CN105543918A - Method for preparing nickel plating steel strip by utilizing sulfamate pulse electronickelling - Google Patents
Method for preparing nickel plating steel strip by utilizing sulfamate pulse electronickelling Download PDFInfo
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- CN105543918A CN105543918A CN201610042272.7A CN201610042272A CN105543918A CN 105543918 A CN105543918 A CN 105543918A CN 201610042272 A CN201610042272 A CN 201610042272A CN 105543918 A CN105543918 A CN 105543918A
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- pulse
- plating solution
- sulfamate
- steel strip
- nickel
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/18—Electroplating using modulated, pulsed or reversing current
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
- C25D7/06—Wires; Strips; Foils
- C25D7/0614—Strips or foils
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electroplating Methods And Accessories (AREA)
Abstract
The invention discloses a method for preparing a nickel plating steel strip by utilizing sulfamate pulse electronickelling. The method comprises the steps that firstly, a plating solution is prepared according to the proportion that the plating solution per cubic liter comprises 200 g to 400 g of sulfamate, 2 g to 10 g of nickel chloride, 30 g to 40 g of boric acid and 2 g to 10 g of an addition agent, a cleaned steel sheet is electroplated, a power source of electronickelling equipment is a double-pulse plating power supply, and the pulses are periodic reversal type pulses; and according to the electroplating technology condition, the average current density ranges from 5 A/dm<2> to 15 A/dm<2>, the pulse current duty ratio ranges from 5% to 40%, the plating solution temperature keeps to be about 50 DEG C to 60 DEG C, and after being subject to electro-deposition for 10 minutes to 30 minutes, the steel sheet is taken out and then is washed and dried. The method is simple in process and convenient to operate; the concentration polarization phenomenon is few, and the large limit current can be borne; the electro-deposition speed is high, and the production period is short; the porosity is low, and the corrosion-resisting performance is good; and the nickel plating steel strip is high in hardness, low in internal stress and good in ductility.
Description
Technical field
The present invention relates to field of metal surface treatment, particularly a kind of nickel plating technology of steel band.
Background technology
Electronickelling technology is applied to protection to metal and decoration usually, and be widely used in the industries such as the anticorrosion of the products such as various ferrous materials, industrial machine, automobile and household implements and decoration, wherein the nickel plating of steel band is comparatively common industrial application.
Nickel plating technology uses watt system as nickel-plating liquid usually, and the usual current density range of the plating solution of watt system is less, is only 0.5 ~ 5A/dm
2, and plated item has internal stress comparatively large, the defects such as porosity is higher, and dispersive ability is poor, and current efficiency is low.When electric current rises to 8A/dm
2time, plating solution concentration polarization is serious, causes hydrogen evolution phenomenon aggravation in electroplating process, and then makes coating produce the defects such as pin hole, burr, pit, coarse-grain; When electric current exceeds 10A/dm
2time, coating have burn phenomenon occur.
In the electroplating technology of routine, usually use direct supply as the device power supply (DPS) of plating.Current density in electroplating technology is the important factor affecting the performances such as coating hardness, internal stress, porosity, erosion resistance and bonding force, but the limiting current of direct supply is less.At current density 0.5-5A/dm
2time in scope, increase current density, cathode overpotential increases, and the critical forming radius of nucleus is diminished, and the synthesis speed of crystal is greater than growth rate, causes crystal size gets smaller, and coating surface roughness reduces; When current density exceeds 5A/dm
2time, electroplating process is mainly by the diffusion control of mass transfer in liquid phase, the mass transfer of nickel ion is the major influence factors in electroplating process, cathode interface nickel deposition speed, nickel ion wear rate is very fast, the growth rate of crystal is greater than synthesis speed, and cause crystalline size to become large, coating surface roughness increases; Current density continues to increase, and concentration polarization phenomenon is aggravated further, and cathode surface evolving hydrogen reaction aggravates, the bubble hydrogen that coating is inner and remained on surface is a large amount of, and make coating internal stress become large, hardness reduces, and porosity increases, and corrosion resistance nature reduces.Because the limiting current of direct current plating method is lower, if current density is excessive, just there will be the defects such as porosity is higher, corrosion resistance nature is poor.
