CN107287470B - A kind of lead storage battery grid alloy and preparation method comprising nanometer tungsten carbide material - Google Patents
A kind of lead storage battery grid alloy and preparation method comprising nanometer tungsten carbide material Download PDFInfo
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- CN107287470B CN107287470B CN201710380920.4A CN201710380920A CN107287470B CN 107287470 B CN107287470 B CN 107287470B CN 201710380920 A CN201710380920 A CN 201710380920A CN 107287470 B CN107287470 B CN 107287470B
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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
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
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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
- C22C11/06—Alloys based on lead with tin as the next major constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0052—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
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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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- 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
- H01M4/70—Carriers or collectors characterised by shape or form
- H01M4/72—Grids
- H01M4/73—Grids for lead-acid accumulators, e.g. frame plates
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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
- 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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- Cell Electrode Carriers And Collectors (AREA)
Abstract
The invention discloses a kind of lead storage battery grid alloys and preparation method comprising nanometer tungsten carbide material, belong to lead storage battery preparation technical field.The grid alloy, by weight percentage, consisting of: tin 0.1~0.8%, nanometer tungsten carbide 0.05~0.5%, lead are surplus.The present invention substitutes used calcium metal, substantially reduces the grid alloy intercrystalline corrosion as caused by calcification lead by addition nanometer tungsten carbide material；The combination and institutional framework for improving metal crystal grain boundary, significantly improve hardness, creep-resistant property, corrosion resistance of metal etc..The present invention prepares the master alloy containing tungsten carbide composite by cold melt process, recycles master alloy to prepare tungsten carbide composite alloy, it is ensured that nanometer tungsten carbide material is evenly dispersed in metal, to improve metal performance.In addition the control of whole preparation process temperature is at 500 DEG C hereinafter, significant energy saving, and the lead skim generated in fusion process is less.
Description
Technical field
The present invention relates to lead storage battery preparation technical fields, and in particular to a kind of lead electric power storage comprising nanometer tungsten carbide material
Pond grid alloy and preparation method.
Background technique
Metal is battery plate grid material, and corrosion resistance directly affects the cycle life of battery.Currently, main
Using Pb-Ca-Sn-Al alloy as grid material, the hardness of the material is higher, it is ensured that industrialized production.Due to element calcium master
Between being present in crystal boundary in the form of calcification lead, therefore its corrosion resistance is poor.Pb-Ca-Sn-Al alloy be easy to cause battery early
Phase capacitance loss, so, novel added material is selected, while ensureing alloy rigidity, its corrosion resistance is improved, is lead electric power storage
The emphasis of pond research.
It since the corrosion of metal is mainly since crystal boundary, deepens continuously, eventually leads to intercrystalline and combine and fall off, so,
Improving crystal boundary performance or improving the corrosion resistance of substance in crystal boundary is the key that improve metal corrosion resistance.
As 105322179 A of patent document CN discloses a kind of anticorrosive positive grid green alloy of lead-acid accumulator, including
Following components in percentage by weight: tin 0.8~1.5%, calcium 0.08~0.15%, aluminium 0.01~0.04%, cerium 0.02~
0.2%, lanthanum 0.02~0.2%, neodymium 0.02~0.2%, silver 0.001~0.05%, remaining is lead.By scientific and reasonable examination
It tests, by the way that Ce, La, Nd, Ag of formula ratio is added, retains the operability in original alloy and high hydrogen-evolution overpotential, original Pb-
Ca-Sn-Al crystalline substance has the change of essence as structure, finds its corrosion resistance than original Pb-Ca-Sn- by corrosion-resistant experiment
Al alloy promotes 3-4 times, and the anticorrosive positive grid green alloy of the invention lead-acid accumulator reaches positive grid when 800 100%DOD
Do not corrode.
As 106058267 A of patent document CN discloses a kind of preparation side of lead-acid battery graphene lead and neodymium isotopes
Method, select metal carbides or solid carbon-contg organic compound be decomposed to form under the high temperature conditions carbon source and under the high temperature conditions into
Enter in lead solution, and lead forms the combination of atomic level, the graphene formed after being cooled down can be uniformly dispersed in metal
In；The reaction carried out in atmospheric conditions also largely saves cost；The graphene grid alloy prepared using the method
The mechanical performance for improving grid alloy enhances its creep resisting ability.
Wherein metal carbides are tungsten carbide, and tungsten carbide is a kind of compound being made of tungsten and carbon, are that production hard closes
The primary raw material of gold is black hexagonal, there is metallic luster, and hardness is close with diamond, for electricity, the good conductor of heat.Carbon
The chemical property for changing tungsten is stablized, and starts active oxidation for 500 DEG C or more in air, oxidation resistance is weak.
