CN103614750A - Preparation process for copper-plate electroplated nickel tungsten electroplated layer of continuous-casting crystallizer - Google Patents
Preparation process for copper-plate electroplated nickel tungsten electroplated layer of continuous-casting crystallizer Download PDFInfo
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Abstract
The invention discloses a preparation process for a copper-plate electroplated nickel tungsten electroplated layer of a continuous-casting crystallizer. The electroplated layer contains tungsten with mass percentage being more than or equal to 44 percent, and the thickness of the electroplated layer is 0.2mm to 1.8mm. The electroplated liquid for the preparation process consists of the following ingredients: 50g/L to 75g/L nickel aminosulfonate, 60g/L to 90g/L sodium tungstate, 55g/L to 120g/L sodium citrate, 1g/L to 4.7g/L saccharin sodium, 0.5g/L to 3g/L sodium allysulfonate and 0.2g/L to 1g/L lauryl sodium sulfate, the current density is 0.5A/dm<2> to 10A/dm<2>, the pH value is 6.5 to 8.0 at the temperature of 55 to 75 DEG C, and the electroplated layer is thermally preserved for 2.5h to 3h in a vacuum heat treatment furnace after the electroplating under the temperature of 350 to 370 DEG C. The electroplated layer is good in heat cracking resistance, oxidation resistance and corrosion resistance and high in heat fatigue resistance, the micro-hardness of the electroplated layer under the plating state can reach over 670HV and can reach about 1230HV after the heat treatment, the abrasion resistance is remarkably improved, and the electroplated layer can be widely applied to the continuous casting of a high-speed continuous-casting machine.
Description
Technical field
The invention belongs to continuous casting crystallizer copper plate technical field of surface, be specifically related to a kind of preparation technology of continuous casting crystallizer copper plate nickel tungsten electroplating coating.
Background technology
Continuous cast mold is the nucleus equipment that whole continuous casting is produced, and the quality of its quality directly affects the quality of strand and the operating rate of continuous caster.And crystallizer performance is towards high pulling rate, high mechanical strength, thermal conductive resin, high rigidity, high-wearing feature and corrosion proof future development, crystallizer surface must be treated.
In existing many crystallizer surface treatment technologies, technical maturity, facility investment is few, productive expense is low, raw material availability is high is still electroplating technology, wherein, electroplate monometallic coating, as the pure Ni coating of routine, though good with basal body binding force, coating hardness is low, not wear-resisting, affect work-ing life of crystallizer.In electroplating binary alloy, Ni-Fe alloy layer wear resistance is good, but fragility is larger, and internal stress is larger, is prone to high temperature thermal crack; Ni-Co coating long service life, but Co content is high, cost is expensive, and alloy fragility is larger, alternating thermal stress resisting poor performance, erosion resistance is bad, applies limitedly, and production process is various.Other,, as electroplated the technology such as ternary alloy and composite deposite, although excellent performance all rests on conceptual phase mostly, cannot carry out large-scale production and application.So, still need to develop new base binary alloy plating, make up the deficiency of existing base binary alloy plating, compare with the technology such as ternary alloy and composite deposite, in large-scale production application, have more feasibility.
Nickel tungsten alloy electroplating layer compact structure, thermotolerance are high, can match in excellence or beauty with pottery, graphite-phase, at high temperature anti-oxidant; corrosion resistance and good, has higher hardness, and due to the existence of tungsten; make to form the stable transfer layer shielding of one deck between itself and mating plate, there is excellent wear resistance.Increase along with W content in coating, W atom enters Ni lattice, cause lattice swell, there is pincushion distortion, when W content reaches 44% when above, the regularly arranged of nickel-tungsten alloy plating atom is damaged, and X diffractogram spike disappears, become smooth broadening peak, now coating structure changes non-crystalline state into by crystalline state.W content is that more than 44% amorphous alloy coating is compared with crystal alloy, and corrosion speed obviously reduces, excellent anti-corrosion performance.Nickel tungsten alloy electroplating liquid is divided into sulfamate type and sulfate type by nickel salt kind, and electroplate liquid contains nickel salt, tungstate, also contains various different additive and complexing agent as citric acid, tartrate, asccharin etc.
