CN100588729C - Lead alloy, uses and manufacturing technique thereof - Google Patents
Lead alloy, uses and manufacturing technique thereof Download PDFInfo
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- CN100588729C CN100588729C CN200710120087A CN200710120087A CN100588729C CN 100588729 C CN100588729 C CN 100588729C CN 200710120087 A CN200710120087 A CN 200710120087A CN 200710120087 A CN200710120087 A CN 200710120087A CN 100588729 C CN100588729 C CN 100588729C
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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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Abstract
The embodiment of the invention provides a leaded alloy, an application and a manufacturing method thereof. The components of the leaded alloy are silver, lead and rare earth metals; the weight percentage of every component is 0.005-0.20 percent of the silver, 0.005-0.3 percent of the rare earth metals and the rest is the reductive lead; the sum of the weight percentage of all the components is equal to 100 percent. The invention also provides an application of the leaded alloy, namely, the leaded alloy is applied in a slab lattice of a valve-controlled storage battery of an electric bicycle;the invention also provides a manufacturing method of the leaded alloy. The leaded alloy is characterized by corrosion resistance, environment protection, and long cycle life for deep discharge, etc.
Description
Technical field
The present invention relates to a kind of lead alloy and application thereof and manufacture method, relate in particular to a kind of application and manufacture method of lead alloy of grid of electric bicycle valve-control storage battery.
Background technology
Electric bicycle valve-control storage battery grid is a most important inactive substance in the lead acid cell, and it plays a part to support active substance and conduction, and grid mainly is that plumbous antimony (Pb-Sb) is and plumbous calcium (Pb-Ca) tie-plate grid alloy.Lead antimony alloy tensile strength, ductility, hardness and grain refining effect obviously are better than pure Plante type plate; Grid is not yielding in the mill; Its fusing point and shrinking percentage are lower than pure lead, have good castability; The pure lead of Pb-Sb alloy ratio has lower thermal expansivity, and between the usage period, grid is not yielding in charging cycle.The most important thing is that the Pb-Sb alloy can effectively improve the adhesivity between grid and the active substance, strengthened " wrapping up in attached power " between grid and the active substance, help the lead storage battery cycle charge discharge life-span, antimony is the catalyzer of plumbic oxide nucleation simultaneously, stoped growing up of active substance crystal grain, make the active substance difficult drop-off, improved the capacity and the life-span of battery.And current electric bicycle valve-control storage battery with grid in the representative of Pb-Sb tie-plate grid alloy be exactly plumbous antimony cadmium (Pb-Sb-Cd) alloy.But because the existence of Cd element in the Pb-Sb-Cd alloy, the direct labor to a line when producing has serious harm, not environmental protection.The existence of antimony causes the reduction of maintenance-free performance, and the Pb-Sb-Cd alloy maintenance-free performance that adds cadmium Cd is better than Pb-Sb alloy, so be not that silver-colored existence causes maintenance-free performance to reduce.
Pb-Ca tie-plate grid alloy has excellent maintenance-free performance; Appearance along with maintenance-free lead-acid battery; Substitute gradually Pb-Sb tie-plate grid alloy; And wherein modal be plumbous calcium tin cadmium (Pb-Ca-Sn-Cd) alloy; But because the existence of Ca element; So that the surface of alloy easily generates the poor corrosion resistance of high impedance passivating film and alloy; The carrying out of battery charge and discharge process and the service life of battery have been had a strong impact on; Though the Cd element has suppressed the generation of high impedance passivating film to a certain extent; But not from this upper head it off more
Thereby shorten the work-ing life of battery; And because the Cd element is a kind of deleterious element, the workman is bigger to physical effects in a line is produced, not environmental protection.
In sum, in realizing process of the present invention, the contriver finds that there are the following problems at least in the prior art:
1) corrosion-resistant relatively poor
When the user used Pb-Sb-Cd or Pb-Ca-Sn-Cd alloy, its alloy intergranular corrosion phenomenon was serious, poor corrosion resistance.
2) environmental issue
When the user uses Pb-Sb-Cd or Pb-Ca-Sn-Cd alloy,, be unfavorable for environmental protection because the existence of poisonous Elements C d has serious harm to the workers'health of forefront of the production in the alloy.
