CN102009504B - Steel strip plated with multi-layer micron/nano-crystal nickel films and preparation method thereof - Google Patents
Steel strip plated with multi-layer micron/nano-crystal nickel films and preparation method thereof Download PDFInfo
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- CN102009504B CN102009504B CN2010101101285A CN201010110128A CN102009504B CN 102009504 B CN102009504 B CN 102009504B CN 2010101101285 A CN2010101101285 A CN 2010101101285A CN 201010110128 A CN201010110128 A CN 201010110128A CN 102009504 B CN102009504 B CN 102009504B
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Abstract
The invention discloses a steel strip plated with multi-layer micron/nano-crystal nickel films and a preparation method thereof. A steel strip is used as a base, and multi-layer micron/nano-crystal nickel films are respectively plated on the two surfaces of the base. The bottom layer of the multi-layer micron/nano-crystal nickel films is a micron-crystal nickel-plated layer, wherein the crystallite dimension of the plated layer is from 0.1 to 0.5 micron, and the thickness of the plated layer is from 0.5 to 2.0 microns. The middle layer of the multi-layer micron/nano-crystal nickel films is a nano-crystal nickel-plated layer, wherein the crystallite dimension of the plated layer is from 50 to 100 nanometers, and the thickness of the plated layer is from 0.5 to 1.5 microns. The surface layer of the multi-layer micron/nano-crystal nickel films is a nano-crystal nickel-plated layer, wherein the crystallite dimension of the plated layer is from 20 to 50 nanometers, and the thickness of the plated layer is from 0.2 to 1 micron. The bottom micron-crystal nickel-plated layer of the multi-layer micron/nano-crystal nickel films is prepared by direct current electroplating, the middle nano-crystal nickel-plated layer is prepared by pulse electroplating, and the surface nano-crystal nickel-plated layer is prepared by pulse jet electroplating. The steel strip has the advantages of excellent elongation, corrosion resistance and stamping properties and can be used as the casing materials of high-performance batteries.
Description
Technical field
The present invention relates to steel band of a kind of plating multi-layer micron/nano-crystal nickel films and preparation method thereof.
Background technology
The steel band of the brilliant nickel film of plating multilayer micro-/ nano is that a kind of multi-layer micron/nano-crystal nickel films and mild steel substrate are combined closely, novel battery casing material with good percentage elongation, antiseptic power and punching performance, but straight forming, need not to carry out follow-up electroplating processes, can realize serialization production.Flourish along with industries such as portable communication apparatus, notebook computer, word processor and electric tools, battery industry will be increasing to the demand of the steel band of the brilliant nickel film of plating multilayer micro-/ nano.
Traditional secondary battery and alkaline primary battery box hat preparation method are with barrel plating layer of metal nickel again after the mild-carbon steel strip punch forming, are used for improving decay resistance.Owing to plating bath in the process of rolling nickel plating plates dark scarce capacity and reasons such as point discharge when electroplating, cause the became uneven of the plating leakage of battery case endoporus and coating, so that the defect rate of battery case is shorter service life high and the battery finished product.
Method at the inner surface plating nickel-cobalt alloy plating of battery steel shell is disclosed in Japanese patent laid-open 10-172521 communique, the Unexamined Patent 10-172522 communique.Because the hardness of nickel cobalt (alloy) is high, therefore when punch process, in coating, formed very thin crackle, cause the surface irregularity, roughness ratio larger, improve contacting of battery container and positive electrode, thereby improved the electrical property of battery.
Method at box hat inner surface plating Ni-Ag alloy layer or Ni-Cr alloy layer is disclosed in the Japanese patent laid-open 11-102671 communique.Because Ni-Ag alloy layer and Ni-Cr alloy layer hardness are all higher, therefore when punch process, generate very thin crackle at coating surface, therefore improve contacting of housing and positive electrode, thereby improved the electrical property of battery.
