CN102280626A - Composite lead dioxide electrode plate and manufacturing method thereof - Google Patents
Composite lead dioxide electrode plate and manufacturing method thereof Download PDFInfo
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- CN102280626A CN102280626A CN201010203738XA CN201010203738A CN102280626A CN 102280626 A CN102280626 A CN 102280626A CN 201010203738X A CN201010203738X A CN 201010203738XA CN 201010203738 A CN201010203738 A CN 201010203738A CN 102280626 A CN102280626 A CN 102280626A
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Abstract
The invention discloses a composite lead dioxide electrode plate, which comprises a composite lead dioxide anode plate and a protective net covering the periphery of the composite lead dioxide anode plate, wherein the composite lead dioxide anode plate is arranged in a framework and comprises a plurality of small anode plates spliced and connected with one another; and each small anode plate comprises a titanium substrate, a transition layer coated on the titanium substrate, an alpha-PbO2 interlayer coated on the transition layer and a beta-PbO2 active layer coated on the alpha-PbO2 interlayer; and the transition layer comprises at least one component of Pt, IrO2, Ta and Ta2O5. Correspondingly, the invention also provides a method for manufacturing the composite lead dioxide electrode plate. The composite lead dioxide electrode plate prepared by the method has long service life, the passivation process is stable, and an excellent implementation effect is achieved.
Description
Technical field
The present invention relates to battery lead plate and manufacture method thereof, relate in particular to a kind of lead dioxide electrode plate and manufacture method thereof.
Background technology
Passivation Treatment is the important ring in the electrotinning process, and purpose is at the passivating film that generates one deck densification through zinc-plated belt steel surface, prevents that tin plate from oxidation taking place in air, thereby strengthens the corrosion resistance of tin plate and covering with paint property.General paralysis facility mainly is made up of cell body, passivating solution, passivated electrodes plate, conductive rollers and rectifier etc., wherein the passivated electrodes plate links to each other with the positive pole of rectifier, for Passivation Treatment provides required electric current, electric current acts on the band steel by passivating solution, forms passivating film at belt steel surface.
Conventional Electroplating Tin Set Passivation Treatment adopts mild steel as battery lead plate more, and such battery lead plate manufacture craft is simple, and cost is lower.But above-mentioned mild steel battery lead plate is the problem of following three aspects of ubiquity in use:
1. mild steel battery lead plate corrosion rate is fast, and corrosion product pollutes passivating solution.Generally between 4.5～5.5, corrosion reaction can take place to the pH value of passivating solution in the mild steel battery lead plate in this acid solution, and produces electrochemical reaction under the effect of passivation current, and corrosion rate is accelerated.When adopting the mild steel battery lead plate as the passivated electrodes plate, corrosion thickness every year on average is up to 15～30mm, and mild steel battery lead plate corrosion back produces a large amount of free carbons, free carbon does not produce reaction with other material after entering passivating solution, is present in the passivating solution with suspension, pollutes passivating solution, when being increased to, carbon just begins enrichment after a certain amount of, be easy to stick to belt steel surface, form the material of the highly dispersed shape of one deck grey black, be called " grey black " defective at belt steel surface.So when adopting mild steel, will change the one-time electrode plate in per about 6 months, and tin plate sheet surface grey black degree is heavy, influences tin plate sheet surface quality and covering with paint property as passivation positive electricity pole plate.
2. the easy oxidation of mild steel battery lead plate causes the passivation effect instability.Very fast generation oxidation reaction behind the mild steel battery lead plate immersion passivating solution, the product of oxidation reaction has FeO, Fe
2O
3And Fe
3O
4These oxides constantly dissolve in passivating solution again in forming process, the oxide components that plays discharge process in the different phase that the mild steel battery lead plate uses constantly changes, and causes the passivation effect instability, passivation film thickness changes greatly, causes the tin plate unstable product quality.