3) deep discharge cycle life is short
Because energy storage battery may be in sunlight and be exposed to the sun under the severe environment, cause internal temperature of battery to increase severely, cell reaction quickens, and the life of storage battery shortens.Recycling deeply, make battery early stage capacitance loss occur in Pb-Sb-Cd or the Pb-Ca-Sn-Cd alloy, equally also can shorten battery deep discharge cycle life because the existence of passive film causes the battery recharge difficulty.
Summary of the invention
In view of above-mentioned existing in prior technology problem, embodiment of the present invention provides a kind of lead alloy and application and manufacture method, add rare earth element in the alloy to improve the corrosion resistance nature and the cycle life of alloy, reach environmental protection requirement simultaneously.
Following percentage composition is weight percent content except that specified otherwise.
Embodiment of the present invention is achieved through the following technical solutions: the invention provides a kind of lead alloy, the composition component of described lead alloy comprises silver, lead, and the weight percent of each component is as follows:
Silver Ag 0.005%～0.20%; That described lead alloy also comprises is at least a in calcium metal, tin, the aluminium, its weight percent is as follows:
Calcium Ca 0.05%～0.12%
Tin Sn 0.6%～2.0%
Aluminium Al 0.01%～0.04%
Reduce plumbous Pb surplus;
The composition weight percent sum of described each component is 100%.
Its preferred weight percent is as follows:
Silver Ag 0.006%～0.15%
Plumbous Pb surplus
The composition weight percent sum of described each component is 100%.
Its optimum weight per-cent is as follows:
Silver Ag 0.01%～0.1%
Plumbous Pb surplus
The composition weight percent sum of described each component is 100%.
Described lead alloy can also comprise rare earth metal, and its weight percent content is respectively: rare earth metal 0.005%～0.3%, and it takies plumbous weight percent content; Its preferred weight percent content is rare earth metal 0.008%～0.2%, and its optimized percentage content is rare earth metal 0.01%～0.1%; Described preferred and best degree all takies plumbous weight percent content.
Rare earth metal in the above-mentioned lead alloy can be: lanthanum, samarium, cerium, yttrium or mishmetal.
Its preferred weight percent is as follows:
Calcium Ca 0.06%～0.10%
Tin Sn 0.8%～1.6%
Aluminium Al 0.015%～0.03%
It takies plumbous weight percent content.
Its optimum weight degree is as follows:
Calcium Ca 0.07%～0.09%
Tin Sn 1.0%～1.5%
Aluminium Al 0.018%～0.02%
It takies plumbous weight percent content.
The present invention also provides a kind of lead alloy, comprises silver, lead, calcium, aluminium, tin, and the weight percent of each component is as follows:
Calcium Ca 0.05%～0.12%
Tin Sn 0.6%～2.0%
Aluminium Al 0.01%～0.04%
Silver Ag 0.005%～0.20%
Reduce plumbous Pb surplus;
The composition weight percent sum of described each component is 100%.
Its preferred weight percent content is:
Calcium Ca 0.06%～0.10%
Tin Sn 0.8%～1.6%
Aluminium Al 0.015%～0.03%
Silver Ag 0.005%～0.15%
Reduce plumbous Pb surplus;
The composition weight percent sum of described each component is 100%.
Its optimum weight degree is:
Calcium Ca 0.07%～0.09%
Tin Sn 1.0%～1.5%
Aluminium Al 0.018%～0.02%
Silver Ag 0.01%～0.1%
Reduce plumbous Pb surplus;
The composition weight percent sum of described each component is 100%.
The present invention also provides the application of above-mentioned lead alloy, and it is applied to the grid of electric bicycle valve-control storage battery.
The present invention also provides a kind of manufacture method of producing lead alloy to comprise following steps:
A, with the purity at least of easy oxidation, scaling loss be 99.9% Ca and at least purity be 99.9%Al under 600～800 ℃ of temperature, vacuumize, carry out the master alloy that melting makes Ca-Al in the crucible furnace of logical nitrogen protection;
B, with the purity at least of surplus be 99.9% Pb, at least purity be 99.9%Sn and at least purity be that 99.9%Ag adds described master alloy according to the ratio of components calculated amount, the alloy melting back insulation 30 minutes that finishes is treated in melting under 550～650 ℃ of temperature, stir, static, drag for slag, sampling.
C, usefulness direct reading spectroscopic instrument are analyzed the alloy composition, carry out the alloy ingredient adjustment according to the sample composition, reach the requirement of component per-cent until the lead alloy Chemical Composition.
By the above-mentioned technical scheme that provides as can be seen, the present invention has advantages such as erosion resistance, environmental protection and deep discharge have extended cycle life.
