Critical patent/CN104221189B/zh
Priority to JP2013558721A priority patent/JP6060909B2/ja
Publication of WO2013122132A1 publication Critical patent/WO2013122132A1/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
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/14—Electrodes for lead-acid accumulators
    • H01M4/16—Processes of manufacture
    • 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
    • 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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/56—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of lead
    • H01M4/57—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of lead of "grey lead", i.e. powders containing lead and lead oxide
    • 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
    • H01M4/64—Carriers or collectors
    • H01M4/66—Selection of materials
    • H01M4/68—Selection of materials for use in lead-acid accumulators
    • 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 positive electrode plate for a lead storage battery and a lead storage battery using the positive electrode plate.
  • Control valve-type lead-acid batteries are inexpensive and highly reliable, and are therefore used for emergency power supply facilities such as uninterruptible power supplies and power storage.
  • a positive electrode plate used for a control valve type lead-acid battery a paste type positive electrode plate in which a paste-like active material is filled in a lead alloy grid and aged and dried is generally used.
  • the paste-like active material is mainly made of lead and lead oxide, and is prepared in paste form by mixing lead powder containing basic lead sulfate with dilute sulfuric acid and water as required. Various prescriptions have been adopted.
  • Patent Document 1 After a paste-form active material is filled in a lattice, first preparation of a paste type positive electrode plate, 2 It is described that the two-stage aging and drying are performed.
  • Patent Document 2 describes that the lifetime is extended by setting the volume of the lattice body in the paste type positive electrode plate to 15 to 30% by volume.
  • the lead storage battery using the paste type positive electrode plate is strongly required to have a high capacity and a long life. However, in general, the two are in a conflicting relationship.
  • a technique of increasing the porosity of the active material layer of the positive electrode plate is effective.
  • increasing the porosity reduces the strength of the active material as a structure.
  • the adhesion of the active material to the lattice is weakened, and as a result, the active material is easily removed from the lattice and the life is shortened.
  • Patent Document 1 the method of generating tetrabasic lead sulfate or tribasic lead sulfate in the active material in the aging / drying process as shown in Patent Document 1 may not provide sufficient characteristics.
  • An object of the present invention is to provide a positive electrode plate for a lead storage battery that is excellent in maintaining a high capacity from the beginning and contributes to a long life, and a lead storage battery using the positive electrode plate.
  • the positive electrode plate for a lead storage battery according to the present invention is a positive electrode plate in which a lattice body is filled with an active material, the active material has the following physical property values, and the lattice body has the following alloy composition: Is.
  • the positive electrode active material when passing through one from the side to the other side with a pressure difference between 0.05MPa water of the active material layer in the charged state, the water 100ml transmission time per area 25 mm 2 with a thickness 5mm
  • the average particle size of the active material particles in the active material layer and the orientation of the active material particles are determined so as to be in the range of 1 to 10 minutes.
  • the grid of the positive electrode plate is made of a lead alloy having a Ca (calcium) content of 0.05 to 0.11 mass% and an Sn (tin) content of 1.1 to 1.8 mass%.
  • the present invention by determining the average particle size of the active material particles and the orientation of the active material particles in the active material layer so that the time for water to permeate the charged positive electrode active material is in the above range, The ratio of the gap between the discontinuous three-dimensional structure formed between the material particles and the gap between the three-dimensional structure continuous in the thickness direction of the active material is within an appropriate range.
  • the lead storage battery using the positive electrode plate for the lead storage battery of the present invention is durable. Excellent long life.
  • the strength of the lattice increases and the structure near the surface of the lattice stabilizes. Corrosion elongation of the metal is reduced, and the adhesion between the active material and the lattice is increased.
  • the lead acid battery using the positive electrode plate for the lead acid battery of the present invention is more durable and has a long life.
  • the lattice body is made of a lead alloy further containing Ag (silver) and having a content of 0.005 to 0.05 mass%.
  • the positive electrode grid is made of a lead alloy containing Ag (silver) in the above range, the metal structure of the grid is difficult to recrystallize even under a high temperature (eg, 50 ° C. or higher) environment. A conductive path is ensured in the bonding layer at the interface between the material and the lattice, and the life characteristics are further improved.