3. the mild steel battery lead plate is subjected to being with steel drift to hit easily, causes scratch and damage: the band steel carries out high-speed cruising with the speed of 200～500m/min in tin plate industrialized production process, and the passivating solution in the deactivation slot is also with 10～30m
3The flow velocity of/h circulates, and the spacing of band steel and battery lead plate only is about 40mm, therefore when belt plate shape is not good, produce to wipe with battery lead plate easily and bump and contact in short-term, electric current directly was transferred to from the positive electricity pole plate and was with steel to cause short circuit this moment, thereby cause the galled spots and the localized burn of positive electricity pole plate, can cause the damage of passivated electrodes plate when serious and then cause the whole piece unit to stop production, influence the steady production of unit.
More than the problem of three aspects are technical barriers that Electroplating Tin Set can't be avoided when using conventional mild steel passivated electrodes plate, therefore need a kind of novel passivated electrodes plate that is applicable to zinc-plated unit Passivation Treatment of invention, address the above problem.
Summary of the invention
The purpose of this invention is to provide a kind of composite lead dioxide battery lead plate and manufacture method thereof, this composite lead dioxide battery lead plate has good corrosion resistance and discharging function, the top layer of this composite lead dioxide battery lead plate should not come off in addition, can effectively avoid bumping and short circuit with the wiping of steel and pole plate, thereby prolong the useful life of battery lead plate, solve the various deficiencies that existing conventional mild steel passivation pole plate exists.
According to above-mentioned purpose of the present invention, a kind of composite lead dioxide battery lead plate is proposed, comprising:
One dioxide composite chloride plate is installed in the framework, comprises the some blocks of primary anode plates that assembly unit each other connects, and described each primary anode plate includes: a titanium-base, is overlying on transition zone, on the titanium-base and is overlying on α-PbO on the transition zone
2The intermediate layer, and one be overlying on α-PbO
2β-PbO on the intermediate layer
2Active layer, the constituent of described transition zone are Pt, IrO
2, Ta, Ta
2O
5In at least a;
One anti-net covers in described dioxide composite chloride plate periphery.
Transition zone in the above-mentioned dioxide composite chloride plate can reduce the oxidation rate of titanium-base, β-PbO
2Active layer is a discharge layer, and its discharging function is cut well has good decay resistance, but β-PbO
2Enbrittle, the inventor passes through at β-PbO
2Between active layer and the transition zone α-PbO is set
2The intermediate layer reduces β-PbO
2Fragility, and the design of anti-net can effectively be avoided being with steel to wipe and be bumped the composite lead dioxide battery lead plate, causes the galled spots and the short circuit scaling loss of pole plate.
Preferably, also be provided with an insulation net between described dioxide composite chloride plate and the anti-net.Under the energising situation, if the band steel contacts with anti-net, can make power supply short circuit, scaling loss is prevented net, therefore is provided with the insulation net between anti-net and lead dioxide electrode plate.
Preferably, the area of described primary anode plate is 0.2～0.4m
2The inventor finds in the invention process, because the phenomenon of expanding with heat and contract with cold of anode of lead dioxide is more serious, when annode area is big, cause coming off of top layer brown lead oxide coating easily, therefore the inventor is divided into plurality of small blocks with monoblock composite lead dioxide battery lead plate, and the area of each piece is controlled at 0.2～0.4m
2Between, thereby the quality of assurance brown lead oxide coating.
Preferably, the constituent of described transition zone is Pt+IrO
2+ Ta
2O
5
The inventor is by evidence, and the constituent of transition zone comprises Pt, IrO
2, Ta, Ta
2O
5In at least aly all can realize the technical program, but its implementation result is slightly different, specifically sees Table 1:
Table 1
| The transition zone constituent | Pt | Pt+IrO 2 | IrO 2+Ta 2O 5 | Ta | Pt+IrO 2+Ta 2O 5 |
| Price | The highest | Higher | Lower | Higher | Higher |
| The manufacture craft difficulty | The easiest | Easier | Easier | The most difficult | Easier |
| Improve effect anode life | Bigger | Bigger | Bigger | Bigger | Maximum |
| Corrosion resistance | Better | Relatively poor | The poorest | Better | Best |
Need be appreciated that, the evaluation of " relatively poor ", " better " is the collocation of each constituent described in the present invention and the comparison of choosing the implementation result of being realized in the table 1, but not the comparison of technical solutions according to the invention and prior art, even if be evaluated as " relatively poor " in the table 1, its performance index also are better than prior art.
