CN1161383A - Rare-earth, zinc and aluminium alloy coating material, and art for hot-dip plating - Google Patents
Rare-earth, zinc and aluminium alloy coating material, and art for hot-dip plating Download PDFInfo
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- CN1161383A CN1161383A CN 96120984 CN96120984A CN1161383A CN 1161383 A CN1161383 A CN 1161383A CN 96120984 CN96120984 CN 96120984 CN 96120984 A CN96120984 A CN 96120984A CN 1161383 A CN1161383 A CN 1161383A
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Abstract
The invented hot dip plating technology includes: the steel wire to be plated is degreased, washed, acid cleaned, treated with rare earth composite salt plating aid solvent, in a plating tank contg. zinc aluminium alloy plating liquid. The steel wire is then drown out of the plating tank, air cooled and wound. The rare earth composite salt plating aid solvent is an aqueous solution containing NH4Cl 280-300 g/l, ZnCl2 200-220g/l, ReCl3 180-220g/l, in which Re is equal to or less than 1.0%, Al is equal to or less than 0.5%, the rest is Zn, total impurity not more than 0.060%, the steel wire moving speed is 11.0m/min.
Description
The present invention relates to novel rare-earth zinc aluminum alloy coating material and or immersion thereof in the field of metallurgy, handle to carry out rare earth reinforced, the rear earth zinc-aluminium alloy coating of formation is plated on the base steel material of different size densely, as all kinds of steel or other steel products for the treatment of plating.
At present; the coating for protection against corrosion of steel product mainly contains different coating systems such as electro-galvanizing, galvanizing, aluminium, aluminium zinc both at home and abroad, utilizes above-mentioned processing method; in steel product (as steel wire etc.) coating surface corrosion resistant coating, be used for realizing protection to matrix metal.Along with the global atmosphere environmental quality worsens, corrosion of coating aggravates day by day, obviously can't satisfy the material protection requirement of modern industry in the erosion resistance of monometallic coating, particularly zinc coating and work-ing life.For corrosion resistance nature aluminium zinc or aluminium-zinc alloy preferably, all exist the manufacturing cost height, product is difficult for defectives such as realization.The common employing gas reduction of industrially developed country (being Sendzimir Sendzimir) method is produced in the world, and production unit is very complicated, is not suitable for China's national situation.Domestic still do not have this method at present and produce the steel wire example.The another one distinct issues of conventional zinc aluminum alloy coating Production for Steel Wire are owing to the zinc-base plating bath that contains 5% aluminium is to be under the zinc one aluminium eutectic composition condition, fusing point only is about 380 ℃, the liquid metal surface tension is little, when so the plating steel wire is drawn, resulting thickness of coating is too thin, as under many circumstances, have to adopt so-called " two plating method " to come coating is thickeied, to reach the thickness requirement of domestic and international product technology standard to coating.It needs to be noted that at aluminium zinc in the past, during the al-zn alloy coating plating was produced, the adding of rare earth metal was only for single technology purpose.For example, the matrix surface of plating metal is carried out wetting, to prevent occurring defectives such as plating leakage in the plating process.The zinc aluminum alloy coating steel wire product requires height to producing apparatus in addition, and complex manufacturing, production quality control are very difficult, and product cost is high, does not still have the national standard of this series products at present.In view of the foregoing, domestic have only only a few producer can adopt simple solvent method to carry out limited scale production.Simultaneously because the inherent defect of simple solvent method production technique, therefore ubiquity and help that plating property is poor, the speed of a motor vehicle is low, molten bath control difficulty, product coating became uneven, coating weight does not reach the index of national regulation, and a series of problems such as quality instability, thereby restricted of the development of this new technology in China.
The object of the present invention is to provide in a kind of field of metallurgy the novel hot-dip depositing process and by the resulting rear earth zinc-aluminium alloy coating material of this technology.This technology is handled by carrying out rare earth reinforced, the rear earth zinc-aluminium alloy coating of formation is plated on the base steel material of different size densely, as all kinds of steel or other steel products for the treatment of plating.