Embodiment
For further describing embodiment of the present invention, now in conjunction with specific embodiments its technical scheme is described further:
Embodiment one: a kind of lead alloy, and the composition component of described lead alloy comprises silver, lead, the weight percent of each component is as follows: silver-colored Ag 0.005%～0.20%, the plumbous Pb surplus of reduction, the composition weight percent sum of described each component is 100%.Produce the middle-weight rare earths metal in reality and can be lanthanum, samarium, cerium, yttrium or mishmetal.
Below the contained element of lead alloy is carried out the technique effect of concrete analysis to explain that it is reached.Implement the lead alloy in 1 owing to contain physical strength and the creep resistance that argent has obviously improved metal, improved the deep discharge cycle performance of maintenance-free battery, the corrosion impedance of alloy strengthens greatly, and insensitive to passivation, particularly in lead alloy, add 0.005%～0.20% silver and can make above-mentioned effect more obvious.
Content obtains lead alloy in can table 1 in the present embodiment
Table 1
Unit: % (weight percent)
| Component | Embodiment 11 | Embodiment 12 | Embodiment 13 | Embodiment 14 | Embodiment 15 | Embodiment 16 |
| Silver Ag | 0.005 | 0.006 | 0.01 | 0.1 | 0.15 | 0.2 |
| Plumbous Pb | Surplus | Surplus | Surplus | Surplus | Surplus | Surplus |
Embodiment two: a kind of lead alloy, the composition component of described lead alloy comprises silver, lead and rare earth metal, the weight percent of each component is as follows: silver-colored Ag 0.005%～0.20%, rare earth metal 0.005%～0.3%, the plumbous Pb surplus of reduction, the composition weight percent sum of described each component is 100%.Produce the middle-weight rare earths metal in reality and can be lanthanum, samarium, cerium, yttrium or mishmetal.
Rare earth element is a kind of additive of monosodium glutamate formula, and it is widely used in every field and bigger to oxygen, sulphur, hydrogen, aluminium ground avidity.Because rare earth element can make the sulfide of alloy become sphere, so it is effective to solving the lead alloy cold cracking that causes because of sulphur content is too high.By the application of above rare earth in the especially metallurgical row of various industries, rare earth element is as the slab lattice alloy of lead-acid battery additive, and mechanical property, corrosion resistance nature, castability and the conductivity etc. of grid alloy are had more or less benefit.And our lead alloy performance in sulphuric acid soln to rare earth element studies show that, adding rare earth element can make the overpotential of hydrogen evolution of alloy and the corrosion resistance nature of alloy significantly improve in lead alloy, also can improve simultaneously the dark circulatory function of grid alloy, the mishmetal effect that particularly adds 0.006%～0.10% lanthanum, 0.005%～0.12% samarium or 0.005%～0.12% is better.Because rare earth alloy has substituted prior art electric bicycle valve-control storage battery with the Cd element in the grid lead alloy, greatly reduces the influence to environment, helps the healthy of a line Manufacturing Worker, can reach environmental protection requirement.
Content obtains lead alloy in can table 2 in the present embodiment
Table 2
Unit: % (weight percent)
| Component | Embodiment 21 | Embodiment 22 | Embodiment 23 | Embodiment 24 | Embodiment 25 | Embodiment 26 |
| Silver Ag | 0.005 | 0.006 | 0.01 | 0.1 | 0.15 | 0.2 |
| Rare earth metal | 0.005 | 0.008 | 0.01 | 0.1 | 0.2 | 0.3 |
| Plumbous Pb | Surplus | Surplus | Surplus | Surplus | Surplus | Surplus |
Embodiment three: add 0.05%～0.12% calcium, 0.6%～2.0% tin and 0.01%～0.04% aluminium and can make the performance such as corrosion-resistant, deep discharge cycle life, environmental protection of alloy better in embodiment two.
