CN111063894A - Rare earth grid alloy for lead-acid storage battery - Google Patents
Rare earth grid alloy for lead-acid storage battery Download PDFInfo
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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
- H01M4/64—Carriers or collectors
- H01M4/66—Selection of materials
- H01M4/68—Selection of materials for use in lead-acid accumulators
- H01M4/685—Lead alloys
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- 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
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- 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
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Abstract
The invention discloses a rare earth grid alloy for a lead-acid storage battery. The rare earth grid alloy comprises the following raw materials in percentage by weight: calcium: 0.10 to 0.14%, tin: 0.8-1.5%, aluminum: 0.02-0.05%, bismuth: 0.2-0.4%, RE: 0.05 to 0.15 percent, and the balance being Pb. When the rare earth element is added into the lead-based alloy for the lead-acid storage battery, the rare earth alloy has the advantages of a Pb-Sb system and a Pb-Ca system, effectively solves the problems of preparing a grid in the prior art, obviously improves the performance of the grid, improves the performance of the battery and prolongs the service life of the battery. And the problem of poor charging acceptance in winter is also solved. Has good application prospect in the field of lead-acid storage batteries.
Description
Technical Field
The invention relates to the technical field of lead-acid storage batteries, in particular to a rare earth grid alloy for a lead-acid storage battery.
Background
With the continuous development of new energy industry, the environment protection and the reasonable utilization of resources are more emphasized by the nation, the lead storage industry pursues high efficiency and practicability in development, pursues the high performance of lead-acid storage batteries, improves the service life, deep cycle and charging acceptance of batteries and the like, wherein the grid alloy plays an important role in the storage batteries, and the improvement of the alloy performance is an important direction.
The grid is a support of the lead-acid storage battery, can support active substances, serves as a carrier of the active substances, and can conduct and collect current, so that the industry has great requirements on the corrosion resistance and the conductivity of grid alloy, and the lead-calcium alloy is generally adopted in the positive grid alloy of the lead-acid storage battery at present. The lead-calcium alloy can replace lead-antimony alloy to become the main alloy used at present, and has the greatest advantages of relatively high hydrogen evolution overpotential of calcium, reduction of hydrogen evolution quantity of a battery cathode, reduction of water loss and good maintenance-free performance. However, the lead-calcium alloy has serious intergranular corrosion phenomenon, the calcium content is not easy to control, and particularly, a high-impedance passive film formed on the surface of a battery grid seriously hinders the progress of the charging and discharging process of the battery, the bonding capability with an active substance is reduced, so that the early capacity loss (PCL) phenomenon of the battery is aggravated, and the service life of the battery is greatly shortened, wherein the influence of a positive grid is the most.
For the above reasons, tin is generally added to the alloy in a high content, and the formed Pb — Sn intermetallic compound is distributed in the lead matrix in the form of precipitates while reducing the oxidation loss of calcium, thereby strengthening the lead alloy. However, the increase of the tin content increases the grain size of the alloy, and at the same time, part of tin is precipitated at the grain boundary, so that the intergranular corrosion phenomenon of the alloy is caused. Cadmium is added into the alloy to improve the hydrogen evolution potential of the alloy, reduce the corrosion degree and eliminate the brittle fracture of the grid, but the cadmium has toxicity, which has great limitation on the production.
Researchers find that the addition of the rare earth element has a good effect on a lead-acid storage battery grid, the added rare earth can form an intermetallic compound with lead, neutralize the intergranular tearing phenomenon of certain lead alloy, improve the tensile strength and the creep resistance of the alloy, improve the deep charging capability of the battery and improve the hydrogen evolution overpotential. The addition of the rare earth elements can increase the self-corrosion potential and the passivation potential of the lead-calcium alloy, improve the width and the over-passivation potential of the passivation region of the lead-calcium alloy and reduce the passivation current of the lead-calcium alloy.
