CN115233033A - Lead-based alloy and product thereof - Google Patents
Lead-based alloy and product thereof Download PDFInfo
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- CN115233033A CN115233033A CN202210827605.2A CN202210827605A CN115233033A CN 115233033 A CN115233033 A CN 115233033A CN 202210827605 A CN202210827605 A CN 202210827605A CN 115233033 A CN115233033 A CN 115233033A
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- lead
- based alloy
- antimony
- alloy
- oxide powder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C11/00—Alloys based on lead
- C22C11/08—Alloys based on lead with antimony or bismuth as the next major constituent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G21/00—Compounds of lead
- C01G21/02—Oxides
-
- 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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/06—Lead-acid accumulators
- H01M10/12—Construction or manufacture
-
- 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
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
-
- 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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention relates to a lead-based alloy, which consists of 4-12% of antimony by total weight percentage of the alloy, and the balance of lead and incidental impurities, wherein the lead-based alloy is used for preparing lead-containing oxide powder, and the lead-containing oxide powder is used for preparing active substances for lead-acid storage batteries. The invention also discloses a lead-acid storage battery and a preparation method thereof. The lead-acid storage battery prepared from the lead-based alloy has long cycle life.
Description
Technical Field
The invention relates to the field of storage battery manufacturing.
Background
At present, in order to improve the performance of a lead-acid storage battery, many attempts are made in the industry, particularly in the preparation of an active substance, an additive such as metallic antimony, bismuth and the like is added in the paste mixing process, however, the additive cannot be uniformly mixed in the paste during the paste mixing process, a certain influence is generated on the performance of the finally prepared lead-acid storage battery, in order to improve the uniform distribution of the additive in the paste, the lead alloy is ground into powder at present, and in the paste mixing process, the uniformity of the additive in the paste is improved to a certain extent.
Disclosure of Invention
In order to solve the technical problems, the invention provides a lead-based alloy, which is characterized by comprising 4-12% of antimony by total weight percentage of the alloy, and the balance of lead and incidental impurities, wherein the lead-based alloy is used for preparing lead-containing oxide powder, and the lead-containing oxide powder is used for preparing an active substance for a lead-acid storage battery.
Further, the antimony is contained in 4% -9% of the total weight percentage of the alloy.
Further, the lead-based alloy also comprises 0.03-0.08% of bismuth.
The invention also provides lead-containing oxide powder prepared from the lead-based alloy by a ball milling or melt atomization method.
The invention also provides an active material of the lead-acid storage battery electrode, which is prepared by mixing the lead-containing oxide powder, water and aqueous sulfuric acid.
Further, the active material is a positive electrode active material.
The invention also protects an electrode of the lead-acid storage battery, which comprises a grid coated with the positive active material.
The invention also protects a lead-acid battery comprising electrodes.
The invention also provides a preparation method of the lead-based alloy, the lead-based alloy consists of 4-12% of antimony by total weight percentage of the alloy, and the balance is lead and incidental impurities, and the preparation method comprises the following steps: antimony in an amount of 4-12% by weight as an alloy is added to molten lead at a temperature in the range of 438-454 c and cooled to a temperature in the range of 399-454 c to cast ingots.
The invention also provides a manufacturing method of the lead-acid storage battery, which comprises the following steps: mixing a lead-based alloy consisting of 4-12% of antimony and the balance of lead and incidental impurities with a lead ingot according to a certain proportion, preparing lead-containing oxide powder by a Buton's or ball milling process, selecting the lead-containing oxide powder, adding fiber, water and sulfuric acid, stirring to prepare lead plaster, and coating the lead plaster on a grid to prepare the positive plate.
The lead-acid storage battery prepared from the lead-based alloy has long cycle life.
Detailed Description
The invention is further described with reference to specific examples.
The lead-based alloy consists of 4-12 percent of antimony by total weight percent of the alloy, and the balance of lead and incidental impurities. Antimony can improve the hydration degree of lead dioxide particles and aggregates in the active substance, is beneficial to enhancing the connection between macromolecules, and further improves the utilization rate of the active substance.
The above lead-based alloys may be formulated with antimony added as an alloy to purified virgin and/or recycled molten lead in an amount of 4-12% by total weight percent. Such as: lead-based alloys having a substantial amount of eutectic formed therein are produced by melting a lead-based alloy by adding antimony alloying elements to molten secondary lead at a temperature in the range of 820 ° F to 850 ° F (438-454 ℃) and cooling the ingot cast at a casting temperature in the range of 750 ° F to 850 ° F (399-454 ℃), preferably by rapid cooling which is non-natural cooling in the sense of the present invention. The formation of a large amount of eutectic is greatly beneficial to the wide and uniform distribution of antimony in the alloy.