Content obtains lead alloy in can table 3 in the present embodiment
Table 3
Unit: % (weight percent)
| Component | Embodiment 31 | Embodiment 32 | Embodiment 33 | Embodiment 34 | Embodiment 35 | Embodiment 36 |
| Silver Ag | 0.005 | 0.006 | 0.01 | 0.1 | 0.15 | 0.2 |
| Calcium Ca | 0.05 | 0.06 | 0.07 | 0.09 | 0.1 | 0.12 |
| Tin Sn | 0.6 | 0.8 | 1 | 1.5 | 1.6 | 2 |
| Aluminium Al | 0.01 | 0.015 | 0.018 | 0.02 | 0.03 | 0.04 |
| Rare earth metal | 0.005 | 0.008 | 0.01 | 0.1 | 0.2 | 0.3 |
| Plumbous Pb | Surplus | Surplus | Surplus | Surplus | Surplus | Surplus |
Embodiment four: a kind of lead alloy, the composition component of described lead alloy comprises silver, lead, calcium, aluminium, tin, and the weight percent of each component is as follows: calcium Ca 0.05%～0.12%, tin Sn 0.6%～2.0%, aluminium Al 0.01%～0.04%, silver-colored Ag 0.005%～0.20%, the plumbous Pb surplus of reduction; The composition weight percent sum of described each component is 100%.
Crystal colloidal theory according to Povlov, active substance and corrosive film all are to have crystal region and gel region to constitute, gel region is to be made of linear hydrated polymer chain, between crystal region, play the connection electric action, rise and decompose the prolongation that will be unfavorable for electrode life, the avidity of Ag and water is higher, polymer chain is aquation to a certain extent, silver ions is easy to form polymer network with the hydrated polymer chain combination, effect is as tamanori, and these tamanoris can the support polymer networks and stoped its change owing to positive active material density to be decomposed promptly to have the prevention corrosive to further develop simultaneously.Yin oxidation products can be mingled with in corrosive film in addition, as doped semiconductor, thereby improve the electroconductibility of internal layer corrosive film, electro-chemical test shows that the interpolation of silver has obviously improved the deep discharge cycle performance of maintenance-free battery, the corrosion impedance of alloy strengthens greatly, and insensitive to passivation.
Content obtains lead alloy in can table 4 in the present embodiment
Table 4
Unit: % (weight percent)
| Component | Embodiment 41 | Embodiment 42 | Embodiment 43 | Embodiment 44 | Embodiment 45 | Embodiment 46 |
| Silver Ag | 0.005 | 0.006 | 0.01 | 0.1 | 0.15 | 0.2 |
| Calcium Ca | 0.05 | 0.06 | 0.07 | 0.09 | 0.1 | 0.12 |
| Tin Sn | 0.6 | 0.8 | 1 | 1.5 | 1.6 | 2 |
| Aluminium Al | 0.01 | 0.015 | 0.018 | 0.02 | 0.03 | 0.04 |
| Plumbous Pb | Surplus | Surplus | Surplus | Surplus | Surplus | Surplus |
Embodiment five: a kind of manufacture method of lead alloy may further comprise the steps:
A, with the purity at least of surplus be 99.9% Pb, at least purity be 99.9%Ag according to the melting under 550～650 ℃ of temperature of ratio of components calculated amount, treat the alloy melting back insulation 30 minutes that finishes, stir, static, drag for slag, sampling;
B, usefulness direct reading spectroscopic instrument are analyzed the alloy composition, carry out the alloy ingredient adjustment according to the sample composition, reach the requirement of component per-cent until the lead alloy Chemical Composition.
It is a kind of based on realizing production technique of the present invention that the present invention also provides, and the step of preparation embodiment one described lead alloy comprises:
A, with the purity at least of surplus be 99.9% Pb and at least purity be that 99.9%Ag adds described master alloy according to the ratio of components calculated amount, the alloy melting back insulation 30 minutes that finishes is treated in melting under 550～650 ℃ of temperature, stirs, and is static, drags for slag, sampling;
B, usefulness direct reading spectroscopic instrument are analyzed the alloy composition, carry out the alloy ingredient adjustment according to the sample composition, reach the requirement of component per-cent until the alloy composition.
The step of preparation embodiment two described lead alloys comprises:
A, will be at least purity be 99.9% rare earth alloy under 600～1000 ℃ of temperature, vacuumize, carry out melting in the crucible furnace of logical nitrogen protection and make master alloy;
B, with the purity at least of surplus be 99.9% Pb and at least purity be that 99.9%Ag adds described master alloy according to the ratio of components calculated amount, the alloy melting back insulation 30 minutes that finishes is treated in melting under 550～650 ℃ of temperature, stir, static, drag for slag, sampling;
C, usefulness direct reading spectroscopic instrument are analyzed the alloy composition, carry out the alloy ingredient adjustment according to the sample composition, reach the requirement of component per-cent until the alloy composition.