Disclosure of Invention
The invention aims at the technical problems that: the grid prepared in the prior art has certain defects, and the performance and the practical application effect of the battery are influenced.
Aiming at the problems, the invention provides a rare earth grid alloy for a lead-acid storage battery. The grid has the advantages of Pb-Sb series and Pb-Ca series, overcomes the defects of grid alloy in the prior art, and obviously improves the performance and service life of the grid alloy and the battery prepared from the grid alloy.
The invention is realized by the following technical scheme
The rare earth grid alloy for the lead-acid storage battery comprises the following raw materials in percentage by weight: calcium: 0.10 to 0.14%, tin: 0.8-1.5%, aluminum: 0.02-0.05%, bismuth: 0.2-0.4%, RE: 0.05 to 0.15 percent, and the balance being Pb.
The rare earth grid alloy for the lead-acid storage battery is characterized in that Pb is refined lead with the purity of more than 99.95%.
The RE is selected from one or a mixture of more of La, Nd and Sm.
The preparation method of the rare earth grid alloy for the lead-acid storage battery comprises the following steps:
preparing Pb-Ca mother alloy, tin, aluminum, bismuth, RE and refined lead Pb according to the required proportion;
heating refined lead to 400-550 ℃ to prepare lead liquid;
taking a part of the lead liquid, adding a Pb-Ca master alloy into the lead liquid, and melting and uniformly mixing to form a Pb-Ca alloy molten liquid;
taking the rest lead liquid, adding RE into the lead liquid, and melting and uniformly mixing to form a Pb-RE alloy molten liquid;
mixing the Pb-Ca alloy melt and the Pb-RE alloy melt, adding Sn, Al and Bi, mixing and melting until the mixture is uniformly mixed, pouring, cooling and forming to obtain the grid alloy.
According to the preparation method of the rare earth grid alloy, the temperature of Ca and lead liquid during mixing and melting is 500-600 ℃, and the mixture is mixed for 15-30 min at the temperature.
According to the preparation method of the rare earth grid alloy, the temperature of RE and lead liquid during mixing and melting is 600-720 ℃, and the mixing and melting are carried out for 15-30 min at the temperature.
According to the preparation method of the rare earth grid alloy, Sn, Al and Bi elements are added, and then the mixture is melted and mixed for 15-40 min at the temperature of 500-550 ℃.
Wherein the rare earth element can inhibit the growth of the divalent lead compound, and promote the divalent lead compound to lead the non-stoichiometric PbO with good conductivity2Transformation, thereby improving the conductivity of the film; the addition of the rare earth can increase the porosity of the film, increase ion channels and further improve the conductivity of the film; for high-calcium low-tin base alloy, the tin in the anode film can increase PbO crystal lattice defects, so that crystal lattices are distorted, thereby increasing hole conduction and improving the conduction performance of the film. When the rare earth element is added into the lead-based grid alloy, alloy crystal grains can be refined, the alloy structure can be purified and homogenized, the comprehensive mechanical property of the alloy can be improved, the compactness of an alloy film can be improved, the corrosion resistance of the alloy can be improved, the growth of divalent lead with poor conductivity in the film can be inhibited, and the growth of tetravalent lead with good conductivity can be promoted, so that the conductivity of the film can be improved, the charging and discharging of the battery can be carried out more easily, and the deep cycle performance of the battery can be improved fundamentally.
Drawings
FIG. 1 is a graph showing the results of a conventional alloy grid corrosion resistance test; the results show that the conventional alloy grid loses 20% weight (corrosion is severe).
FIG. 2 is a graph showing the results of the corrosion resistance test of the rare earth grid prepared by the present invention; the result shows that the rare earth alloy grid of the invention has 12 percent of weight loss (good corrosion resistance).
FIG. 3 is a graph showing the results of a conventional alloy grid tensile test; the maximum tensile force is 229.6N, and the tensile strength is 20.4 MPa.