Purpose of the present invention and characteristics are based on technical scheme realization of the present invention, therefore in the present invention:
The rear earth zinc-aluminium alloy coating or immersion that is provided among the present invention mainly comprises steel wire to be plated through after a series of comprehensive pretreatment, use compound rare-earth salt galvanizing-aid solvent used for hot-dip galvanizing provided by the present invention, it is inserted carry out hot dip process in the zinc-base plating bath and handle, when steel wire is drawn in the alloy molten bath continuously automatically, attached to the liquid alloy on the steel wire matrix surface in process of setting, along with system temperature reduces, rare earth as solute metal, aluminium element will constantly be separated out preferential crystallization with hypersaturated state from zinc, and will be enriched in the zinc oxide soil (Re that coating surface forms densification
2O
3) aluminum oxide (Al
2O
3) the composite table facial mask (δ=10nm-50nm) that constituted.Inferior top layer is bred and is rear earth zinc-aluminium alloy, below is pure zinc layer and transition layer.The existence of wherein top layer composite membrane has certain mechanical protection effect to coating, isolated contacting of coating surface and corrosive medium, thereby slowed down corrosion of coating.The existence of this film, increased simultaneously electrochemical system resistance, thereby suppressed electrochemical process.The existence of this oxide film has also improved coating surface state (as the change of refractive index), thereby has made the coating appearance luster beautiful, so that the outward appearance of product has is stronger ornamental.
Wherein comparatively detailed rear earth zinc-aluminium alloy coating or immersion comprises: with steel wire to be plated through degrease, washing, pickling, utilize the rare earth composite salt to help the plating solvent treatment, enter and carry out plating in 470 ± 5 ℃ the liquid rear earth zinc-aluminium alloy coating bath and handle, after steel wire is drawn crystallization, through the air naturally cooling, on roll up or send strand;
It is NH that wherein said rare earth composite salt helps the plating solvent composition
4Cl=280--300g/L, ZnCl
2=200-220g/L, ReCl
3=180-220g/L, NH
4The aqueous solution of F=40-60g/L;
Wherein said liquid rear earth zinc-aluminium alloy plating bath consists of Re≤1.0%, Al≤0.5%, Pb≤0.03%, Fe≤0.02%, Cd≤0.001%, Cu≤0.001%, and surplus is Zn, and Pb, Fe, Cd, Cu total amount are not more than 0.060%;
Wherein said steel wire travelling speed is 11.0m/min, and the cell body useful length is 5500mm.
Such plating alloy coating weight can reach 360g/m
2-390g/m
2Coating constituent structure analytical results is Re for top layer
2O
3+ Al
2O
3, the composite membrane thickness that is constituted is 10nm-50nm, and inferior top layer is rear earth zinc-aluminium alloy (Re-Zn-Al) alloy, and composition and content are: Al＞25%, La=0.3%, Ce=0.5% (atomic percent).Internal layer is essentially pure zinc layer, with the matrix transition layer be plasticity iron zinc-aluminium ternary alloy preferably, tack test shows that self twines does not ftracture, the coating outward appearance is bright and clean, color and luster is beautiful, has stronger decorative appearance.
As can be seen from the above technical solutions: technology purpose of the present invention is extensive: the adding of rare earth metal is also considered the metallurgy processing effect of rare earth metal emphatically in the present invention except that the common process purpose.The bigger rare earth metal of chemically reactive can form the less mixture of density with the detrimental impurity reaction in the plating bath, floats to the alloy electroplating bath surface on easily, purifies the plating bath metal; Coating surface can form the rare earth alloy component among the present invention and constitute surface film: " under the rare earth reinforced treatment process control condition, can form the alumite of one deck densification.When steel wire is drawn the coating crystallization from plating bath, the aluminium of hypersaturated state and rare earth will be separated out from zinc, preferential crystallization, and be enriched in the Al that coating surface forms phase against corrosion and is oxidized to one deck densification rapidly
2O
3+ RE
2O
3Oxide film.This oxide film has not only improved the condition of surface (as the change of refractive index) of coating; make the coating appearance luster beautiful; this class oxide film has higher stability than the zinc oxide film simultaneously; coating had certain mechanical protection effect; isolate contacting of coating surface and corrosive medium, thereby slowed down corrosion of coating.The existence of this oxide film has increased the resistance of electrochemical system simultaneously, has suppressed electrochemical process, under the rare earth element effect, produces the non-crystalline state oxide film of one deck densification, further improves the corrosion stability of coating; The adding approach is different with the molten principle method of joining among the present invention: utilize the solid solubility temperature of norium in zinc liquid among the present invention first, create solid-state norium is inserted in the fused alloy plated state, utilize the dissolving of rare earth metal, spread, make the special process method of the certain equilibrium concentration of alloy electroplating bath middle-weight rare earths content maintenance.Created the molten method of completing the square of secondary master alloy in addition, the molten temperature of joining is low, and alloy ingredient is easy to control, and mobility strong is easy to operate.Compare with the gas reduction method (being Sendzimir Sendzimir) that developed country generally adopts; it need not obtain coating under tight gas shield environment; but the solvent method of having continued to use suitable China's national situation is produced; therefore; production unit is simple relatively, investment descends significantly; production cost also reduces significantly, and the coating outward appearance that obtains surpasses general zinc aluminum alloy coating, and corrosion resistance also is significantly increased.