Embodiment six: the production technique of the embodiment of the invention four is to choose batching in ratio in the table 4:
A, with the purity at least of easy oxidation, scaling loss be 99.9% Ca and at least purity be 99.9%Al under 600～800 ℃ of temperature, vacuumize, carry out the master alloy that melting makes Ca-Al in the crucible furnace of logical nitrogen protection;
B, with the purity at least of surplus be 99.9% Pb, at least purity be 99.9%Sn and at least purity be that 99.9%Ag adds described master alloy according to the ratio of components calculated amount, the alloy melting back insulation 30 minutes that finishes is treated in melting under 550～650 ℃ of temperature, stir, static, drag for slag, sampling;
C, usefulness direct reading spectroscopic instrument are analyzed the alloy composition, carry out the alloy ingredient adjustment according to the sample composition, reach the requirement of component per-cent until the alloy composition.
Embodiment seven: the production technique of the embodiment of the invention three is to choose batching in ratio in the table 3:
A, with the purity at least of easy oxidation, scaling loss be 99.9% Ca, at least purity be 99.9%Al and rare earth alloy under 600～1000 ℃ of temperature, vacuumize, carry out the master alloy that melting makes Ca-Al in the crucible furnace of logical nitrogen protection;
B, with the purity at least of surplus be 99.9% Pb, at least purity be 99.9%Sn and at least purity be that 99.9%Ag adds described master alloy according to the ratio of components calculated amount, the alloy melting back insulation 30 minutes that finishes is treated in melting under 550～650 ℃ of temperature, stir, static, drag for slag, sampling;
C, usefulness direct reading spectroscopic instrument are analyzed the alloy composition, carry out the alloy ingredient adjustment according to the sample composition, reach the requirement of component per-cent until the alloy composition.
Above-mentioned rare earth metal can be at least purity be 99.9% lanthanum, at least purity be 99.9% samarium, at least purity be 99.9% cerium and at least purity be 99.9% yttrium, also can be mishmetal.
When rare earth metal was lanthanum, the lead alloy effect that obtains when the temperature of steps A is controlled at 600～800 ℃ was better; When rare earth metal was samarium, the lead alloy effect that obtains when the temperature of steps A is controlled at 600～900 ℃ was better.
In sum, technical scheme of the present invention has characteristics such as environmental protection, corrosion resistance nature are strong, deep discharge cycle life height with respect to prior art.
The above; only be the preferable embodiment of the present invention; but protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the embodiment of the invention discloses; the variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claim.
Claims (6)
1, a kind of lead alloy is characterized in that, the composition component of described lead alloy comprises that the weight percent of silver, plumbous each component is as follows:
Silver Ag 0.005%～0.20%;
Described lead alloy also comprises in calcium metal, tin, the aluminium at least a; Its weight percent content is:
Calcium Ca 0.05%～0.12%
Tin Sn 0.6%～2.0%
Aluminium Al 0.01%～0.04%
Reduce plumbous Pb surplus;
The composition weight percent sum of described each component is 100%.
2, lead alloy according to claim 1 is characterized in that, described lead alloy also comprises rare earth metal, and its weight percent is as follows:
Rare earth metal 0.005%～0.3%
And rare earth metal takies plumbous weight percent content.
3, lead alloy according to claim 2 is characterized in that, described rare earth metal comprises in lanthanum, samarium, cerium, yttrium or the mishmetal at least a.
According to the application of the arbitrary described lead alloy of claim 1～3, it is characterized in that 4, described lead alloy is applied to the grid of electric bicycle valve-control storage battery.
5, the application of lead alloy according to claim 4 is characterized in that, described lead alloy is applied to the grid of electric bicycle valve-control storage battery.
6, the manufacture method of lead alloy according to claim 1 is characterized in that, comprises following steps:
A, with the purity at least of easy oxidation, scaling loss be 99.9% Ca and at least purity be 99.9%Al under 600～800 ℃ of temperature, vacuumize, carry out the master alloy that melting makes Ca-Al in the crucible furnace of logical nitrogen protection;
B, with the purity at least of surplus be 99.9% Pb, at least purity be 99.9%Sn and at least purity be that 99.9%Ag adds described master alloy according to the ratio of components calculated amount, the alloy melting back insulation 30 minutes that finishes is treated in melting under 550～650 ℃ of temperature, stir, static, drag for slag, sampling.
C, usefulness direct reading spectroscopic instrument are analyzed the alloy composition, carry out the alloy ingredient adjustment according to the sample composition, reach the requirement of component per-cent until the lead alloy Chemical Composition.
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