FIG. 4 is a graph showing the tensile test results of the rare earth alloy grid prepared according to the present invention; the maximum tensile force is 271.7N, and the tensile strength is 24.2 MPa. Compared with the prior art, the invention has the following positive beneficial effects
The rare earth raw materials used by the lead-based rare earth alloy are rich, the price is only 1/4-1/5 of Pb-Sb series and 1/8-1/9 of Pb-Ca series, and the lead-based rare earth alloy is non-toxic and non-radioactive, has no pollution to the environment and is harmless to human bodies. When the rare earth element is added into the lead-based alloy for the lead-acid storage battery, the rare earth alloy has the advantages of a Pb-Sb system and a Pb-Ca system, effectively solves the problems of preparing a grid in the prior art, obviously improves the performance of the grid, improves the performance of the battery and prolongs the service life of the battery.
The rare earth grid alloy is used as the anode of the lead-acid storage battery, the conventional lead-calcium alloy is used as the cathode, the manufactured 6-DZM-20 battery for the electric vehicle is subjected to cycle life test, and compared with the conventional battery, the cycle life is about 50 times longer than that of the conventional battery, and the cycle service life of the storage battery is prolonged; the service lives of the low temperature of-15 ℃ and the low temperature of-10 ℃ are respectively prolonged by 10 minutes and 5 minutes; and the problem of poor charging acceptance in winter is also solved. Has good application prospect in the field of lead-acid storage batteries.
Detailed Description
The present invention will be described in more detail with reference to the following embodiments in order to further understand the technical scheme of the present invention, but the present invention is not limited to the scope of the present invention.
Example 1
A rare earth grid alloy for a lead-acid storage battery comprises the following elements in percentage by weight: 0.125% of Ca, 0.022% of Al, 1.16% of Sn, 0.21% of Bi and 0.059% of RE, wherein RE is La, and the balance is Pb (refined lead with the purity of more than 99.95%).
The preparation method of the grid alloy comprises the following steps:
(1) preparing Pb-Ca mother alloy, tin, aluminum, bismuth, RE and refined lead Pb according to the required proportion;
(2) heating the prepared refined lead to 400-550 ℃ to prepare lead liquid;
(3) taking a half of the lead liquid obtained in the step (2), adding a Pb-Ca master alloy into the lead liquid, melting and mixing the lead liquid and the Pb-Ca master alloy for 15-30 min at 500-600 ℃, and uniformly mixing to form a Pb-Ca alloy molten liquid;
(4) adding La into the lead liquid left in the step (2), melting and mixing for 15-30 min at 600-720 ℃, and melting and mixing uniformly to form a Pb-La alloy molten liquid;
(5) and (3) mixing the Pb-Ca alloy melt in the step (3) and the Pb-La alloy melt in the step (4), adding Sn, Al and Bi, melting and mixing at 500-550 ℃ for 15-30 min, mixing and melting to be uniform, and pouring, cooling and forming to obtain the grid alloy.
Example 2
A rare earth grid alloy for a lead-acid storage battery comprises the following elements in percentage by weight: 0.119% of Ca, 0.029% of Al, 1.21% of Sn, 0.23% of Bi and 0.121% of RE, wherein the RE is Nd, and the balance is Pb (refined lead with the purity of more than 99.95%).
The preparation method of the grid alloy comprises the following steps:
(1) preparing Pb-Ca mother alloy, tin, aluminum, bismuth, RE and refined lead Pb according to the required proportion;
(2) heating the prepared refined lead to 400-550 ℃ to prepare lead liquid;
(3) taking a half of the lead liquid obtained in the step (2), adding a Pb-Ca mother alloy into the lead liquid, melting and mixing the lead liquid and the Pb-Ca mother alloy for 15-30 min at 500-600 ℃, and uniformly mixing to form a Pb-Ca alloy;
(4) adding Nd into the residual lead liquid in the step (2), melting and mixing for 15-30 min at 600-720 ℃, and melting and mixing uniformly to form a Pb-Nd alloy;
(5) and (3) mixing the Pb-Ca alloy melt in the step (3) and the Pb-Nd alloy melt in the step (4), adding Sn, Al and Bi, melting and mixing at 500-550 ℃ for 15-30 min, mixing and melting to be uniform, and pouring, cooling and forming to obtain the grid alloy.