Chinese patent CN1600904A discloses a kind of nickel-plated deeply-draw steel strip and production method thereof, continuous electroplating 2～3 μ m nickel films on mild-carbon steel strip, process by heat treatment and laser-impact, make nickel coating and base material form nickel/iron diffusion layer by thermal diffusion, then obtain the corrosion-resistant steel band of desired thickness by finishing procedure.The coating percentage elongation is not less than 8%, and decay resistance reaches 8 grades, has good percentage elongation and decay resistance, is mainly used in the heavy-duty battery shell.
A kind of erosion-resisting nickel-clad steel plate or steel band and method for making thereof are disclosed among the Chinese patent ZL93107442.8.It mainly is that steel plate or the steel band of nickel coating carry out forming nickel/iron diffusion layer after the annealing in process to having at least on one side, with adhesion and the decay resistance that improves coating.
Above-described traditional nickel plated steel strip can roughly be divided into two classes, and the first kind has mainly been considered the decay resistance of steel band, and the punching performance of steel band is not had enough attention; Equations of The Second Kind has mainly been considered the punching performance of steel band, improves the case hardness of coating, reduces friction, yet will cause like this steel band crackle dark and many, leaks the iron rate and uprises, so that the decay resistance of material reduces.
In above-mentioned various prior aries, improving case hardness mainly is by form the precious metal alloys coating such as nickel cobalt (alloy), bazar metal on the surface, and then improve coating surface compactness and case hardness through the finishing procedure such as cold rolling, process or heat treatment forms nickel/iron diffusion layer improving binding force of cladding material by laser-impact, complex procedures, production cost are higher.
Summary of the invention
Purpose of the present invention aims to provide a kind of steel band of plating multi-layer micron/nano-crystal nickel films, it has good corrosion resistance energy and punching performance, do not add expensive alloys coating and do not need to anneal and the prerequisite of the operation such as cold rolling under, reach the purpose that binding force of cladding material is good, case hardness is high and fine and close, simplified production process, reduce production cost, reduced the possibility that coating comes off and the surface is scratched.
Another object of the present invention aims to provide the preparation method that above-mentioned steel band is fit to.
The objective of the invention is to realize by following manner.
A kind of steel band of plating multi-layer micron/nano-crystal nickel films, the BDCK battery special steel strip of producing take Shanghai Baoshan Steel stock Co., Ltd be as substrate, the two sides of steel band respectively plating multi-layer micron/nano-crystal nickel films.The bottom of multi-layer micron/nano-crystal nickel films is the brilliant nickel coating of micron, and the coating crystallite dimension is 0.1～0.5 μ m, and thickness is 0.5～2.0 μ m; The intermediate layer of multi-layer micron/nano-crystal nickel films is nano-crystal nickel coating, and the crystallite dimension of coating is 50～100nm, and thickness is 0.5～1.5 μ m; The top layer of multi-layer micron/nano-crystal nickel films is nano-crystal nickel coating, and the crystallite dimension of coating is 20～50nm, and thickness is 0.2～1 μ m.As shown in Figure 1.
The steel band of the brilliant nickel film of plating multilayer micro-/ nano of the present invention has adopted multi-layer film structure, has both improved the bond strength of substrate and coating, also improves coating surface hardness, has reduced the coating porosity, improves the distribution of coating internal stress and crackle.To the top layer, it is negative that current potential becomes gradually by bottom for coating, top layer coating as anode loss protection bottom, improved the decay resistance of material.In addition, because the inventor has carried out effective restriction to the thickness of the film of each layer and the crystallite dimension of formation film, so that the hardness of coating becomes step increase, reduce the coating of steel band in punching course and come off.
By limiting the crystallite dimension (50～100nm) of intermediate layer nano-crystal nickel coating, the crystallite dimension of top layer nano-crystal nickel coating (20～50nm) and specific preparation method (intermediate layer coating is prepared from by the method for pulse plating, outermost layer coating is prepared from by the method for impulse jet), do not adding expensive alloys coating and cancelling under the prerequisite of carrying out cold rolling finishing procedure such as grade after the plating, reached the purpose of case hardness height and coating densification, simplify production process, reduced the possibility that production cost and surface are scratched.