Present stage, nickel-tungsten alloy plating was mainly used in mould and oil engine part workpiece, for the data of continuous casting crystallizer copper plate, substantially do not have, the ubiquitous weak point of nickel tungsten technique of preparing of mould aspect is that coating is coarse, irregular or contain the defects such as pit.How the alloy of die industry will be mainly used in originally, can mass-producing be applied to continuous cast mold field, realize the span in two onrelevant fields, and how to control electroplating technical conditions and solution composition, from numerous solution additives, select suitable additive, maximize the performance that reduces plating solution impurity and improve nickel tungsten, make up the existing ubiquitous weak point of nickel tungsten technique of preparing, obtain the continuous cast mold base binary alloy plating that over-all properties is more more excellent than prior art, obtain economic benefit and realize mass-producing application, it is all problem demanding prompt solution.
Summary of the invention
The object of the invention is in order to make up above-mentioned deficiency, a kind of preparation technology of continuous casting crystallizer copper plate nickel tungsten electroplating coating is provided, the coating microhardness that utilizes this technique to prepare is high, heat crack resistance is good, anti-oxidant, corrosion resistance and good, heat-resistant anti-fatigue drag is high, can in high-speed continuous casting machine continuous casting, be widely used.
A preparation technology for continuous casting crystallizer copper plate nickel tungsten electroplating coating, described nickel tungsten plating contains the tungsten that is more than or equal to quality of coating 44%, and thickness of coating is 0.2～1.8mm;
Described preparation technology's processing step is: electrochemical deoiling, sandblast, electrolytic degreasing, clear water clean, fixedly auxiliary mould, acid activation processing, plating, vacuum heat treatment;
The electroplate liquid of described plating consists of:
Nickel sulfamic acid 50～75 g/L,
Sodium wolframate 60～90 g/L,
Trisodium Citrate 55～120g/L,
Soluble saccharin 1～4.7g/L,
Sodium allyl sulfonate 0.5～3g/L,
Sodium lauryl sulphate 0.2～1g/L;
Described electroplating technique parameter is:
D
k 0.5～10 A/dm
2
pH 6.5～8.0
T 55～75℃
Agitation condition pressurized air stirs and recycle pump stirs
The interpolation of described sodium wolframate, adopts electromagnetic dosing pump by the specified amount continuous adding of every kiloampere electric current;
The interpolation of described soluble saccharin, sodium allyl sulfonate, adopts electromagnetic dosing pump by the specified amount continuous adding of every kiloampere electric current, after regularly detecting, supplements and adds again;
The interpolation of described sodium lauryl sulphate, adopts and first before plating, detects after the surface tension of electroplate liquid, and the result disposable sodium lauryl sulphate of adding before plating detecting according to surface tension, makes the surface tension of electroplate liquid be controlled at 27～34mN/m.
Described vacuum heat treatment is in vacuum tightness≤10
-2in the vacuum heat treatment furnace of Pa, carry out, coating is incubated at 350～370 ℃ to 2.5～3 h, then cools with argon gas or nitrogen.
The sulfamate bath system that the present invention selects,, hardness less than sulfate bath system gained coating internal stress and current efficiency are higher, and sulfamate solubleness in water is large, and deposition rate of metal are is fast, is easy to high current density operation; Adopt Citrate trianion and nickel complexing, make current potential become negative, close with the sedimentation potential of tungsten, thus impelling co-precipitation, Trisodium Citrate can improve solution dispersibility and current efficiency, significantly improves coating microhardness; In the situation that there is no Trisodium Citrate, the existence of sodium wolframate can make current efficiency decline, and when concentration of sodium tungstate is 60～90g/L, adds Trisodium Citrate 55～120g/L can effectively improve current efficiency.
Electroplate one of reason of the defects such as easily generation is coarse, uneven, pit, main relevant with the foreign matter content in plating solution, and additive types and add-on are too much, can produce or bring into impurity, these impurity can deposit or be mixed on crystal boundary together with coated metal, impurity metal lattice is around distorted, increases internal stress.The present invention is after composite test, analysis and research, and additive adopts the soluble saccharin of 1～4.7g/L, the sodium lauryl sulphate of the sodium allyl sulfonate of 0.5～3g/L, 0.2～1g/L, to obtain higher luminance brightness and to reduce as far as possible internal stress.Soluble saccharin has destressing, by quantity not sufficient, can make coating poor flatness, crosses and causes at most coating fragility large, when concentration is controlled at 1～4.7g/L, can effectively improve the bonding force of coating and matrix; Sodium lauryl sulphate is as brightening agent and wetting agent, and concentration is controlled at 0.2～1g/L, can effectively reduce the surface tension between plating solution and plating piece, makes hydrogen be difficult to be attached to cathode surface, reduces the probability that pin hole appears in coating; Sodium allyl sulfonate, as auxiliary brightener, can be assisted soluble saccharin and sodium lauryl sulphate, makes coating obtain good bright property.After three kinds of additive combinations, can effectively improve current efficiency, impel grain refining, align, accelerate bright dipping and leveling speed, effectively reduce internal stress, and reduce pin hole.