Example 3
A rare earth grid alloy for a lead-acid storage battery comprises the following elements in percentage by weight: 0.121 percent of Ca, 0.026 percent of Al, 1.35 percent of Sn, 0.32 percent of Bi, 0.089 percent of RE, wherein the RE is Sm, and the balance of Pb (refined lead with the purity of more than 99.95 percent).
The preparation method of the grid alloy comprises the following steps:
(1) preparing Pb-Ca mother alloy, tin, aluminum, bismuth, RE and refined lead Pb according to the required proportion;
(2) heating the prepared refined lead to 400-550 ℃ to prepare lead liquid;
(3) taking a half of the lead liquid obtained in the step (2), adding a Pb-Ca mother alloy into the lead liquid, melting and mixing the lead liquid and the Pb-Ca mother alloy for 15-30 min at 500-600 ℃, and uniformly mixing to form a Pb-Ca alloy;
(4) taking the residual lead liquid in the step (2), adding Sm into the lead liquid, melting and mixing the Sm for 15-30 min at the temperature of 600-720 ℃, and melting and mixing the Sm and the lead liquid uniformly to form a Pb-Sm alloy;
(5) and (3) mixing the Pb-Ca alloy molten liquid in the step (3) and the Pb-Sm alloy molten liquid in the step (4), adding Sn, Al and Bi, melting and mixing at 500-550 ℃ for 15-30 min, mixing and melting to be uniform, and pouring, cooling and forming to obtain the grid alloy.
Example 4
A rare earth grid alloy for a lead-acid storage battery comprises the following elements in percentage by weight: 0.117% of Ca, 0.043% of Al, 1.22% of Sn, 0.26% of Bi and 0.074% of RE, wherein the RE is La and Nd, and the balance is Pb (refined lead with the purity of more than 99.95%).
The preparation method of the grid alloy comprises the following steps:
(1) preparing Pb-Ca mother alloy, tin, aluminum, bismuth, RE and refined lead Pb according to the required proportion;
(2) heating the prepared refined lead to 400-550 ℃ to prepare lead liquid;
(3) taking a half of the lead liquid obtained in the step (2), adding a Pb-Ca mother alloy into the lead liquid, melting and mixing the lead liquid and the Pb-Ca mother alloy for 15-30 min at 500-600 ℃, and uniformly mixing to form a Pb-Ca alloy;
(4) taking the residual lead liquid in the step (2), adding La and Nd (the mass ratio of La to Nd is 1: 1-2), melting and mixing for 15-30 min at the temperature of 600-720 ℃, and melting and mixing uniformly to form a Pb-RE alloy;
(5) and (3) mixing the Pb-Ca alloy molten liquid in the step (3) and the Pb-RE alloy molten liquid in the step (4), adding Sn, Al and Bi, melting and mixing at 500-550 ℃ for 15-30 min, mixing and melting to be uniform, and pouring, cooling and forming to obtain the grid alloy.
Example 5
A rare earth grid alloy for a lead-acid storage battery comprises the following elements in percentage by weight: 0.118% of Ca, 0.044% of Al, 1.11% of Sn, 0.38% of Bi and 0.076% of RE, wherein the RE is Nd and Sm, and the balance is Pb (refined lead with the purity of more than 99.95%).