The lead-based alloy may be used to prepare doped lead-containing oxide powders in a barton process, a ball milling process, or other lead oxide preparation process. The lead-based alloy can be used to prepare doped lead oxide-containing powders in a barton reactor operating at a temperature in the range of 675 deg.f to 700 deg.f (357-371 deg.c), with an agitator speed in the range of 150-500RPM and an air blower operating in the range of 44-49 hertz. The ball milling process is a batch or semi-batch process, wherein a lead-based alloy ingot is put into a ball mill or a pure lead ingot and a lead-based alloy ingot in a certain proportion are put into the ball mill. The oxidation reaction is initiated by the friction heat generated by rolling the pure lead ingot and the lead-based alloy ingot, and the oxygen in the air reacts with the lead to generate lead oxide in the oxidation reaction. During the milling process, the lead oxide particles formed on the ingot surface and particles of unoxidized lead fall off the ingot, producing a powder that can be removed from the ball mill by a circulating air stream. 4% -12% of antimony in the lead-based alloy can be uniformly distributed in the lead-based alloy, so that antimony oxide in the lead-containing oxide powder can be better and uniformly mixed in the powder.
Doped lead-containing oxide powders prepared from lead-based alloys can be used as the preparation active, the lead-containing oxide powder and water are mixed to form a slurry or paste, and then aqueous and sulfuric acid can be added with continued mixing and optional cooling until the desired paste consistency and density is obtained.
Lead-acid battery electrodes are made by applying a paste of doped lead-containing oxide powder prepared from a lead-based alloy to a grid comprising metallic lead or any suitable lead-based alloy (e.g., lead-antimony alloy, lead-calcium-tin-silver alloy, lead-calcium-aluminum alloy, or lead-tin-calcium-aluminum alloy). And the lead-acid storage battery is prepared by the lead-acid storage battery electrode.
The antimony with the content of 4% -12% in the lead-based alloy, preferably 4% -9% can form a large amount of eutectic in the lead-based alloy, so that the antimony can be distributed in the alloy relatively uniformly, uniform mixing in a lead oxide can be better realized, the structure of an active substance is further changed, the overall utilization rate of the active substance in the charging process is improved, and the service life and the capacity of a battery are prolonged.
The method for preparing the lead-acid storage battery comprises the following steps: 4 to 12 percent of lead-based alloy, 88 to 96 percent of lead and incidental impurities by total weight percent of the alloy; cutting the alloy into small alloy lead blocks, feeding the small alloy lead blocks into a ball mill to be ball-milled with a lead ingot in a certain proportion, wherein the proportion range of the alloy lead blocks to the lead ingot is 1-4-1; the mass percentages of the lead powder, the fiber, the water and the sulfuric acid are as follows: 0.0008-0.0012:0.08-0.12:0.08-0.12, selecting 1000kg of ball milling lead powder, adding 0.8-1.2 kg of fiber and 80-120 kg of water; 80kg-120kg of sulfuric acid with the density of 1.40g/ml, and stirring for 30 minutes-60 minutes to prepare lead plaster; and coating the prepared lead plaster on a lead-tin-calcium-aluminum alloy grid to prepare the positive plate. Then curing and drying for 48-72 hours at 30-70 ℃; finally, assembling the lead-acid storage battery, electrifying for 48-72 hours, and preparing the lead-acid storage battery.
Example 1
1000kg of lead-based alloy: 4% of antimony, lead and incidental impurities 96%; cutting the alloy into small lead blocks, feeding the lead blocks into a ball mill, and carrying out ball milling on 3000kg of lead ingots according to a certain proportion at the ball milling temperature of 200 ℃ to obtain ball-milled lead powder with the oxidation degree of 76%; selecting 1000kg of ball milling lead powder, adding 1kg of fiber and 85kg of water; 85kg of sulfuric acid with the density of 1.40g/ml, and stirring for 45 minutes to prepare lead plaster; and coating the prepared lead plaster on a lead-tin-calcium-aluminum alloy grid to prepare the positive plate. Then curing and drying for 60 hours at 55 ℃; finally, the lead-acid storage battery is assembled and electrified for 65 hours.
10 of the 20AH cells prepared in example 1 were selected and tested to obtain discharge capacity and cycle life data.
Example 2
The same procedure as in example 1 was repeated, except that the ratio of the components of the lead-based alloy was changed, and 4000kg of a lead ingot was ball-milled. The lead-based alloy comprises 5% of antimony, 95% of lead and incidental impurities.
10 of the 20AH cells prepared in example 2 were selected and tested to obtain discharge capacity and cycle life data.
Example 3
The same procedure as in example 1 was repeated, except that the lead-based alloy was used in a different composition ratio, and 8000kg of lead ingots were ball-milled. The lead-based alloy comprises 9% of antimony, 91% of lead and accidental impurities.