For solving the problem, have employed pulse plating process, although the porosity of coating can be reduced, elimination of hydrogen embrittlement, reduce the internal stress of coating, but the restriction of capacity effect cannot be selected by the logical section time when using pulse plating, this brings trouble with regard to giving workpiece in the control of electroplating process, and in use pulse plating time maximum average deposition speed can not exceed limit deposit speed under same fluid dynamic conditions, so current pulse plating still also exists a no small difficult problem.
Summary of the invention
The object of the present invention is to provide that a kind of technique is simple, electrodepositing speed is fast, comparatively light, that porosity the is low sulfamate Pulse-Electroplated Nickel that utilizes of concentration polarization phenomenon prepares the method for nickel plated steel strip.The present invention mainly passes through pulse plating process with the sulfamate bath of preparation, carries out galvanic deposit to steel band, obtains the nickel plated steel strip that physical and chemical performance is excellent.
Preparation method of the present invention is as follows:
(1) preparation of plating solution: every liter plating solution is containing nickel sulfamic acid 200 ~ 400g, nickelous chloride 2 ~ 10g, boric acid 30 ~ 40g, and additive 2 ~ 10g, the solvent that plating solution uses is pure deionized water.With hydrochloric acid, plating solution pH value is adjusted to 4 ~ 7, plating solution is warming up to 50 DEG C ~ 60 DEG C.
Described additive is a kind of or mixture of at least two kinds of propiolic alcohol propoxy-ether, propiolic alcohol oxyethyl group ether, propane sulfonic acid pyridinium salt, the interpolation mass ratio of its two kinds of mixtures is 1:1, preferably add the mixture of propiolic alcohol propoxy-ether, propiolic alcohol oxyethyl group ether, propane sulfonic acid pyridinium salt three, its mass ratio added is 1:1:1.
(2) pre-treatment of steel band: wash steel disc with deionized water, acetone oil removing, alkali cleaning oil removing, hydrochloric acid activation, uses washed with de-ionized water.
(3) electroplating technology flow process: the power supply of electronickelling equipment is Double-pulse Plating Power Source, pulse pattern is the pulse of periodic reverse type; Electroplating technical conditions is average current density 5 ~ 15A/dm
2, pulsed current dutycycle is 5% ~ 40%.Keep bath temperature 50 ~ 60 DEG C, take out after galvanic deposit 10-30 minute, then wash, dry.
The present invention compared with prior art tool has the following advantages:
(1) technique is simple, convenient operation;
(2) concentration polarization phenomenon is comparatively light, can bear larger limiting current;
(3) electrodepositing speed is fast, with short production cycle;
(4) porosity is low, fine corrosion resistance;
(5) hardness of nickel plated steel strip is high, internal stress is low, has good ductility.
Embodiment:
Embodiment 1
Be that propiolic alcohol propoxy-ether, propiolic alcohol oxyethyl group ether, propane sulfonic acid pyridinium salt three are by 1:1:1 2g mixed preparing plating solution altogether by every liter containing nickel sulfamic acid 200g, nickelous chloride 2g, boric acid 30g, additive, the solvent that wherein plating solution uses is pure deionized water, with hydrochloric acid, plating solution pH value is adjusted to 4, plating solution is warming up to 50 DEG C.
With deionized water, steel disc is washed, acetone oil removing, alkali cleaning oil removing, hydrochloric acid activation, then use washed with de-ionized water.
Electroplate steel disc, the power supply of electronickelling equipment is Double-pulse Plating Power Source, and pulse pattern is the pulse of periodic reverse type; Electroplating technical conditions is average current density 5A/dm
2, pulsed current dutycycle is 5%, and keep bath temperature 50 DEG C, galvanic deposit was taken out after 10 minutes, then washed, dried.
This Nickeled Steel Plate smooth surface, plated layer compact, internal stress is 0.035Mpa, and hardness is 400HV, and mean roughness is that the continuous salt-fog test of 0.354mm, 16h can reach 8 grade standards.