The preparation method of the grid alloy comprises the following steps:
(1) preparing Pb-Ca mother alloy, tin, aluminum, bismuth, RE and refined lead Pb according to the required proportion;
(2) heating the prepared refined lead to 400-550 ℃ to prepare lead liquid;
(3) taking a half of the lead liquid obtained in the step (2), adding a Pb-Ca mother alloy into the lead liquid, melting and mixing the lead liquid and the Pb-Ca mother alloy for 15-30 min at 500-600 ℃, and uniformly mixing to form a Pb-Ca alloy;
(4) taking the lead liquid in the step (1), adding RE (Nd) and Sm (the mass ratio of Nd to Sm is 1:1) into the lead liquid, melting and mixing for 15-30 min at the temperature of 600-720 ℃, and melting and mixing uniformly to form a Pb-RE alloy;
(5) and (3) mixing the Pb-Ca alloy molten liquid in the step (3) and the Pb-RE alloy molten liquid in the step (4), adding Sn, Al and Bi, melting and mixing at 500-550 ℃ for 15-30 min, mixing and melting to be uniform, and pouring, cooling and forming to obtain the grid alloy.
Example 6
A rare earth grid alloy for a lead-acid storage battery comprises the following elements in percentage by weight: 0.116% of Ca, 0.035% of Al, 0.98% of Sn, 0.27% of Bi and 0.132% of RE, wherein RE is La and Sm, and the balance is Pb (refined lead with the purity of more than 99.95%).
The preparation method of the grid alloy comprises the following steps:
(1) preparing Pb-Ca mother alloy, tin, aluminum, bismuth, RE and refined lead Pb according to the required proportion;
(2) heating the prepared refined lead to 400-550 ℃ to prepare lead liquid;
(3) taking a half of the lead liquid obtained in the step (2), adding a Pb-Ca mother alloy into the lead liquid, melting and mixing the lead liquid and the Pb-Ca mother alloy for 15-30 min at 500-600 ℃, and uniformly mixing to form a Pb-Ca alloy;
(4) taking the residual lead liquid in the step (2), adding RE (La) and Sm (the mass ratio of La to Sm is 1:1) into the lead liquid, melting and mixing the lead liquid and the La to Sm for 15-30 min at the temperature of 600-720 ℃, and melting and mixing the lead liquid and the Sm uniformly to form a Pb-RE alloy;
(4) and (3) mixing the Pb-Ca alloy melt in the step (2) and the Pb-RE alloy melt in the step (3), adding Sn, Al and Bi, melting and mixing at 500-550 ℃ for 15-30 min, mixing and melting to be uniform, and pouring, cooling and forming to obtain the grid alloy.
Example 7
A rare earth grid alloy for a lead-acid storage battery comprises the following elements in percentage by weight: 0.123% of Ca, 0.027% of Al, 1.25% of Sn, 0.31% of Bi and 0.087% of RE, wherein the RE is La, Nd and Sm, and the balance is Pb (refined lead with the purity of more than 99.95%).
The preparation method of the grid alloy comprises the following steps:
(1) preparing Pb-Ca mother alloy, tin, aluminum, bismuth, RE and refined lead Pb according to the required proportion;
(2) heating the prepared refined lead to 400-550 ℃ to prepare lead liquid;
(3) taking a half of the lead liquid obtained in the step (2), adding a Pb-Ca mother alloy into the lead liquid, melting and mixing the lead liquid and the Pb-Ca mother alloy for 15-30 min at 500-600 ℃, and uniformly mixing to form a Pb-Ca alloy;
(4) taking the residual lead liquid in the step (2), adding RE (La), Nd and Sm into the lead liquid, melting and mixing for 15-30 min at the temperature of 600-720 ℃, and melting and mixing uniformly to form a Pb-RE alloy;
(5) and (3) mixing the Pb-Ca alloy molten liquid in the step (3) and the Pb-RE alloy molten liquid in the step (4), adding Sn, Al and Bi, melting and mixing at 500-550 ℃ for 15-30 min, mixing and melting to be uniform, and pouring, cooling and forming to obtain the grid alloy.