One of important feature of the present invention is exactly to help the rare-earth salt processing of plating solvent.Rare-earth salts and " zinc chloride+ammonium chloride " mixing salt are configured as the mishmetal composite salt, can significantly improve plating condition lower substrate metallic surface state, strengthen and help the plating effect.Rare-earth salt processing is removed base metal surface impurity and oxide compound thereof to increasing the solvent activity, improves wettingly, adjusts and helps the physico-chemical property of plating solvent, has irreplaceable effect of other any salt and technological effect.
Resisting atmosphere quality worsens, controls steel product and expose corrosion of coating and add according to being the common issue that countries in the world material protection research workers are faced.One of important development trend of world industry developed country steel anti-corrosive coating is exactly to replace traditional pot galvanize coating for protection against corrosion with the pot galvanize aluminum alloy coating.Novel coating for protection against corrosion such as internationally recognized Galvalume, Galfan have been produced by product standard (as ASTM) in industrially developed country such as the U.S., and are used widely.Positive achievement is being obtained aspect the research and development of zinc aluminum alloy coating steel wire product and the production in China metal products field.Yet because the difference of technical equipment, product manufacture state of the art, compare with gas reduction (being Sendzimir Sendzimir) the method production technique that industrially developed country in the world generally adopts, the zinc aluminum alloy coating steel wire that domestic solvent process is produced, compare with industrially developed country aspect quality in the quantity of product that still there is a big difference, product far can not satisfy the demand of domestic and international market.Develop and produce rear earth zinc-aluminium alloy coating wire series product with international most advanced level, for basic industries such as China's electric power, communication, railway traffic provide the service of high-quality relevant equipment, the technology that enlarges rare earth resources is used, build up rear earth zinc-aluminium alloy coating wire production line, Chinese national economy is built have very positive meaning with advanced international level.Therefore the invention provides compound rare-earth salt galvanizing-aid solvent used for hot-dip galvanizing, and adopt or immersion and obtained effect preferably, why the present invention is achieved and the advantage that has above prior art is: for zinc base alloy coating system, the self-passivation effect of aluminium shows that it can improve the thermodynamic stability of coating system.Under good process control condition, coating surface can form the alumite of one deck densification.When steel wire is drawn the coating crystallization from plating bath, the aluminium of hypersaturated state and rare earth will be separated out from zinc, preferential crystallization, and be enriched in the Al that coating surface forms phase against corrosion and is oxidized to one deck densification rapidly
2O
3+ Re
2The O complex oxide film.This oxide film has not only improved the condition of surface (as the change of refractive index) of coating; make the coating appearance luster beautiful; this class oxide film has higher thermodynamic stability than the zinc oxide film simultaneously; coating had certain mechanical protection effect; isolated coating surface and corrosive medium contact, thereby slow down corrosion of coating.The existence of this oxide film has increased the resistance of electrochemical system simultaneously, has suppressed electrochemical process.Under the rare earth element effect, be expected to produce the non-crystalline state oxide film of one deck densification, further improve the corrosion stability of coating.