Embodiment 2
Be that propiolic alcohol propoxy-ether, propiolic alcohol oxyethyl group ether, propane sulfonic acid pyridinium salt three are by 1:1:1 10g mixed preparing plating solution altogether by every liter containing nickel sulfamic acid 400g, nickelous chloride 10g, boric acid 40g, additive, the solvent that plating solution uses is pure deionized water, with hydrochloric acid, plating solution pH value is adjusted to 7, plating solution is warming up to 60 DEG C.
With deionized water, steel disc is washed, acetone oil removing, alkali cleaning oil removing, hydrochloric acid activation, then use washed with de-ionized water.
Electroplate steel disc, the power supply of electronickelling equipment is Double-pulse Plating Power Source, and pulse pattern is the pulse of periodic reverse type; Electroplating technical conditions is average current density 15A/dm
2, pulsed current dutycycle is 40%.Keep bath temperature about 60 DEG C, galvanic deposit was taken out after 30 minutes, then washed, dried.
This Nickeled Steel Plate smooth surface is smooth, and coating is finer and close, and internal stress is 0.031Mpa, and hardness is 454HV, and mean roughness is that the continuous salt-fog test of 0.329mm, 16h can reach 8 grade standards.
Embodiment 3
Be that propiolic alcohol propoxy-ether, propiolic alcohol oxyethyl group ether, propane sulfonic acid pyridinium salt three are by 1:1:1 8g mixed preparing plating solution altogether by every liter containing nickel sulfamic acid 350g, nickelous chloride 7g, boric acid 40, additive, the solvent that plating solution uses is pure deionized water, with hydrochloric acid, plating solution pH value is adjusted to 4.5, plating solution is warming up to 60 DEG C.
With deionized water, steel disc is washed, acetone oil removing, alkali cleaning oil removing, hydrochloric acid activation, then use washed with de-ionized water.
Electroplate steel disc, the power supply of electronickelling equipment is Double-pulse Plating Power Source, and pulse pattern is the pulse of periodic reverse type; Electroplating technical conditions is average current density 10A/dm
2, pulsed current dutycycle is 6%.Keep bath temperature about 60 DEG C, galvanic deposit was taken out after 10 minutes, then washed, dried.
This Nickeled Steel Plate smooth surface is smooth, and coating is finer and close, and internal stress is 0.024Mpa, and hardness is 473HV, and mean roughness is that the continuous salt-fog test of 0.296mm, 16h can reach 9 grade standards.
Embodiment 4
Prepare plating solution by every liter containing nickel sulfamic acid 350g, nickelous chloride 7g, boric acid 40g, propiolic alcohol propoxy-ether 5g, the solvent that plating solution uses is pure deionized water, with hydrochloric acid, plating solution pH value is adjusted to 4.5, and being heated up by plating solution is 55 DEG C.
With deionized water, steel disc is washed, acetone oil removing, alkali cleaning oil removing, hydrochloric acid activation, then use washed with de-ionized water.
Electroplate steel disc, the power supply of electronickelling equipment is Double-pulse Plating Power Source, and pulse pattern is the pulse of periodic reverse type; Electroplating technical conditions is average current density 13A/dm
2, pulsed current dutycycle is 30%.Keep bath temperature about 55 DEG C, galvanic deposit was taken out after 25 minutes, then washed, dried.
This Nickeled Steel Plate smooth surface is smooth, and coating is finer and close, and internal stress is 0.026Mpa, and hardness is 462HV, and mean roughness is that the continuous salt-fog test of 0.304mm, 16h can reach 8 grade standards.
Embodiment illustrates the nickel plated steel strip that present invention process obtains, and smooth surface is smooth, and coating is finer and close, and internal stress is low, and hardness is high, and surfaceness is little, fine corrosion resistance.
Embodiment 5
Prepare plating solution by every liter containing nickel sulfamic acid 400g, nickelous chloride 8g, boric acid 38g, propiolic alcohol oxyethyl group ether 7g, the solvent that plating solution uses is pure deionized water, with hydrochloric acid, plating solution pH value is adjusted to 4.5, plating solution is warming up to 55 DEG C.
With deionized water, steel disc is washed, acetone oil removing, alkali cleaning oil removing, hydrochloric acid activation, then use washed with de-ionized water.