  • the positive electrode active material can be prepared from a lead powder containing tetrabasic lead sulfate.
  • the positive electrode active material is prepared from lead powder containing tetrabasic lead sulfate, it becomes easier to control the growth rate and size of the crystal particles in the active material, and the aging condition of the active material having a predetermined permeation time In addition, the aging time can be easily shortened.
  • the active material particles in the specific active material layer have, for example, an average particle size in the major axis direction of 20 to 100 ⁇ m, and the amount of the active material particles whose major axis extends in the thickness direction of the active material layer intersects the thickness direction. It is preferable that the orientation is determined so as to be smaller than the amount of the active material particles having a longer diameter. With such an orientation, the initial capacity of the lead-acid battery (initial capacity) can be made higher than that of a positive electrode plate having an active material layer in which active material particles are randomly oriented, and durability can be improved. Can be higher. When the average particle size in the major axis direction is smaller than 20 ⁇ m, the gap between particles becomes too small, and when the average particle size in the major axis direction is larger than 100 ⁇ m, the gap between particles becomes too large.
  • the positive electrode plate for a lead storage battery according to the present invention is prepared, for example, by filling an active material paste containing active material particles made of lead powder into a grid body to produce an undried positive electrode plate.
  • the undried positive electrode plate aged in the first aging step is subjected to a second aging step under the aging conditions of temperature: 60 ° C. ⁇ 5 ° C., relative humidity: 95% or more, time: 18 hours ⁇ 1 hour. carry out.
  • the non-dried positive electrode plate aged in the second aging step is further subjected to a drying step under the conditions of temperature: 80 ° C. ⁇ 5 ° C. and relative humidity: 40% ⁇ 5%.
  • the drying time in a drying process is 48 hours or less and 120 hours or less.
  • the positive electrode plate for a lead storage battery of the present invention in which the positive electrode active material is prepared from a lead powder containing tetrabasic lead sulfate has, for example, a Ca (calcium) content of 0.05 to 0.11.
  • a lattice is manufactured from a lead alloy having a mass%, a Sn (tin) content of 1.1 to 1.8 mass%, and an Ag (silver) content of 0.005 to 0.05 mass%.
  • An active material paste containing active material particles made of lead powder containing lead is filled in a lattice body to produce an undried positive electrode plate.
  • an undried positive electrode plate can be obtained by carrying out the aging step under the aging conditions of temperature: 35 ° C. ⁇ 5 ° C., relative humidity: 90% or more, and time: 24 ⁇ 1 hour.
  • the present invention can be understood as a lead storage battery using the positive electrode plate for a lead storage battery of the present invention.
  • the permeation time of 100 ml of water per area of 25 mm 2 is 5 mm thick. Since the average particle diameter of the active material particles and the orientation of the active material particles in the active material layer are determined so as to be in a range of up to 10 minutes, the gap between the active material particles can be appropriately secured, and the gap By sufficiently diffusing the electrolytic solution, a high capacity can be maintained from the initial state. And since the coupling
  • the strength of the lattice increases and the structure near the surface of the lattice stabilizes. Corrosion elongation is reduced, the adhesion between the active material and the grid is maintained, and a lead-acid battery having a higher durability and a longer life can be obtained.
  • FIG. 1 The schematic of the testing apparatus which measures the time for water to permeate
  • (A) to (D) schematically show the orientation states of the particles corresponding to “extremely strong”, “strong”, “medium” and “random” in the “particle orientation” column of Table 1, respectively.
  • FIG. 1 The schematic of the testing apparatus which measures the time for water to permeate
  • (A) to (D) schematically show the orientation states of the particles corresponding to “extremely strong”, “strong”, “medium” and “random” in the “particle orientation” column of Table 1, respectively.
  • ⁇ Lattice> As the lattice used in the present invention, either a lattice formed by a casting method or a lattice formed by an expanding method can be used, and any lattice can be used as long as it can hold an active material described later.
  • the body structure is not particularly limited.
  • lead is the main raw material, and both calcium and tin are added as alloy components to this. Self-discharge can be suppressed by adding calcium.