In addition, traditional Pb-Ca-Sn-Al alloy needs to carry out melting at 650 DEG C or more, in melting due to adding calcium metal
It is easy to produce lead skim in the process, is unfavorable for energy conservation.
Summary of the invention
The purpose of the present invention is to provide a kind of lead storage battery grid alloy comprising nanometer tungsten carbide material, using nanometer
Tungsten carbide replaces the calcium metal in traditional metal to significantly improve lead storage battery grid creep resistant to reduce alloy grain size
The performance of property, corrosion resistance etc..
To achieve the above object, the present invention adopts the following technical scheme:
A kind of lead storage battery grid alloy comprising nanometer tungsten carbide material, by weight percentage, consisting of: tin
0.1~0.8%, nanometer tungsten carbide 0.05~0.5%, lead are surplus.
In the present invention, the addition of nanometer tungsten carbide can not only significantly improve the hardness of metal, can also significantly improve
Crystal grain, the grain boundary features of alloy, crystallite dimension are substantially reduced, and grain boundary area increases, and under same current density, can substantially reduce corruption
Erosion amount, to extend the cycle life of battery.
The effect that the present invention adds tin in lead storage battery grid formula is to improve the mobility and ductility of alloy.
Preferably, by weight percentage, the composition of alloy are as follows: tin 0.2~0.5%, nanometer tungsten carbide 0.2~
0.5%, lead is surplus.
When preparing grid alloy, it is desirable that the nano powder of tungsten carbide of addition, partial size be 10~100nm, purity >=
99.9%, carbon content >=5.0%, single metals content impurity≤0.01%.
Since the partial size of nano powder of tungsten carbide is nanoscale, keep its evenly dispersed by stirring in lead liquid.
The present invention also provides a kind of sides for preparing the lead storage battery grid alloy comprising nanometer tungsten carbide material
Method, comprising:
(1) master alloy is prepared
A) metallic tin is added in the lead liquid of fusing, heating is melted and stirred evenly, and aluminium alloy is obtained；
B) temperature control will be enclosed in the sheet lead packet indentation aluminium alloy of nano powder of tungsten carbide, stirring makes to 350~400 DEG C
Nano powder of tungsten carbide is dispersed in aluminium alloy, is cast into master alloy ingot；
(2) grid alloy is prepared
I) lead pig for accounting for lead gross mass 70~80% is added in intermediate frequency furnace, heating fusing；
II) for control temperature in 380~450 DEG C of master alloy ingots that into melt prepared by addition step (1), stirring makes master alloy
It is completely melt and is uniformly mixed；
III) remaining lead pig, fusing, stirring, cast alloys ingot after scarfing cinder is added.
The present invention prepares the master alloy containing tungsten carbide composite by cold melt process, and master alloy is recycled to prepare carbon
Change tungsten composite alloy, it is ensured that nanometer tungsten carbide material is evenly dispersed in metal, to improve metal performance.In addition entire
The control of preparation process temperature is at 500 DEG C hereinafter, significant energy saving, and the lead skim generated in fusion process is less.
Preferably, in step a) lead pig being added in intermediate frequency furnace be heated to 480~520 DEG C first, keep it sufficiently molten
Change, metallic tin is then added, stirs 5~60min, be completely melt metallic tin.
Preferably, stirring 1~3h after being pressed into sheet lead packet in step b).
Preferably, step I) in, being heated to 320~350 DEG C melts lead pig.
Preferably, step II) in, 5~60min is stirred after master alloy ingot is added.
In above-mentioned whipping process, the rate of stirring can have an impact for the slag yield of alloy, and stirring rate is unsuitable too fast.If
Metal Theil indices are insufficient in master alloy, can be in step II) when the desired amount of metallic tin is added.
It is that the present invention has the utility model has the advantages that
(1) by addition nanometer tungsten carbide material, used calcium metal is substituted, the grid as caused by calcification lead is substantially reduced
Alloy intercrystalline corrosion；Crystal grain, the grain boundary features of alloy can be significantly improved, crystallite dimension is substantially reduced, and grain boundary area increases；Change
The combination and institutional framework of kind metal crystal grain boundary, mention hardness, creep-resistant property, corrosion resistance of metal etc. significantly
It is high.
(2) present invention uses low smelting heat technique, significant energy saving, and lead skim is less in fusion process.
Specific embodiment
Below with reference to embodiment, the invention will be further described.But following embodiments are only preferred implementation of the invention
Example, and it is not all.Based on the implementation example in the implementation mode, those skilled in the art are without making creative work
Obtained other embodiments, belong to protection scope of the present invention.