The coating basic mechanical design feature index comparing result table 1 as shown in table 1 (steel core steel wire part) of resulting coating of the coating material that uses compound rare-earth salt galvanizing-aid solvent used for hot-dip galvanizing provided by the present invention and technology to obtain and domestic and international correlation standard
| Sequence number | The contrast project | GB1200 | ASTM??B 802 | IEC?209 | Company's product standard | |
| 1 | The coated metal classification | Zinc | Aluminium zinc | Zinc | Rear earth zinc-aluminium alloy | |
| 2 | Maximum coating weight (g/m 2) | 259 | 305、 610、915 | 305、610 | 305、610 | |
| 3 | The coating adhiesion test | The wrapping test number of turns | 8 | 8 | 8 | 8 |
| Axle diameter/steel wire diameter | 4、5 | 3、4、5 | 3、4、5 | 2、3、4 | ||
| 4 | Copper sulfate test (inferior) | 4、5 | 3、4、5 | 3、4、5 | 2-4 (A level) | |
| 5 | Artificial accelerated corrosion test (NSS test) | No requirement (NR) | No requirement (NR) | No requirement (NR) | Recommend requirement | |
| 6 | The surface chromating is handled | No requirement (NR) | No requirement (NR) | No requirement (NR) | Recommend requirement | |
| 7 | Coating wire density (g/m 2) | No standard | 7.78 | 7.78 | 7.78 | |
| 8 | Steel wire resistivity (r 20＝0.191，57 Ω.mm 2/m | No standard | Provide representative value | Provide representative value | Provide representative value | |
Test-results proves simultaneously, have good material compatibility (Compatibility) as steel core steel wire, rear earth zinc-aluminium alloy coated steel core wire and Aluminium Cable Steel Reinforced (ACSR), steel core rare earth aluminum stranded conductor, can significantly slow down the galvanic corrosion between aluminium-zinc, the work-ing life that crevice corrosion is inclined to, has improved the power transmission and transformation cable products.The coating microstructure analysis proved and do not contained the fragility phase in the coating system, therefore can fundamentally stop the cracking of coating or comes off.The positive effect of eliminating fragility phase in the coating also shows, can avoid the steel wire brittle fracture that fragility influences formed steel wire micro-flaw mutually and causes thus in the system, thereby improve the electric transmission and distribution circuit operating safety.
Country's technology authoritative department detects proof to every technical feature of the rear earth zinc-aluminium alloy coating wire product that technology realized according to the present invention, this product is significantly higher than the technical requirements of national standard to the galvanized steel wire product, and part has surpassed ASTM, IEC index.Aspect the artificial accelerated corrosion test of coating; GB 6458 (ISO 3768) " metal cladding neutral salt spray test (NSS test) " presses in ferrous materials test center of country, Wuhan Material Protection Inst., Ministry of Machine Building; GB 9789 (ISO 3988) standards such as " the sulfur dioxide corrosion tests under metal and the common condensation condition of other non-organic coating layer "; this product strict test and examination have been carried out; test-results shows that this coating product corrosion resistance significantly is better than the hot dip galvanizing coating steel wire.
Economic worth analytical results of the present invention shows: work-ing life of (1) product and social benefit analysis: the artificial accelerated corrosion test of this product and galvanized steel wire product as seen, its SO
2Test, indexes such as the steel wire erosion rate the NSS test conditions under, weightlessness only are thread 1/2 or lower of galvanized steel wire, and the corrosion resistance that has proved this product is 2 times of general galvanized steel wire or higher.Product expected service life is by being higher than 1 times of calculating of common galvanized steel wire, and product use value can improve more than 1 times.Count the steel wire residual life behind the corrosion of coating, comprehensive maintenance is changed factors such as the labour cost, the increase of product safety coefficient of circuit, and obvious user can obtain double product utilization coefficient.By our company's 1.2 ten thousand tons of output now, can be the economize on the use of funds economic interests of ten thousand yuan of 12000 * 7000=8400 of user altogether, promptly can produce 8,400 ten thousand yuan social benefit at least, my the company's annual production of back of expanding production is 3.2 ten thousand tons, and the social benefit that is produced is more considerable; (2) this product has overcome domestic production zinc aluminum alloy coating steel wire coating thin thickness, and weak point such as cost an arm and a leg.By the International Usage requirement supply of material, steel wire coating thickness is significantly higher than national standard, and the general zinc aluminum alloy coating steel wire thickness of domestic production only has 2/3 of this product, and general about 9000 yuan/ton of price.My company's high-quality coating wire price only is about 7000 yuan per ton.Owing to creatively adopted advanced production technology, reduced all kinds of consumption, product cost is reduced, product is in great demand simultaneously, impel company's industrial scale constantly to enlarge, so the business economic benefit is also very remarkable; (3) use the coating wire product of explained hereafter provided by the present invention to supply by the technical qualification of international standards such as the IEC of International Electrotechnical Commission, U.S. ASTM, international advanced industrial standards requirement, product standard and International Usage are pressed rail, therefore have certain capacity to earn foreign exchange through exports.