Electroplate steel disc, the power supply of electronickelling equipment is Double-pulse Plating Power Source, and pulse pattern is the pulse of periodic reverse type; Electroplating technical conditions is average current density 14A/dm
2, pulsed current dutycycle is 30%.Keep bath temperature about 55 DEG C, galvanic deposit was taken out after 18 minutes, then washed, dried.
This Nickeled Steel Plate smooth surface is smooth, and coating is finer and close, and internal stress is 0.028Mpa, and hardness is 450HV, and mean roughness is that the continuous salt-fog test of 0.314mm, 16h can reach 8 grade standards.
Embodiment 6
Prepare plating solution by every liter containing nickel sulfamic acid 380g, nickelous chloride 8g, boric acid 40g, propane sulfonic acid pyridinium salt 8g, the solvent that plating solution uses is pure deionized water, with hydrochloric acid, plating solution pH value is adjusted to 5.5, plating solution is warming up to 60 DEG C.
With deionized water, steel disc is washed, acetone oil removing, alkali cleaning oil removing, hydrochloric acid activation, then use washed with de-ionized water.
Electroplate steel disc, the power supply of electronickelling equipment is Double-pulse Plating Power Source, and pulse pattern is the pulse of periodic reverse type; Electroplating technical conditions is average current density 14A/dm
2, pulsed current dutycycle is 30%.Keep bath temperature about 60 DEG C, galvanic deposit was taken out after 20 minutes, then washed, dried.
This Nickeled Steel Plate smooth surface is smooth, and coating is finer and close, and internal stress is 0.025Mpa, and hardness is 410HV, and mean roughness is that the continuous salt-fog test of 0.300mm, 16h can reach 8 grade standards.
Embodiment 7
Be total to 10g in the ratio mixing of 1:1 in every liter prepare plating solution containing nickel sulfamic acid 400g, nickelous chloride 9g, boric acid 40g, additive propiolic alcohol propoxy-ether, propiolic alcohol oxyethyl group ether, the solvent that plating solution uses is pure deionized water, with hydrochloric acid, plating solution pH value is adjusted to 4, plating solution is warming up to 55 DEG C.
With deionized water, steel disc is washed, acetone oil removing, alkali cleaning oil removing, hydrochloric acid activation, then use washed with de-ionized water.
Electroplate steel disc, the power supply of electronickelling equipment is Double-pulse Plating Power Source, and pulse pattern is the pulse of periodic reverse type; Electroplating technical conditions is average current density 10A/dm
2, pulsed current dutycycle is 30%.Keep bath temperature about 55 DEG C, galvanic deposit was taken out after 10 minutes, then washed, dried.
This Nickeled Steel Plate smooth surface is smooth, and coating is finer and close, and internal stress is 0.027Mpa, and hardness is 398HV, and mean roughness is that the continuous salt-fog test of 0.297mm, 16h can reach 8 grade standards.
Embodiment 8
Be total to 10g in the ratio mixing of 1:1 in every liter prepare plating solution containing nickel sulfamic acid 200g, nickelous chloride 10g, boric acid 32g, additive propiolic alcohol oxyethyl group ether, propane sulfonic acid pyridinium salt, the solvent that plating solution uses is pure deionized water, with hydrochloric acid, plating solution pH value is adjusted to 6, plating solution is warming up to 60 DEG C.
With deionized water, steel disc is washed, acetone oil removing, alkali cleaning oil removing, hydrochloric acid activation, then use washed with de-ionized water.
Electroplate steel disc, the power supply of electronickelling equipment is Double-pulse Plating Power Source, and pulse pattern is the pulse of periodic reverse type; Electroplating technical conditions is average current density 15A/dm
2, pulsed current dutycycle is 30%.Keep bath temperature about 60 DEG C, galvanic deposit was taken out after 10 minutes, then washed, dried.
This Nickeled Steel Plate smooth surface is smooth, and coating is finer and close, and internal stress is 0.029Mpa, and hardness is 394HV, and mean roughness is that the continuous salt-fog test of 0.295mm, 16h can reach 8 grade standards.
Embodiment illustrates the nickel plated steel strip that present invention process obtains, and smooth surface is smooth, and coating is finer and close, and internal stress is low, and hardness is high, and surfaceness is little, fine corrosion resistance.