Preferably, described anti-net is the titanium net.The purpose of preferred titanium net is its good toughness, and the resistance to wear height is difficult in the course of the work by the scratch of band steel.
Correspondingly, the present invention also provides a kind of manufacture method of above-mentioned composite lead dioxide battery lead plate, and wherein, the manufacturing step of described primary anode plate comprises:
(1) pre-treatment of titanium-base: the titanium oxide of removing the titanium-base surface according to the order of alkali cleaning → pickling → texturing;
(2) transition zone preparation: will in sintering solution, carry out sintering through the titanium-base of pre-treatment, sintering temperature is controlled at 450～500 ℃, the solvent of described sintering solution is an alcohol, and solute is at least a in platinum salt, iridium salt or the tantalum salt, and the thickness of finally controlling transition zone is 3～5 μ m;
(3) α-PbO
2The preparation in intermediate layer: will be through the titanium-base of transition zone preparation at Pb
2+Concentration is that 120～145g/L, NaOH concentration are to electroplate in the aqueous solution of 4～8mol/L, and electroplating temperature is controlled at 40～50 ℃, and current density is controlled at 3～7A/dm
2, finally control α-PbO
2The thickness in intermediate layer is 10～20 μ m;
(4) β-PbO
2The preparation of active layer: will be through α-PbO
2The titanium-base of intermediate layer preparation is at HNO
3Concentration is 0.1～0.2mol/L, Pb
+Concentration is to electroplate in the mixed aqueous solution of 0.3～0.8mol/L, and electroplating temperature is controlled at 60～80 ℃, and current density is controlled at 2～5A/dm
2, finally control β-PbO
2The thickness of active layer is 0.5～1.0mm.
Preferably, sintering solution is Pt in the described step (2)
4+Concentration be 10～20g/L, Ta
5+Concentration be 30～70g/L, Ir
4+Concentration be the alcoholic solution of 30～70g/L.
After making above-mentioned primary anode plate, some blocks of primary anode plates are assembled into a bulk of anode of lead dioxide plate, are installed in the framework then.On the forward and backward two sides of anode of lead dioxide plate the insulation net is installed then, in the outside of insulation net anti-net is installed then.
The present invention makes it compared to prior art owing to adopted technique scheme, has following advantage:
(1) the composite lead dioxide battery lead plate is slow as anodic attack speed, has guaranteed the cleaning of passivating solution, can significantly alleviate the grey black degree of belt steel surface;
(2) use the composite lead dioxide battery lead plate, the stable of passivation effect index such as band steel passivation film thickness are increased dramatically, the maximum of lead dioxide electrode plate in passivating process uses current density can reach 50A/dm far above the current density of mild steel battery lead plate in passivating process
2, this current density is about 5 times of ordinary low-carbon steel battery lead plate, therefore can increase strip speed, improves output;
(3) be much higher than existing mild steel battery lead plate the useful life of composite lead dioxide battery lead plate, can reach 12 months its average life, and only have 6 months the useful life of ordinary low-carbon steel anode.
Description of drawings
Fig. 1 is the structural scheme of mechanism of composite lead dioxide battery lead plate in a kind of exemplary embodiment of the present invention.
Fig. 2 is the structural representation of a certain primary anode plate in the composite lead dioxide battery lead plate of the present invention.
Fig. 3 is a composite lead dioxide electrode plate structure schematic diagram of the present invention.