PH value and the excess Temperature of electroplate liquid, citrate ions easily decomposes, cause plating solution unstable, the ability of complexing tungsten a little less than, the too low nickel salt of acidity is hydrolyzed, the too low coating blackout of temperature, when pH6.5～8.0, temperature is controlled at 55～75 ℃, can effectively improve the diffusive migration speed of metal ion and electrodeposit metals in the current efficiency of negative electrode, and increase current density, contribute to current potential to bear the increase of deposition rate of metal are, the cathodic polarization of tungsten strengthens, can refinement coating structure, but current density is excessive, having hydrogen separates out from cathode surface, coating is thin and coarse, in this electroplate liquid, cathode current density D
kat 0.5～10 A/dm
2time, thickness of coating is even, compact structure.
Electroplate one of reason that defect causes and be that copper coin is processed is unreasonable or insufficient, during sandblast, adhere to sand grains or chiltern bad or impure etc., so this process using electrochemical deoiling, sandblast, electrolytic degreasing, clear water clean, acid activation is processed, and fully process matrix.In addition, after plating completes, adopt vacuum heat treatment, coating is in vacuum tightness≤10
-2at Pa, 350～370 ℃, be incubated 2.5～3h, degas, promote the effects such as diffusion, eliminate the unrelieved stress producing in electrodeposition process, improve the density of coating, promote the combination of coating and matrix, reach maximum precipitation hardening effect.
The present invention be take sulfamate bath system as basis, adopt 60～90g/L sodium wolframate and 55～120g/L Trisodium Citrate proportioning, add the soluble saccharin of 1～4.7g/L, the sodium lauryl sulphate of the sodium allyl sulfonate of 0.5～3g/L, 0.2～1g/L, the stable performance of electroplate liquid system, safeguard simple and conveniently, long processing period, effectively overcomes plating defect, improve quality of coating, add reasonable control PH, T and D
kgained continuous casting crystallizer copper plate nickel tungsten plating, anti-oxidant, corrosion resistance and good, heat-resistant anti-fatigue drag is high, more than under its plated state, microhardness can reach 670HV, after thermal treatment, hardness can reach 1230HV left and right, significantly improved the wear resistance of coating, after electroplating, internal stress is 185～196MPa, and thermal treatment internal stress is reduced to 129～131MPa, and heat crack resistance is good, guaranteed that coating is not easy to crack, extended the work-ing life of continuous casting crystallizer copper plate, improved the operating rate of continuous-casting steel-making, can in high-speed continuous casting machine continuous casting, be widely used.
Embodiment
Embodiment
Below will from five groups test the present invention will be further described.
In five groups of tests, each continuous casting crystallizer copper plate nickel tungsten electroplating Coating composition and thickness are as shown in the table
The preparation technology of above-mentioned continuous casting crystallizer copper plate nickel tungsten alloy electroplating layer, comprise the following steps: electrochemical deoiling, sandblast, electrolytic degreasing, clear water clean, fixedly auxiliary mould, acid activation are processed, electroplated, then carry out vacuum heat treatment and eliminate electrolytic coating internal stress, described vacuum heat treatment is in vacuum tightness≤10
-2in the vacuum heat treatment furnace of Pa, carry out, coating is incubated at 350～370 ℃ to 2.5～3 h, then cools with argon gas or nitrogen;
Described preparation technology's electroplate liquid consists of:
| Component (g/L) | 1 | 2 | 3 | 4 | 5 |
| Nickel sulfamic acid | 50 | 56 | 62 | 69 | 75 |
| Sodium wolframate | 60 | 67 | 74 | 82 | 90 |
| Trisodium Citrate | 50 | 67 | 85 | 102 | 120 |
| Soluble saccharin | 1.0 | 1.9 | 2.8 | 3.7 | 4.7 |
| Sodium allyl sulfonate | 0. 5 | 1.1 | 1.7 | 2.3 | 3.0 |
| Sodium lauryl sulphate | 0.2 | 0.4 | 0.6 | 0.8 | 1.0 |
Described preparation technology's processing parameter is:
| Group time | 1 | 2 | 3 | 4 | 5 |
| PH | 6.5～6.7 | 6.8～7.0 | 7.1～7.3 | 7.4～7.6 | 7.8～8.0 |
| Current density (A/dm 2） | 0.5 | 4.0 | 6.0 | 9.0 | 10.0 |
| Temperature (℃) | 55～59 | 59～63 | 63～67 | 67～71 | 71～75 |
Test-results:
1. microhardness and internal stress: detect respectively microhardness and the internal stress of coating after electroplating and after thermal treatment, as shown in the table by statistics;
As seen from the above table, after electroplating, the plated state microhardness of coating is 670～689HV, internal stress is 185～196MPa, wear resistance and heat crack resistance are good, after thermal treatment, the microhardness of coating is 1225～1236HV, internal stress is 129～131MPa, has obviously further improved coating hardness, and has reduced to a certain extent the internal stress of coating.