Claims (4)
1. utilize sulfamate Pulse-Electroplated Nickel to prepare a method for nickel plated steel strip, it is characterized in that: it comprises the following steps:
(1) preparation of plating solution: every liter plating solution contains nickel sulfamic acid 200 ~ 400g, nickelous chloride 2 ~ 10g, boric acid 30 ~ 40g, additive 2 ~ 10g, and the solvent that plating solution uses is pure deionized water, with hydrochloric acid, plating solution pH value is adjusted to 4 ~ 5;
(2) pre-treatment of steel band: steel disc is washed with deionized water, acetone oil removing, alkali cleaning oil removing, hydrochloric acid activation, by washed with de-ionized water;
(3) electroplating technology flow process: electroplating technical conditions is average current density 5 ~ 15A/dm
2, pulsed current dutycycle is 5% ~ 40%, keeps bath temperature 50 DEG C ~ 60 DEG C, takes out, then wash, dry after galvanic deposit 10-30 minute.
2. sulfamate Pulse-Electroplated Nickel according to claim 1 prepares the method for nickel plated steel strip, it is characterized in that: described additive is a kind of or mixture of at least two kinds of propiolic alcohol propoxy-ether, propiolic alcohol oxyethyl group ether, propane sulfonic acid pyridinium salt, and the mass ratio adding two or more mixture is equal.
3. sulfamate Pulse-Electroplated Nickel according to claim 1 prepares the method for nickel plated steel strip, it is characterized in that: described additive is the mixture of propiolic alcohol propoxy-ether, propiolic alcohol oxyethyl group ether, propane sulfonic acid pyridinium salt three, its part by weight added is 1:1:1.
4. sulfamate Pulse-Electroplated Nickel according to claim 1 prepares the method for nickel plated steel strip, it is characterized in that: the power supply of the electronickelling equipment used is Double-pulse Plating Power Source, and pulse pattern is the pulse of periodic reverse type.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610042272.7A CN105543918A (en) | 2016-01-21 | 2016-01-21 | Method for preparing nickel plating steel strip by utilizing sulfamate pulse electronickelling |
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| CN201610042272.7A CN105543918A (en) | 2016-01-21 | 2016-01-21 | Method for preparing nickel plating steel strip by utilizing sulfamate pulse electronickelling |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107022775A (en) * | 2017-04-20 | 2017-08-08 | 南通惠能镀镍钢带有限公司 | A kind of preparation method of nickel plated steel strip |
| CN112813469A (en) * | 2020-12-30 | 2021-05-18 | 遵义智通金属表面技术处理有限公司 | Nanocrystalline deposition method for copper alloy and steel matrix |
| CN113046815A (en) * | 2021-02-01 | 2021-06-29 | 许昌学院 | Preparation method of double-pulse electroplated nickel-graphene composite coating of continuous casting crystallizer |
| CN113151869A (en) * | 2021-04-13 | 2021-07-23 | 苏州磊屹光电科技有限公司 | Nickel pretreatment method for improving appearance of stainless steel/foreign copper material nickel layer |
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| US6402922B1 (en) * | 1999-03-17 | 2002-06-11 | Sony Dadc Austria Ag | Pulse plating |
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2016
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| CN101215708A (en) * | 2008-01-08 | 2008-07-09 | 厦门大学 | Method for preparing corrosion resistant nickel/chromium plating steel belt |
| CN102534695A (en) * | 2010-12-29 | 2012-07-04 | 京东方科技集团股份有限公司 | Metal substrate for flexible display and preparation method for metal substrate |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107022775A (en) * | 2017-04-20 | 2017-08-08 | 南通惠能镀镍钢带有限公司 | A kind of preparation method of nickel plated steel strip |
| CN112813469A (en) * | 2020-12-30 | 2021-05-18 | 遵义智通金属表面技术处理有限公司 | Nanocrystalline deposition method for copper alloy and steel matrix |
| CN113046815A (en) * | 2021-02-01 | 2021-06-29 | 许昌学院 | Preparation method of double-pulse electroplated nickel-graphene composite coating of continuous casting crystallizer |
| CN113151869A (en) * | 2021-04-13 | 2021-07-23 | 苏州磊屹光电科技有限公司 | Nickel pretreatment method for improving appearance of stainless steel/foreign copper material nickel layer |
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