10 of the 20AH cells prepared in example 3 were selected and tested to obtain discharge capacity and cycle life data.
Example 4
The same procedure as in example 1 was repeated, except that the ratio of the components of the lead-based alloy was changed, and 11000kg of a lead ingot was ball-milled in a predetermined ratio. The composition of the lead-based alloy is 12% antimony, lead and incidental impurities 88%.
10 of the 20AH cells prepared in example 4 were selected and tested to obtain discharge capacity and cycle life data.
Comparative example 1
The same as in example 1 was repeated except that the ratio of the lead-based alloy was changed. 1% of antimony, lead and incidental impurities 99%.
10 of the 20AH cells prepared in example 4 were selected and tested to obtain discharge capacity and cycle life data.
Comparative example 2
The same procedure as in example 1 was repeated, except that the ratio of the components of the lead-based alloy was changed, and 2000kg of lead ingot was ball-milled. The lead-based alloy comprises 3% of antimony, lead and incidental impurities of 97%.
10 of the 20AH cells prepared in example 4 were selected and tested to obtain discharge capacity and cycle life data.
Comparative example 3
The same procedure as in example 1 was repeated, except that the ratio of the components of the lead-based alloy was changed, and the alloy was ball-milled with 12000kg of lead ingot in a predetermined ratio. The lead-based alloy comprises 13% of antimony, lead and 87% of incidental impurities.
10 of the 20AH cells prepared in example 4 were selected and tested to obtain discharge capacity and cycle life data.
Comparative example 4
The same procedure as in example 1 was repeated, except that the ratio of the components of the lead-based alloy was changed, and 14000kg of lead ingot was ball-milled in a predetermined ratio. The lead-based alloy comprises 15% of antimony, 85% of lead and incidental impurities.
10 of the 20AH cells prepared in example 4 were selected and tested to obtain discharge capacity and cycle life data.
Cell discharge capacity and cycle life data were obtained from the 4 examples and 4 comparative examples above, as shown in the following table:
it can be seen from the above table that when the antimony content in the alloy is less than 4%, because there is not a large amount of eutectic formation, it is inhomogeneous to lead to the distribution of antimony in the ball crocus, and the final test cycle life of battery is showing lowly, and when the antimony content was higher than 12%, the hardness of alloy was too high, when the ball crocus, leads to alloy crocus efficiency to descend, finally influences the evenly distributed of antimony in the crocus, and the final test cycle life of battery descends.
The lead-based alloy can also comprise 0.03 to 0.08 percent of bismuth according to the requirement, and the realization of the aim of the invention is not influenced.
The above-described embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way, and other variations and modifications may be made without departing from the spirit of the invention as set forth in the claims.
Claims (10)
1. The lead-based alloy is characterized by consisting of 4-12% of antimony by total weight percentage of the alloy, and the balance of lead and incidental impurities, wherein the lead-based alloy is used for preparing lead-containing oxide powder, and the lead-containing oxide powder is used for preparing active substances for lead-acid storage batteries.
2. The lead-based alloy of claim 1, comprising 4% to 9% antimony, by weight of the total alloy.
3. The lead-based alloy according to claim 1 or 2, wherein the lead-based alloy further comprises 0.03% to 0.08% bismuth.
4. A lead-containing oxide powder produced by using the lead-based alloy according to claim 1 or 2 for ball milling or melt atomization.
5. An active material for an electrode of a lead-acid storage battery, characterized in that the active material is obtained by mixing the lead-containing oxide powder according to claim 4 with water and aqueous sulfuric acid.
6. The active material for an electrode of a lead-acid battery according to claim 5, wherein the active material is a positive electrode active material.
7. An electrode for a lead-acid storage battery comprising a grid, wherein the positive electrode active material according to claim 6 is coated on the grid.
8. A lead-acid battery comprising an electrode, wherein the electrode is the electrode of claim 7.
9. The preparation method of the lead-based alloy comprises the following steps of, by total weight percent, 4% -12% of antimony, and the balance of lead and incidental impurities, and is characterized by comprising the following steps: antimony as an alloy in an amount of 4-12% by weight is added to molten lead at a temperature in the range of 438-454 c and cooled to a temperature in the range of 399-454 c and cast into ingots.
10. A method for manufacturing a lead-acid storage battery is characterized by comprising the following steps: mixing a lead-based alloy consisting of 4-12% of antimony and the balance of lead and incidental impurities with a lead ingot according to a certain proportion, preparing lead-containing oxide powder by a Buton's or ball milling process, selecting the lead-containing oxide powder, adding fiber, water and sulfuric acid, stirring to prepare lead plaster, and coating the lead plaster on a grid to prepare the positive plate.
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| CN202210827605.2A CN115233033A (en) | 2022-07-14 | 2022-07-14 | Lead-based alloy and product thereof |
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