2. oxidation-resistance: nickel tungsten plating is in 700 ℃, 800 ℃ and 900 ℃ of High Temperature Furnaces Heating Apparatuss respectively after continuous calcination 1h, and coating has higher oxidation-resistance without decortication, de-slag and weightening finish phenomenon, explanation nickel tungsten plating.
3. erosion resistance: nickel tungsten alloy electroplating layer is put into 30 ℃, the HNO of 1mol/L
3in corrosive medium, soak 100h, erosion rate is 0.019～0.026mm/a, lower than 0.04～0.10mm/a of similar coating, and this electrolytic coating presents good erosion resistance.
4. heat-resistant anti-fatigue drag: after plating, through 15s, from room temperature, be heated to 800 ℃, insulation l0s, water-cooled is below 10s to 100 ℃, and 15s reheats 800 ℃, and so cold cycling is 250 weeks, and sample is not all found any crackle, illustrates that the thermal fatigue resistance of this coating is high.
Production practice:
3 the high pulling rate casting machine of medium thin slab crystallizers of certain steel mill, ladleful 150t, size of plate blank is 900mm * 135mm, continuous caster radius is 5m, metallurgical length 24.2m, and design pulling rate is 1.8～2.6m/min, copper coin surface temperature is 160～180 ℃, and crystallizer heat flow density is 1.95～2.25Mw/m
2, this high pulling rate casting machine crystallizer mean lifetime is 270 stoves.
This copper plate of crystallizer is used after the ceramic coating of the technical program design, and copper plate temperature is 110～120 ℃, and crystallizer heat flow density is 1.15～1.20Mw/m
2effectively weakened because heat flow density is high, the heat distortion amount of the high copper coin causing of steel plate working temperature and coating is large, slowed down that coating be full of cracks, coating come off, the generation of copper coin defects i.e.cracks, this high pulling rate casting machine crystallizer mean lifetime is extended for 400 stoves, has increased substantially the life-span of continuous casting of middle-thin slabs crystallizer.
Claims (2)
1. a preparation technology for continuous casting crystallizer copper plate nickel tungsten electroplating coating, is characterized in that: described nickel tungsten plating contains the tungsten that is more than or equal to quality of coating 44%, and thickness of coating is 0.2～1.8mm;
Described preparation technology's processing step is: electrochemical deoiling, sandblast, electrolytic degreasing, clear water clean, fixedly auxiliary mould, acid activation processing, plating, vacuum heat treatment;
The electroplate liquid of described plating consists of:
Nickel sulfamic acid 50～75 g/L,
Sodium wolframate 60～90 g/L,
Trisodium Citrate 55～120g/L,
Soluble saccharin 1～4.7g/L,
Sodium allyl sulfonate 0.5～3g/L,
Sodium lauryl sulphate 0.2～1g/L;
Described electroplating technique parameter is:
D
k 0.5～10 A/dm
2
pH 6.5～8.0
T 55～75℃
Agitation condition pressurized air stirs and recycle pump stirs
The interpolation of described sodium wolframate, adopts electromagnetic dosing pump by the specified amount continuous adding of every kiloampere electric current;
The interpolation of described soluble saccharin, sodium allyl sulfonate, adopts electromagnetic dosing pump by the specified amount continuous adding of every kiloampere electric current, after regularly detecting, supplements and adds again;
The interpolation of described sodium lauryl sulphate, adopts and first before plating, detects after the surface tension of electroplate liquid, and the result disposable sodium lauryl sulphate of adding before plating detecting according to surface tension, makes the surface tension of electroplate liquid be controlled at 27～34mN/m.