  • the lattice is easily corroded, but this can be suppressed by adding tin.
  • the amount of tin added is large, tin is unevenly distributed in the grain boundaries of the metal structure, causing intergranular corrosion due to stress corrosion, and at the same time, the adhesion between the active material and the lattice is reduced, resulting in a short life. It is known that it is easy to become. Therefore, the calcium content is set to 0.05 to 0.11% by mass, and the tin content is set to 1.1 to 1.8% by mass.
  • the positive electrode lattice body may preferably further be made of a lead alloy containing silver.
  • a lead alloy containing silver By containing silver, the metal structure of the lattice becomes difficult to recrystallize, and the conductive path formed in the bonding layer at the interface between the active material and the lattice is less likely to collapse.
  • the silver content 0.005% by mass or more, an effect that the metal structure of the lattice body becomes difficult to recrystallize appears.
  • the content exceeds 0.05% by mass, a non-uniform corrosion phenomenon due to the segregation of Ag appears and the cycle life is reduced, so the amount of silver added is 0.005 to 0.05% by mass. It is preferable to be in the range.
  • aluminum or the like can be added to the positive electrode grid as an alloy component.
  • ⁇ Positive electrode active material> When the positive electrode active material used in the present invention passes water with a pressure difference of 0.05 MPa from one side to the other side of the active material layer in a charged state, it permeates 100 ml of water per 5 mm in thickness and 25 mm 2 in area. The average particle diameter of the active material particles in the active material layer and the orientation of the active material particles are determined so that the time is in the range of 1 to 10 minutes.
  • parameters such as active material density, maximum particle size, and average pore size have been used as indicators for determining the physical properties of the active material.
  • the target active material characteristics only by controlling these parameters.
  • the desired performance can be exhibited by grasping the physical properties of the active material from the permeation time of water and limiting the permeation time.
  • the average particle diameter of the active material and the orientation of the active material have a great influence on the water permeation time. The present invention is based on such knowledge.
  • the water permeation time that is, the water permeation resistance of the active material depends on the diameter of the pores formed in the active material layer, the volume of the pores, the average particle diameter of the active material particles, and the orientation of the active material particles. It is a parameter.
  • the positive electrode active material used in the present invention is preferably prepared from a lead powder containing tetrabasic lead sulfate.
  • lead powder containing metal lead and lead oxide as a main component, or lead powder containing red lead as necessary is kneaded with water and dilute sulfuric acid, tribasic lead sulfate and A pasty active material mainly composed of lead oxide can be prepared. After this is filled in the lattice, it undergoes aging and drying steps to obtain an unformed positive electrode plate. At this time, if the positive electrode active material is prepared from a lead powder containing tetrabasic lead sulfate, the aging process and battery cell formation necessary for the active material to be a positive electrode plate having predetermined physical property values (permeation time) The process can be simplified and the time can be shortened.
  • the aging time is about 7 times longer and the battery case formation time is required for the active material to be a positive electrode plate having a predetermined physical property value (permeation time). Is expected to be about twice as long.
  • the transmission time specified in the present invention can be measured, for example, using the test apparatus shown in FIG.
  • a pressure gauge 4, a pressure regulating valve 5, and a cold trap 6 are connected in series from a side close to the Buchner funnel 2 between the Buchner funnel 2 and a vacuum pump 3 for evacuating the Buchner funnel 2. It is connected to the.
  • the cold trap 6 is used to prevent moisture and the like from entering the vacuum pump 3.
  • a positive electrode grid having a long side of 300 mm and a short side of 200 mm made of a lead-calcium-tin alloy (calcium: 0.08 mass%, tin: 1.5 mass%, the balance being substantially lead) was cast.
  • a positive electrode paste active material B was prepared in the same manner as described above except that 2.5% by mass of the lead powder was replaced with tetrabasic lead sulfate.
  • the moisture content of the positive electrode paste-like active material is 11% by mass, and the density is 5.0 g / cm 3 .
  • ⁇ Preparation of positive electrode plate> A plurality of positive electrode plates filled with the paste-like active material A described above and a plurality of positive electrode plates filled with the paste-like active material B described above were produced with respect to the lattice body described above. And in order to obtain the positive electrode active material from which the physical property of permeation
  • temperature 80 ° C.