By each coating crystallite dimension of strict control, so that multilayer film is from the bottom to the top layer, it is negative that current potential becomes gradually, and the current potential between the different coating is at 120～150mv, top layer coating as anode loss protection bottom.
The steel band of the brilliant nickel film of plating multilayer micro-/ nano of the present invention is measured through the HV-1000 Vickers, and its coating surface hardness is HV 300 ± 10.
The preparation method of steel band of the present invention is as substrate take BDCK battery special steel strip, on the two sides of steel band respectively plating multi-layer micron/nano-crystal nickel films, the brilliant nickel coating of bottom micron prepares by the mode of direct current electrode position, the nano-crystal nickel coating in intermediate layer prepares by the mode of pulse plating, and the mode that the nano-crystal nickel coating on top layer is electroplated by impulse jet prepares.Each thickness of coating is determined by electroplating time.
The preparation method of steel band of the present invention comprises following concrete Step By Condition:
(1) plating front surface preliminary treatment
The substrate steel band is carried out electrochemical deoiling, activation process.
Degreasing fluid is: NaOH 70g/L
Na
2CO
3 40g/L
Na
3PO
4 25g/L
Na
2SiO
3 10g/L
Degreasing fluid temperature: 80～90 ℃
The oil removing time: 3～5min
After the oil removing fully, with distilled water specimen surface is rinsed well, put into again activator and activate.
Activator forms: 1～5vol%HCl
Soak time: 1～3min.
(2) the brilliant nickel coating of direct current electrode position crystallite dimension 0.1-0.5 μ m micron
Plating bath forms: NiSO
47H
2O 250～300g/L
NiCl
2·6H
2O 30～50g/L
Boric acid 30～50g/L
Direct current electrode position preparation method parameter: current density: 3～6A/dm
2
PH value: 3.5～4.5
Temperature: 40～60 ℃
Anode: nickel plate
(3) the pulse plating crystallite dimension is the nickel coating of 50～100nm
Plating bath forms: NiSO
47H
2O 250～300g/L
NiCl
2·6H
2O 30～50g/L
H
3BO
3 30～50g/L
Cumarin 0.05～0.15g/L
Formaldehyde 0.2～0.3ml/L
Pulse plating preparation method parameter: average current density: 3～6A/dm
2
PH value: 3.5～4.5
i
on： 5～50ms
i
off： 5～250ms
Temperature: 40～60 ℃
Anode: nickel plate
(4) impulse jet plating crystallite dimension is the nickel coating of 20～50nm
Plating bath forms: NiSO
47H
2O 250～300g/L
NiCl
2·6H
2O 30～50g/L
Boric acid 30～50g/L
ALS 0.4～2g/L
Butynediols 0.4～0.5ml/L
Asccharin 0.8～1g/L
Impulse jet electroplating preparation method parameter: peak current density: 47～82A/dm
2
Dutycycle: 15～25%
Plating bath spray speed: 1000～1500L/h
Temperature: 55～65 ℃
PH value: 2.5～3.5
Anode: nickel plate;
(5) it is clean with distilled water flushing to plate good steel band, then oven dry.
The steel band of the brilliant nickel film of the plating multilayer micro-/ nano that the inventive method makes also has higher case hardness having good percentage elongation and corrosion proof while, is beneficial to punch forming, can be used as the sheathing material of heavy-duty battery.
Description of drawings
Fig. 1 is the coating structure schematic diagram of the steel band of the brilliant nickel film of plating multilayer micro-/ nano, and wherein 1 is substrate, and 2 is bottom, and 3 is the intermediate layer, and 4 is the top layer;
Fig. 2 is process chart of the present invention.
The specific embodiment
Following examples are intended to illustrate the present invention rather than limitation of the invention further.