Embodiment 1
1, master alloy is prepared
Master alloy formula is as follows: tin: 5.0%, nanometer tungsten carbide 3.0%, lead are surplus, and aforementioned proportion is weight percent
Than.
(1) according to said ratio, metallic tin, nanometer tungsten carbide, lead are weighed；
(2) 2/3 amount of raw material lead is added in mid-frequency melting furnace and is heated to 500 DEG C, melt lead button sufficiently；
(3) metallic tin is added to melt, stirs at low speed (magnetic force or mechanical stirring) 30min, is completely melt metallic tin simultaneously
It is uniformly mixed；
(4) 380 DEG C are cooled to, the nano powder of tungsten carbide of quality needed for being matched with sheet lead package is pressed into lead liquid,
Moderate-speed mixer 3h is dispersed in tungsten-carbide powder in lead liquid；
(5) master alloy ingredient is measured, cast alloys ingot after setting proportion is reached.
In above-mentioned preparation method, the nano powder of tungsten carbide partial size of addition is 10~100nm, purity >=99.9%, carbon
Content >=5.0%, single metals content impurity≤0.01%.
2, the preparation of lead storage battery grid alloy
By weight percentage, it forms are as follows: tin 0.5%, nanometer tungsten carbide 0.3%, lead are surplus.
The following steps are included:
(1) according to said ratio, each raw material are weighed；
(2) lead button for accounting for leady raw materials gross mass 70~80% is added in intermediate frequency furnace and is heated to 350 DEG C, keep lead button sufficiently molten
Change；
(3) continue to be heated to 380 DEG C of master alloys that the required quality of proportion is added to melt, stir 30min, keep master alloy complete
Running down is simultaneously uniformly mixed；
(4) remaining lead button is added, melt is stirred；
(5) slag-cleaning agent is spread to bath surface, stirs 20min, then removes dross；
(6) alloying component is measured, cast alloys ingot after setting proportion is reached.
3, lead storage battery grid performance detection
A, timeliness hardness
After 5 days timeliness of alloy, using the experiment power of 0.098N (0.01kg), retention time 30s or more detects Vickers hardness
Value.
B, oxygen current density is analysed
It is anode with alloy, platinum electrode is cathode, three-electrode system lower linear electric potential scanning is carried out, when electrode potential is
1.50V(vs.Hg/Hg2SO4) when, detect the analysis oxygen current density of alloy.
C, corrosion resistance
It is anode with length and width, the alloy that thickness is 10 × 1 × 0.2cm, stereotype is cathode, constant current under the conditions of 50 DEG C
For 0.8A, weight pulling force is 550g, the time that alloy sample corrosion disconnects.
The results are shown in Table 1, and alloy made from the present embodiment obtains in terms of timeliness hardness, creep-resistant property, corrosion resistance
To significantly improving.
Table 1
The alloy formula of above-mentioned control 1 is the conventional plato grid alloy formulation that uses: calcium 0.08%, tin 1.0%, aluminium 0.05%,
Lead is surplus.
The alloy formula of control 2 are as follows: tin 0.5%, lead are surplus.
Embodiment 2
By weight percentage, it forms are as follows: tin 0.5%, nanometer tungsten carbide 0.5%, lead are surplus.
Preparation method and test method are with embodiment 1, and the results are shown in Table 2.
Table 2
The alloy formula of above-mentioned control 1 is the conventional plato grid alloy formulation that uses: calcium 0.08%, tin 1.0%, aluminium 0.05%,
Lead is surplus.
Embodiment 3
By weight percentage, it forms are as follows: tin 0.5%, nanometer tungsten carbide 0.1%, lead are surplus.
Preparation method and test method are with embodiment 1, and the results are shown in Table 3.
Table 3
The alloy formula of above-mentioned control 1 is the conventional plato grid alloy formulation that uses: calcium 0.08%, tin 1.0%, aluminium 0.05%,
Lead is surplus.
Claims (7)
1. a kind of lead storage battery grid alloy comprising nanometer tungsten carbide material, which is characterized in that by weight percentage, group
Become: tin 0.1~0.8%, nanometer tungsten carbide 0.05~0.5%, lead are surplus；
Preparation method, comprising the following steps:
(1) master alloy is prepared
A) metallic tin is added in the lead liquid of fusing, heating is melted and stirred evenly, and aluminium alloy is obtained；
B) temperature control will be enclosed in the sheet lead packet indentation aluminium alloy of nano powder of tungsten carbide, stirring makes nanometer to 350~400 DEG C
Tungsten-carbide powder is dispersed in aluminium alloy, is cast into master alloy ingot；
(2) grid alloy is prepared
I) lead pig for accounting for lead gross mass 70~80% is added in intermediate frequency furnace, heating fusing；
II) for control temperature in 380~450 DEG C of master alloy ingots that into melt prepared by addition step (1), stirring keeps master alloy complete
It melts and is uniformly mixed；
III) remaining lead pig, fusing, stirring, cast alloys ingot after scarfing cinder is added.