Embodiment
Embodiment 1-5
Make the composite lead dioxide battery lead plate by following step among the embodiment of the invention 1-5, at first carry out the manufacturing of primary anode plate, comprise the steps (the concrete technological parameter among each embodiment is referring to table 2):
(1) pre-treatment of titanium-base:
1. alkali cleaning: titanium-base was soaked 20～40 minutes in mass percent concentration is 3～7% the NaOH aqueous solution, and the alkali cleaning temperature is 80～90 ℃;
2. pickling: with titanium-base at H
2SO
4And HNO
3Pickling is 5～15 minutes in the nitration mixture of forming, and pickling temperature is 60～80 ℃, wherein H
2SO
4The mass percent concentration of solution is 5～15%, HNO
3The mass percent concentration of solution is 3～7%;
3. texturing: at pressure is 5～6Kg/cm
2Compressed air in the carborundum of 100～500 order numbers titanium-base is carried out texturing and handles, the titanium-base roughness is controlled at 5～7 μ m after the texturing.
(2) transition zone preparation: will carry out sintering in sintering solution through the titanium-base of pre-treatment, sintering temperature is controlled at 450～500 ℃, and sintering solution is Pt
4+Concentration be 10～20g/L, Ta
5+Concentration be 30～70g/L, Ir
4+Concentration be the alcoholic solution of 30～70g/L.Need be appreciated that, composite lead dioxide electrode plate manufacturing method of the present invention is when the preparation transition zone, the broad matter of sintering solution can be at least a in platinum salt, iridium salt or the tantalum salt, but after taking all factors into consideration multiple factors such as manufacturing cost, performance index, the inventor has all selected the combination of platinum salt, tantalic chloride and iridium chloride as solute in embodiment 1-5, and the thickness of finally controlling transition zone is 3～5 μ m.
(3) α-PbO
2The preparation in intermediate layer: will be through the titanium-base of transition zone preparation at Pb
2+Concentration is that 120～145g/L, NaOH concentration are to electroplate in the aqueous solution of 4～8mol/L, and electroplating temperature is controlled at 40～50 ℃, and current density is controlled at 3～7A/dm
2, finally control α-PbO
2The thickness in intermediate layer is 10～20 μ m;
(4) β-PbO
2The preparation of active layer: will be through α-PbO
2The titanium-base of intermediate layer preparation is at HNO
3Concentration is 0.1～0.2mol/L, Pb
+Concentration is to electroplate in the mixed aqueous solution of 0.3～0.8mol/L, and electroplating temperature is controlled at 60～80 ℃, and current density is controlled at 2～5A/dm
2, finally control β-PbO
2The thickness of active layer is 0.5～1.0mm.
The primary anode plate structure that makes through above-mentioned steps as shown in Figure 2, the center is a titanium-base 1, is followed successively by transition zone 2, α-PbO then from the inside to surface
2 Intermediate layer 3 and β-PbO
2Active layer 4.As shown in figures 1 and 3, some primary anodes 5 plates are assembled into a bulk of anode of lead dioxide plate 9, are installed in then in the framework 8, on the forward and backward two sides of anode of lead dioxide plate 9 insulation net 6 is installed then, the material of insulation net 6 is a polytetrafluoroethylene, and width of mesh is controlled at 2～6cm
2, in the outside of insulation net 6 anti-friction titanium net 7 is installed then, the Thickness Design of anti-net 7 is 1～3mm, mesh is 2～6cm
2 Size.Insulation net 6, anti-net 9 realize with being connected by bolt of anode of lead dioxide plate 9, so at the bolt connecting portion, insulated with fluoroplastic plate and lining, thereby guaranteed the insulation between anti-friction titanium net 7 and the anode of lead dioxide plate 9.
Use is carried out passivation, the following existing processes parameter that still adopts of the main technologic parameters of passivation by the composite lead dioxide battery lead plate that said method makes to the band steel.Check repeatedly that in use do not find phenomenons such as battery lead plate abrades, the titanium net is pulled, the brown lead oxide coating is intact, mesh does not stop up, and can continue to use, and useful life was up to 14 months.
In whole use, passivation film thickness is stable is controlled at 0.3～0.9ug/cm
2, the CPK value reaches more than 1.67, and surperficial grey black is brought up to average one-level level by average three grades.