Embodiment:
The steel band of a kind of plating multi-layer micron/nano-crystal nickel films of the present invention, take steel band as substrate 1, on the two sides of substrate 1 respectively plating multi-layer micron/nano-crystal nickel films; Described multi-layer micron/nano-crystal nickel films bottom 2 is crystallite dimension 0.1～0.5 μ m, and thickness is the brilliant nickel coating of micron of 0.5～2.0 μ m; Intermediate layer 3 is crystallite dimension 50～100nm, and thickness is the nano-crystal nickel coating of 0.5～1.5 μ m; Top layer 4 is 20～50nm for crystallite dimension, and thickness is the nano-crystal nickel coating of 0.2～1 μ m.As shown in Figure 1.
Fig. 2 is seen in technological process of the present invention.
The thickness of selecting Shanghai Baoshan Steel stock Co., Ltd to produce is that the BDCK battery special steel strip of 0.25mm is as electroplated substrates.
Its chemical composition is: C:0.029% (% represents percetage by weight, and is lower same)
Si：0.02％
Mn：0.2％
P：0.09％
S：0.003％
Al：0.06％。
1, plating front surface preliminary treatment
First degreasing fluid is put in substrate and carried out chemical high temperature oil removing, then rinse well with the substrate surface of distilled water after with oil removing, put into again activator and activate;
Degreasing fluid is: NaOH 70g/L
Na
2CO
3 40g/L
Na
3PO
4 25g/L
Na
2SiO
3 10g/L
Degreasing fluid temperature: 80 ℃
The oil removing time: 3min
After the oil removing fully, with distilled water specimen surface is rinsed well, put into again activator and activate.
Activator forms: 3vol%HCl
Soak time: 1min.
2, the brilliant nickel coating of direct current electrode position crystallite dimension 0.1-0.5 μ m micron
Plating bath forms: NiSO
47H
2O 250g/L
NiCl
2·6H
2O 40g/L
Boric acid 40g/L
Direct current electrode position preparation method parameter: current density: 4A/dm
2
PH value: 4
Temperature: 50 ℃
Anode: nickel plate;
Time: 60s
Under these conditions, preparing one deck crystallite dimension is 0.1～0.5 μ m, and thickness is the brilliant nickel coating of micron of 0.8 μ m
3, the pulse plating crystallite dimension is the nickel coating of 50～100nm
Plating bath forms: NiSO
47H
2O 280g/L
NiCl
2·6H
2O 40g/L
Boric acid 40g/L
Cumarin 0.1g/L
Formaldehyde 0.25ml/L pulse plating preparation method parameter: average current density: 4A/dm
2
PH value: 4
i
on： 30ms
i
off： 120ms
Temperature: 50 ℃
Anode: nickel plate
Time: 60s
Under these conditions, preparing one deck crystallite dimension is 50～100nm, and thickness is the nano-crystal nickel coating of 0.8 μ m.
4, impulse jet plating crystallite dimension is the nickel coating of 20～50nm
Plating bath forms: NiSO
47H
2O 280g/L
NiCl
2·6H
2O 40g/L
Boric acid 40g/L
ALS 1.2g/L
Butynediols 0.5ml/L
Asccharin 0.8g/L
Impulse jet electroplating preparation method parameter: peak current density: 65A/dm
2
Dutycycle: 20%
Plating bath spray speed: 1400L/h
Temperature: 60 ℃
PH value: 3
Anode: nickel plate
Electroplating time: 10s
Under these conditions, preparing one deck crystallite dimension is 20～50nm, and thickness is the nano-crystal nickel coating of 0.5 μ m.
5, cleaning, drying
The steel band that plating is good is clean with distilled water flushing, then oven dry.
Performance test
Produce in the following manner sample, as a comparative example.