2. as described in claim 1 including the lead storage battery grid alloy of nanometer tungsten carbide material, which is characterized in that with weight
Percentages, composition are as follows: tin 0.2~0.5%, nanometer tungsten carbide 0.2~0.5%, lead are surplus.
3. as claimed in claim 1 or 2 including the lead storage battery grid alloy of nanometer tungsten carbide material, which is characterized in that institute
The partial size for stating nanometer tungsten carbide is 10~100nm, wherein mass percentage content >=5.0% of carbon.
4. as described in claim 1 including the lead storage battery grid alloy of nanometer tungsten carbide material, which is characterized in that step a)
In, lead pig is added in intermediate frequency furnace be heated to 480~520 DEG C first, melted it sufficiently, be then added metallic tin, stirring 5~
60min is completely melt metallic tin.
5. as described in claim 1 including the lead storage battery grid alloy of nanometer tungsten carbide material, which is characterized in that step b)
In, 1~3h is stirred after being pressed into sheet lead packet.
6. as described in claim 1 including the lead storage battery grid alloy of nanometer tungsten carbide material, which is characterized in that step I)
In, being heated to 320~350 DEG C melts lead pig.
7. as described in claim 1 including the lead storage battery grid alloy of nanometer tungsten carbide material, which is characterized in that step
II) in, 5~60min is stirred after master alloy ingot is added.
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| CN111647769B (en) * | 2020-06-18 | 2021-03-30 | 超威电源集团有限公司 | Storage battery grid alloy and preparation method thereof |
| CN114134538B (en) * | 2021-12-08 | 2024-03-26 | 昆明理工恒达科技股份有限公司 | Zinc electrowinning system suitable for high current density |
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| JPS4839332B1 (en) * | 1968-10-31 | 1973-11-22 | ||
| US3879217A (en) * | 1973-03-15 | 1975-04-22 | Electric Power Storage Ltd | Electric storage battery grids |
| EP1093674A1 (en) * | 1998-06-17 | 2001-04-25 | C & D Technologies, Inc. | Catalyst equipped vapor-communicating multi-cell valve regulated lead-acid battery |
| CN104073683A (en) * | 2014-06-27 | 2014-10-01 | 天能集团江苏科技有限公司 | Low-temperature deep-cycle positive grid alloy and preparation method thereof |
| CN104073682A (en) * | 2014-06-27 | 2014-10-01 | 浙江天能电池(江苏)有限公司 | Long-service-life deep-cycle positive grid alloy and preparation method thereof |
| CN105648268A (en) * | 2016-04-12 | 2016-06-08 | 李程 | Radiation-shielding high-voltage grid power distribution cabinet |
| CN105671362A (en) * | 2016-03-22 | 2016-06-15 | 安徽华铂再生资源科技有限公司 | Lanthanum mother alloy for positive electrode grid of lead-acid storage battery and preparation process |
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2017
- 2017-05-25 CN CN201710380920.4A patent/CN107287470B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4839332B1 (en) * | 1968-10-31 | 1973-11-22 | ||
| US3879217A (en) * | 1973-03-15 | 1975-04-22 | Electric Power Storage Ltd | Electric storage battery grids |
| EP1093674A1 (en) * | 1998-06-17 | 2001-04-25 | C & D Technologies, Inc. | Catalyst equipped vapor-communicating multi-cell valve regulated lead-acid battery |
| CN104073683A (en) * | 2014-06-27 | 2014-10-01 | 天能集团江苏科技有限公司 | Low-temperature deep-cycle positive grid alloy and preparation method thereof |
| CN104073682A (en) * | 2014-06-27 | 2014-10-01 | 浙江天能电池(江苏)有限公司 | Long-service-life deep-cycle positive grid alloy and preparation method thereof |
| CN105671362A (en) * | 2016-03-22 | 2016-06-15 | 安徽华铂再生资源科技有限公司 | Lanthanum mother alloy for positive electrode grid of lead-acid storage battery and preparation process |
| CN105648268A (en) * | 2016-04-12 | 2016-06-08 | 李程 | Radiation-shielding high-voltage grid power distribution cabinet |
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Address after: 313100 Coal Mountain Industrial Park, Changxing County, Huzhou City, Zhejiang Province Patentee after: Tianneng Battery Group Co., Ltd. Address before: 313100 Coal Mountain Industrial Park, Changxing County, Huzhou City, Zhejiang Province Patentee before: Tianneng Battery Group Co., Ltd. |