2. the preparation technology of a kind of continuous casting crystallizer copper plate nickel tungsten electroplating coating as claimed in claim 1, is characterized in that: described vacuum heat treatment is in vacuum tightness≤10
-2in the vacuum heat treatment furnace of Pa, carry out, coating is incubated at 350～370 ℃ to 2.5～3 h, then cools with argon gas or nitrogen.
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| CN103911637A (en) * | 2014-03-28 | 2014-07-09 | 马鞍山马钢表面工程技术有限公司 | Ni-Co-W alloy electroplating solution for working surface of copper plate of continuous casting crystallizer and preparation method of Ni-Co-W alloy electroplating solution |
| CN104028716A (en) * | 2014-06-19 | 2014-09-10 | 马鞍山马钢表面工程技术有限公司 | Method for using Ni-Co-W alloy electroplate liquid to repair nickel-plated combined crystallizer narrow plate in electroplating manner |
| CN104762644A (en) * | 2015-04-24 | 2015-07-08 | 西峡龙成特种材料有限公司 | Electroplated amorphous-state nickel-tungsten-phosphorous alloy for copper plate of crystallizer for continuous casting and preparation process of amorphous-state nickel-tungsten-phosphorous alloy |
| CN104846409A (en) * | 2015-04-30 | 2015-08-19 | 云南民族大学 | High-tungsten-content flawless tungsten-nickel alloy coating layer and electroplating liquid and electroplating process |
| CN106048680A (en) * | 2016-07-22 | 2016-10-26 | 东莞普瑞得五金塑胶制品有限公司 | Special galvanical corrosion-resistant coating for fast charging interface of mobile phone |
| CN107958946A (en) * | 2017-11-17 | 2018-04-24 | 扬州乾照光电有限公司 | A kind of light-emitting diode chip for backlight unit for improving current expansion and preparation method thereof |
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| CN112267134A (en) * | 2020-11-24 | 2021-01-26 | 赵玉平 | Electroplating solution additive for electroplating Co-Ni alloy |
| CN115182009A (en) * | 2022-07-11 | 2022-10-14 | 余姚市爱迪升电镀科技有限公司 | Bright nickel-tungsten alloy plating solution and preparation process of corrosion-resistant multilayer plating layer |
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| CN103911637A (en) * | 2014-03-28 | 2014-07-09 | 马鞍山马钢表面工程技术有限公司 | Ni-Co-W alloy electroplating solution for working surface of copper plate of continuous casting crystallizer and preparation method of Ni-Co-W alloy electroplating solution |
| CN103911637B (en) * | 2014-03-28 | 2016-08-17 | 马鞍山马钢表面工程技术有限公司 | Copper plate working surface of continuously casting crystallizer Ni-Co-W alloy plating liquid and preparation method thereof |
| CN104028716A (en) * | 2014-06-19 | 2014-09-10 | 马鞍山马钢表面工程技术有限公司 | Method for using Ni-Co-W alloy electroplate liquid to repair nickel-plated combined crystallizer narrow plate in electroplating manner |
| CN104028716B (en) * | 2014-06-19 | 2016-03-23 | 马鞍山马钢表面工程技术有限公司 | The method of nickel plating fourplatemold narrow boards is repaired with the plating of Ni-Co-W alloy plating liquid |
| CN104762644A (en) * | 2015-04-24 | 2015-07-08 | 西峡龙成特种材料有限公司 | Electroplated amorphous-state nickel-tungsten-phosphorous alloy for copper plate of crystallizer for continuous casting and preparation process of amorphous-state nickel-tungsten-phosphorous alloy |
| CN104846409A (en) * | 2015-04-30 | 2015-08-19 | 云南民族大学 | High-tungsten-content flawless tungsten-nickel alloy coating layer and electroplating liquid and electroplating process |
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| CN107958946A (en) * | 2017-11-17 | 2018-04-24 | 扬州乾照光电有限公司 | A kind of light-emitting diode chip for backlight unit for improving current expansion and preparation method thereof |
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| CN112267134A (en) * | 2020-11-24 | 2021-01-26 | 赵玉平 | Electroplating solution additive for electroplating Co-Ni alloy |
| CN112267134B (en) * | 2020-11-24 | 2023-05-30 | 中山市康迪斯威科技有限公司 | Alloy electroplating solution |
| CN115182009A (en) * | 2022-07-11 | 2022-10-14 | 余姚市爱迪升电镀科技有限公司 | Bright nickel-tungsten alloy plating solution and preparation process of corrosion-resistant multilayer plating layer |
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