Comparative example preparation method: select the substrate identical with embodiment and plating pre-treating method.Adopt the method for direct current electrode position, equal plating a layer thickness is the brilliant nickel coating of micron of 2.2 μ m on the substrate two sides, and electroplating technology is as follows:
Plating bath comprises: NiSO
47H
2O 280g/L
NiCl
2·6H
2O 40g/L
Boric acid 40g/L
Direct current electrode position technological parameter: current density: 4A/dm
2
PH value: 4
Temperature: 50 ℃
Anode: nickel plate
Electroplating time: 160s
With the obtained material of comparative example at protective atmosphere (25%N
2+ 75%H
2) under do the insulation dehydrogenation, temperature is 200 ℃, temperature retention time 3 hours.At last the gained steel band is annealed and cold-rolling treatment.
The material that embodiment and comparative example are made strikes out battery case, with identical preparation method and prescription assembling LR6 battery, then makes the contrast test of battery performance.Following table 1 is finished product battery performance test comparative analysis report.
Table 1 finished product battery performance test comparative analysis report
Claims (2)
1. the steel band of a plating multi-layer micron/nano-crystal nickel films is characterized in that, take steel band as substrate (1), the two sides of steel band respectively plating multi-layer micron/nano-crystal nickel films; The bottom of multi-layer micron/nano-crystal nickel films (2) is crystallite dimension 0.1 ~ 0.5 μ m, the brilliant nickel coating of micron of thickness 0.5 ~ 2.0 μ m; The intermediate layer of multi-layer micron/nano-crystal nickel films (3) is crystallite dimension 50 ~ 100nm, the nano-crystal nickel coating of thickness 0.5 ~ 1.5 μ m; The top layer of multi-layer micron/nano-crystal nickel films (4) is crystallite dimension 20 ~ 50nm, the nano-crystal nickel coating of thickness 0.2 ~ 1 μ m;
The brilliant nickel coating of micron of described multi-layer micron/nano-crystal nickel films bottom (2) prepares by the mode of direct current electrode position, the nano-crystal nickel coating in multi-layer micron/nano-crystal nickel films intermediate layer (3) prepares by the mode of pulse plating, and the mode that the nano-crystal nickel coating of multi-layer micron/nano-crystal nickel films top layer (4) is electroplated by impulse jet prepares.
2. the preparation method of the steel band of plating multi-layer micron/nano-crystal nickel films claimed in claim 1 is characterized in that, may further comprise the steps and condition:
[1] plating front surface preliminary treatment
Substrate (1) steel band is carried out electrochemical deoiling, activation process
Degreasing fluid forms: NaOH 70g/L;
Na
2CO
3 40g/L；
Na
3PO
4 25g/L；
Na
2SiO
3 10g/L；
Degreasing fluid temperature: 80～90 ℃;
The oil removing time: 3 ~ 5min;
After the oil removing fully, with distilled water specimen surface is rinsed well, then put into activator and activate;
Activator forms: 1 ~ 5vol%HCl;
Soak time: 1 ~ 3min;
[2] the brilliant nickel coating of micron of direct current electrode position crystallite dimension 0.1 ~ 0.5 μ m
Plating bath forms: NiSO
47H
2O 250 ~ 300g/L;
NiCl
2·6H
2O 30~50g/L；
Boric acid 30 ~ 50g/L;
Direct current electrode position preparation method parameter: current density: 3 ~ 6A/dm
2
PH value: 3.5 ~ 4.5;
Temperature: 40 ~ 60 ℃;
Anode: nickel plate;
[3] the pulse plating crystallite dimension is the nano-crystal nickel coating of 50 ~ 100nm
Plating bath forms: NiSO
47H
2O 250 ~ 300g/L;
NiCl
2·6H
2O 30~50g/L；
Boric acid 30 ~ 50g/L;
Cumarin 0.05-0.15g/L;
Formaldehyde 0.2-0.3ml/L;
Pulse plating preparation method parameter: average current density: 3 ~ 6A/dm
2
PH value: 3.5 ~ 4.5;
i
on： 5~50ms；
i
off： 5~250ms；
Temperature: 40 ~ 60 ℃;
Anode: nickel plate;
[4] impulse jet plating crystallite dimension is the nanocrystalline nickel coating of 20 ~ 50nm
Plating bath forms: NiSO
47H
2O 250 ~ 300g/L;
NiCl
2·6H
2O 30~50 g/L；
Boric acid 30 ~ 50g/L;
ALS 0.4 ~ 2g/L;
Butynediols 0.4 ~ 0.5ml/L;
Asccharin 0.8 ~ 1g/L;
Impulse jet electroplating preparation method parameter: peak current density: 47 ~ 82A/dm
2
Dutycycle: 15 ~ 25%;
Plating bath spray speed: 1000 ~ 1500L/h;
Temperature: 55 ~ 65 ℃;
PH value: 2.5 ~ 3.5;
Anode: nickel plate;
[5] it is clean with distilled water flushing to plate good steel band, then oven dry.