  • relative humidity 40%
  • time 48 hours to 120 hours (drying process).
  • temperature 80 ° C.
  • relative humidity 40%
  • time 48 hours to 120 hours (drying process).
  • the negative electrode plate used was obtained by adding 0.3% by mass of carbon black to lead powder containing 75% by mass of lead monoxide, and adding 90% by mass of 10% by mass of 40% sulfuric acid, water and a negative electrode additive.
  • the negative electrode paste-like active material kneaded in this manner is obtained by filling a grid with a long side of 300 mm and a short side of 200 mm.
  • the battery case was formed under the following various conditions.
  • Table 1 also shows the average particle size and orientation of the active material particles of the positive electrode active materials of the produced lead storage batteries 1 to 7.
  • the average particle size and orientation of the active material particles were measured and evaluated based on the analyzed cross-sectional shape by analyzing the cross-sectional shape of the image taken with a microscope using image analysis software.
  • the average particle diameter was calculated based on the long diameter (average length dimension in the long axis direction of the particles).
  • FIG. 2A to 2D schematically show the orientation states of the particles corresponding to “extremely strong”, “strong”, “medium” and “random” in the column of “particle orientation” in Table 1, respectively.
  • the initial capacity is discharged at 10A and the capacity until the battery voltage drops to 1.85V is obtained.
  • Recovery charge after discharge is performed for 24 hours at 2.45 V-limited current of 10 A. This discharging / charging is repeated as one cycle for two cycles. This discharge test is based on “JISC8704-2-01”.
  • a sample obtained by disassembling the lead storage battery after taking out the above discharge / charge cycle for 2 cycles, taking out the positive electrode plate, collecting it from the positive electrode active material, washing it with water and drying it is used.
  • the cycle life is 100 cycles after repeating the above discharge / charge cycle for 2 cycles, discharging for 3 hours at 16 A, charging for 8 hours at 2.4 V-limited current 20 A, and resting for 1 hour. For each cycle, the capacity is confirmed by discharging at 10 A, and the number of cycles up to that time is counted with the time when 80% of the initial capacity is reached as the life.
  • the lead storage batteries 1 to 4 and 7 (Examples 1 to 5 according to the present invention) having a permeation time in the range of 1 to 10 minutes exhibit good performance with an initial capacity relative value of 100 or more. I understand that.
  • the initial capacity relative value is less than 100. More specifically, the lead storage battery 5 has a permeation time of 0.5 minutes, and the electrolyte solution retention of the positive electrode plate is inferior, so that the contact time between the positive electrode active material and the electrolyte solution cannot be sufficiently secured, The reaction of the active material is not sufficiently performed and the initial capacity is lowered.
  • the lead storage battery 6 has a permeation time of 12 minutes and the electrolyte solution retention of the positive electrode plate is good, but the electrolyte solution is not sufficiently diffused and the capacity is low.
  • the lead storage batteries 1 to 4 and 7 (Examples 1 to 5 according to the present invention) having a transmission time in the range of 1 to 10 minutes have good performance with a cycle life relative value of 100 or more. It can be seen that On the other hand, in the lead storage batteries 5 and 6 whose permeation time is outside the range of 1 to 10 minutes, the cycle life relative value is less than 100.
  • the orientation of the active material particles is “strong” to “medium”.
  • the ratio of the gap of the three-dimensional structure (electrolyte flow path) extending discontinuously in the thickness direction of the active material layer and the gap of the three-dimensional structure extending continuously in the thickness direction in the active material layer is appropriate. It has become a thing. Therefore, even if the average particle diameters of the active material particles are different, the electrolyte plate retainability of the positive electrode plate is good, and the electric path per unit volume is not relatively reduced. As a result, charges easily move, and a resistance layer containing lead oxide as a main component is not generated at the interface between the active material and the lattice. Therefore, an increase in electrical resistance and a decrease in capacity do not occur even when the discharge cycle proceeds.