The rare earth grid alloy prepared by the invention is detected as follows:
1. the performance detection results of the lead-acid storage battery prepared from the rare earth grid alloy prepared by the invention are shown in table 1.
Table 2 lead-acid battery performance test results prepared by using the rare earth grid alloy of the present invention
2. And (3) performing corrosion resistance test on the prepared grid, which specifically comprises the following steps: the prepared rare earth grid and the conventional grid are directly charged in acid for 7 days respectively, and the results of weight loss comparison are shown in fig. 1 and fig. 2.
3. The rare earth grid prepared by the invention is compared with the conventional grid in a tensile test, and the results are shown in fig. 3 and fig. 4. The detection result also shows that the maximum tensile force of the conventional grid is 229.6N, and the tensile strength is 20.4 MPa; the maximum tensile force of the prepared grid is 271.7N, and the tensile strength is 24.2 MPa.
Namely, the corrosion resistance and the tensile property of the rare earth grid alloy prepared by the invention are both obviously improved.
Claims (7)
1. The rare earth grid alloy for the lead-acid storage battery is characterized by comprising the following elements in percentage by weight: calcium: 0.10 to 0.14%, tin: 0.8-1.5%, aluminum: 0.02-0.05%, bismuth: 0.2-0.4%, RE: 0.05 to 0.15 percent, and the balance being Pb.
2. The rare earth grid alloy for lead-acid batteries according to claim 1, wherein the Pb is refined lead having a purity of 99.95% or more.
3. The rare earth grid alloy for lead-acid storage batteries according to claim 1, wherein RE is selected from one or a mixture of La, Nd and Sm.
4. A preparation method of the rare earth grid alloy for the lead-acid storage battery according to any one of claims 1 to 3, characterized by comprising the following steps:
preparing Pb-Ca mother alloy, tin, aluminum, bismuth, RE and refined lead Pb according to the required proportion;
heating refined lead to 400-550 ℃ to prepare lead liquid;
taking lead liquid, adding Pb-Ca master alloy into the lead liquid, and melting and uniformly mixing the lead liquid and the Pb-Ca master alloy to form Pb-Ca alloy molten liquid;
taking lead liquid, adding RE into the lead liquid, and melting and uniformly mixing to form a Pb-RE alloy molten liquid;
mixing the Pb-Ca alloy melt and the Pb-RE alloy melt, adding Sn, Al and Bi, mixing and melting until the mixture is uniformly mixed, pouring, cooling and forming to obtain the grid alloy.
5. The method for preparing a rare earth grid alloy according to claim 4, wherein the temperature for mixing and melting Ca and the lead liquid is 500-600 ℃, and the mixing is carried out at the temperature for 15-30 min.
6. The preparation method of the rare earth grid alloy according to claim 4, wherein the temperature for mixing and melting RE and lead liquid is 600-720 ℃, and the mixing and melting are carried out for 15-30 min at the temperature.
7. The method for preparing a rare earth grid alloy according to any one of claims 4 to 6, wherein the Sn, Al and Bi elements are added and then melted and mixed at 500 to 550 ℃ for 15 to 40 min.
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| CN111682166A (en) * | 2020-05-14 | 2020-09-18 | 天能电池集团股份有限公司 | Positive plate for high-capacity battery, preparation method and high-capacity battery |
| CN113097573A (en) * | 2021-03-25 | 2021-07-09 | 北京阳光鸿志电气工程技术有限公司 | Quick-charging full-sealed maintenance-free lead-acid storage battery |
| CN115198124A (en) * | 2022-06-13 | 2022-10-18 | 风帆有限责任公司 | Process for preparing lead-base rare-earth alloy |
| CN115418527A (en) * | 2022-08-22 | 2022-12-02 | 铅锂智行(北京)科技有限公司 | Grid alloy of lead-acid storage battery |
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Application publication date: 20200424 |