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| CN102009504B true CN102009504B (en) | 2013-04-24 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103534389A (en) * | 2011-05-10 | 2014-01-22 | Jx日矿日石金属株式会社 | Ni-plated metal sheet, welded structure, and method for making battery material |
| CN103343367A (en) * | 2013-07-12 | 2013-10-09 | 深圳市中金高能电池材料有限公司 | Nickel-plated steel strip and preparation method thereof |
| CN103847162B (en) * | 2014-02-21 | 2016-01-27 | 苏州米达思精密电子有限公司 | A kind of golden reinforcing chip of surface gold-plating and preparation technology thereof |
| CN105063677A (en) * | 2015-08-21 | 2015-11-18 | 无锡桥阳机械制造有限公司 | Electroplating nickel solution and electroplating method thereof |
| CN106245069A (en) * | 2015-12-01 | 2016-12-21 | 江苏九天光电科技有限公司 | A kind of preparation method of the quick electronickelling steel band for battery case |
| CN105506689B (en) * | 2015-12-22 | 2018-02-16 | 福建金杨科技股份有限公司 | Battery steel shell made from a kind of battery steel shell duplex nickel plating technique and the technique |
| CN105779723B (en) * | 2015-12-27 | 2019-02-15 | 陕西专壹知识产权运营有限公司 | A kind of metal material and preparation method thereof having both intensity and plasticity |
| CN109301094A (en) * | 2017-07-25 | 2019-02-01 | 宁波堇山新材料有限公司 | A kind of plating Ni steel band uses the preparation method of the battery steel shell of the steel band and the steel shell |
| CN110079841B (en) * | 2019-04-17 | 2021-05-11 | 无锡市程晖电源配件有限公司 | Battery steel strip and preparation method thereof |
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| DE3934111A1 (en) * | 1988-10-29 | 1990-05-03 | Usui Kokusai Sangyo Kk | STEEL PRODUCT WITH HEAT-RESISTANT, CORROSION-RESISTANT COATING LAYERS |
| CN1082988A (en) * | 1992-06-22 | 1994-03-02 | 东洋钢钣株式会社 | Erosion-resisting Nickeled Steel Plate or steel bar and method for making thereof |
| CN1722498A (en) * | 2004-07-15 | 2006-01-18 | 常德力元新材料有限责任公司 | Punched nickel-plated steel strip and its manufacturing method |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5259938B2 (en) * | 2006-08-14 | 2013-08-07 | スタンレー電気株式会社 | Metal multilayer structure and method for forming the same |
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|---|---|---|---|---|
| DE3934111A1 (en) * | 1988-10-29 | 1990-05-03 | Usui Kokusai Sangyo Kk | STEEL PRODUCT WITH HEAT-RESISTANT, CORROSION-RESISTANT COATING LAYERS |
| CN1082988A (en) * | 1992-06-22 | 1994-03-02 | 东洋钢钣株式会社 | Erosion-resisting Nickeled Steel Plate or steel bar and method for making thereof |
| CN1722498A (en) * | 2004-07-15 | 2006-01-18 | 常德力元新材料有限责任公司 | Punched nickel-plated steel strip and its manufacturing method |
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