This shows, the use of composite lead dioxide battery lead plate has improved band steel passivation technology, has reduced the replacing frequency of passivating solution, has reduced defectives such as tin plate sheet surface grey black, roll marks, reduce the frequent environmental pollution caused by discharge of passivating solution, be applicable to zinc-plated unit Passivation Treatment fully.
Be noted that above enumerate only for specific embodiments of the invention, obviously the invention is not restricted to above embodiment, many similar variations are arranged thereupon.If those skilled in the art all should belong to protection scope of the present invention from all distortion that content disclosed by the invention directly derives or associates.
Claims (7)
1. a composite lead dioxide battery lead plate is characterized in that, comprising:
One dioxide composite chloride plate is installed in the framework, comprises the some blocks of primary anode plates that assembly unit each other connects, and described each primary anode plate includes: a titanium-base, is overlying on transition zone, on the titanium-base and is overlying on α-PbO on the transition zone
2The intermediate layer, and one be overlying on α-PbO
2β-PbO on the intermediate layer
2Active layer, the constituent of described transition zone comprises Pt, IrO
2, Ta, Ta
2O
5In at least a;
One anti-net covers in described dioxide composite chloride plate periphery.
2. composite lead dioxide battery lead plate as claimed in claim 1 is characterized in that: also be provided with an insulation net between described dioxide composite chloride plate and the anti-net.
3. composite lead dioxide battery lead plate as claimed in claim 2 is characterized in that: the area of described primary anode plate is 0.2～0.4m
2
4. composite lead dioxide battery lead plate as claimed in claim 3 is characterized in that: the constituent of described transition zone is Pt+IrO
2+ Ta
2O
5
5. as claim 1 or 4 described composite lead dioxide battery lead plates, it is characterized in that: described anti-net is the titanium net.
6. the manufacture method of composite lead dioxide battery lead plate as claimed in claim 1 is characterized in that: the manufacturing step of described primary anode plate comprises:
(1) pre-treatment of titanium-base: the titanium oxide of removing the titanium-base surface according to the order of alkali cleaning → pickling → texturing;
(2) transition zone preparation: will in sintering solution, carry out sintering through the titanium-base of pre-treatment, sintering temperature is controlled at 450～500 ℃, the solvent of described sintering solution is an alcohol, and solute is at least a in platinum salt, iridium salt or the tantalum salt, and the thickness of finally controlling transition zone is 3～5 μ m;
(3) α-PbO
2The preparation in intermediate layer: the titanium-base that will be covered with transition zone is at Pb
2+Concentration is that 120～145g/L, NaOH concentration are to electroplate in the aqueous solution of 4～8mol/L, and electroplating temperature is controlled at 40～50 ℃, and current density is controlled at 3～7A/dm
2, finally control α-PbO
2The thickness in intermediate layer is 10～20 μ m;
(4) β-PbO
2The preparation of active layer: will be covered with α-PbO
2The titanium-base in intermediate layer is at HNO
3Concentration is 0.1～0.2mol/L, Pb
+Concentration is to electroplate in the mixed aqueous solution of 0.3～0.8mol/L, and electroplating temperature is controlled at 60～80 ℃, and current density is controlled at 2～5A/dm
2, finally control β-PbO
2The thickness of active layer is 0.5～1.0mm.
7. the manufacture method of composite lead dioxide battery lead plate as claimed in claim 6 is characterized in that: sintering solution is Pt in the described step (2)
4+Concentration be 10～20g/L, Ta
5+Concentration be 30～70g/L, Ir
4+Concentration be the alcoholic solution of 30～70g/L.
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| CN104362301A (en) * | 2014-10-14 | 2015-02-18 | 浙江南都电源动力股份有限公司 | Carbon coated titanium-based lead dioxide positive plate for lead-acid storage battery |
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| CN104362301A (en) * | 2014-10-14 | 2015-02-18 | 浙江南都电源动力股份有限公司 | Carbon coated titanium-based lead dioxide positive plate for lead-acid storage battery |
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