  • the lead storage battery 5 having a permeation time of 0.5 minutes has a large average particle diameter of the active material particles of the positive electrode active material, and therefore has a three-dimensional structure gap (electrolyte flow path) formed between the active material particles. growing. Moreover, since the positive electrode active material uses the positive electrode paste active material B prepared from lead powder containing tetrabasic lead sulfate, the active material particles are extremely strongly oriented. For this reason, the gap in the three-dimensional structure (electrolyte flow path) formed between the active material particles tends to be continuous in the thickness direction of the active material layer.
  • the electrolyte solution retention of the positive electrode plate is inferior and the number of electrical paths per unit volume is relatively small. Therefore, the electrical paths are easily lost before the active material is sufficiently discharged.
  • a resistance layer mainly composed of lead oxide is generated at the interface between the active material and the lattice, and as the discharge cycle proceeds, the electric resistance rapidly increases and the capacity decreases, This leads to significant cycle deterioration.
  • the lead storage battery 6 having a permeation time of 12 minutes has a small average particle diameter of the active material particles of the positive electrode active material, and a three-dimensional structure gap formed between the active material particles is small. Further, since the active material particles are not in a state of being oriented in a specific direction (random), the ratio of formation of a three-dimensional structure gap continuous in the thickness direction of the active material layer is low. Therefore, even if the porosity is the same, the electrolyte solution retainability of the positive electrode plate is good, but the electrolyte solution is not sufficiently diffused, and the chargeability tends to be insufficient, and the cycle characteristics are deteriorated.
  • the aging conditions can be simplified and the aging time can be shortened compared to the lead storage battery 1 having the same transmission time.
  • the battery case formation time can also be shortened.
  • the same positive electrode active material has a smaller average particle size than the lead storage battery 5 prepared from lead powder containing tetrabasic lead sulfate, both the initial capacity and the cycle life are better than the lead storage battery 5. ing.
  • Table 2 shows a relative comparison value as a result of carrying out a cycle life test in the case where the calcium content and the tin content of the lead alloy constituting the positive electrode lattice body are changed.
  • the cycle life can be maintained when the tin content of the positive electrode lattice body is in the range of 1.1 to 1.8 mass%. .
  • the cycle life can be improved by adding silver to the lead alloy constituting the positive electrode grid.
  • the effect becomes remarkable by setting the silver content to 0.005% by mass or more.
  • the silver content exceeds 0.05% by mass (lead storage battery 21)
  • the silver content is preferably 0.05% by mass or less because the cycle life is reduced.

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
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  • Inorganic Chemistry (AREA)
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PCT/JP2013/053505 2012-02-14 2013-02-14 鉛蓄電池用正極板及び該極板の製造方法並びにこの正極板を用いた鉛蓄電池 WO2013122132A1 (ja)

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CN201380005144.XA CN104221189B (zh) 2012-02-14 2013-02-14 铅蓄电池用正极板和该极板的制造方法以及使用该正极板的铅蓄电池
JP2013558721A JP6060909B2 (ja) 2012-02-14 2013-02-14 鉛蓄電池用正極板及び該極板の製造方法並びにこの正極板を用いた鉛蓄電池

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JP2012-029294 2012-02-14

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JP2013211205A (ja) * 2012-03-30 2013-10-10 Furukawa Battery Co Ltd:The 鉛蓄電池用負極板、その製造方法及び鉛蓄電池
CN115842106A (zh) * 2023-02-20 2023-03-24 淄博火炬能源有限责任公司 铅酸电池板式正极及其制造工艺
US11894560B2 (en) 2019-09-27 2024-02-06 Gs Yuasa International Ltd. Lead-acid battery

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JP6940025B1 (ja) * 2019-09-30 2021-09-22 昭和電工マテリアルズ株式会社 鉛蓄電池
CN112002877B (zh) * 2020-07-23 2022-03-01 天能电池集团股份有限公司 一种板栅与活性物质界面的优化工艺

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US11894560B2 (en) 2019-09-27 2024-02-06 Gs Yuasa International Ltd. Lead-acid battery
CN115842106A (zh) * 2023-02-20 2023-03-24 淄博火炬能源有限责任公司 铅酸电池板式正极及其制造工艺

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JP6060909B2 (ja) 2017-01-25
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