Use the coating wire analyzing and testing result of explained hereafter provided by the present invention to be: to have Zn, Al, O, C (date file MA01) .XPS to measure Zn2p on the new immersion plating specimen surface
3/2The bound energy at peak is that the kinetic energy at 1023.7eV, ZnLMM Auger peak is the binding ability 75.1eV at 992.3eV and 987.1eV, Al2P peak.The composition of sample surfaces is ZnO, Al
2O
3, element Zn, pollute carbon.Peel off (date file MA11) behind about 10nm with argon ion sputtering, the main component of sample surfaces is element Zn and Al
2O
3, a spot of ZnO, to pollute carbon, also have the valency of 0.3% La, 0.5% Ce, Ce in addition be trivalent, the XPS quantitative result sees Table 2.Table 2:XPS quantitative result (atomic percent %)
| Sample | zn | Al | O | C | La | Ce |
| New immersion plating sample | 4.2 | 11.4 | 32.7 | 51.7 | ||
| New immersion plating sample is peeled off 10nm | 8.1 | 27.9 | 48.2 | 14.9 | 0.3 | 0.5 |
Fig. 1 is a process flow sheet of the present invention.
Plating production with steel wire is example, specifies implementation procedure of the present invention:
Embodiment 1
With φ=2.2mm, its Chemical Composition is C=0.67-0.75%, Si=0.17-0.37%, Mn=0.50-0.80%, P≤0.035%, S≤0.035%, Ni≤0.25%, Cr≤0.25, the steel wire of Cu≤0.25% uses after degrease, washing, pickling and consists of NH
4Cl=280--300g/L, ZnCl
2=200-220g/L, ReCl
3=180-220g/L, NH
4The rare earth composite salt of F=40-60g/L helps plating aqueous solvent solvent to handle, enter then 470 ± 5 ℃, in component is arranged is that Re≤1.0%, Al≤0.5%, total impurities are not more than and carry out plating in the zinc-base plating bath coating bath of 0.060% liquid rear earth zinc-aluminium alloy and handle, after steel wire is drawn crystallization, through the air naturally cooling, on roll up or send strand.Wherein the steel wire travelling speed is 11.0m/min, and the cell body useful length is 5500mm, and only a plating alloy coating weight can reach 360g/m
2-390g/m
2The constituent structure analytical results of coating is Re for top layer
2O
3+ Al
2O
3, the composite membrane that is constituted, thickness are 10nm-50nm, and inferior top layer is rear earth zinc-aluminium alloy (Re-Zn-Al) alloy, and composition and content are: Al＞25%, La=0.3%, Ce=0.5% (atomic percent).Internal layer is essentially pure zinc layer, with the matrix transition layer be plasticity iron zinc-aluminium ternary alloy preferably, tack test: self twines and does not ftracture, and the coating outward appearance is bright and clean, and color and luster is beautiful, has stronger decorative appearance.
The artificial accelerated corrosion test of coating wire (comparing under the identical condition of thickness of coating) result is:
1, SO
2Concentration is 675ppm, RH 〉=95%, 40 ± 3 ℃ of test temperatures, etching time 72 hours, test-results: anti-SO
2Performance significantly is better than hot-dip galvanizing steel wire;
2, salt-fog test: 5%NaCl solution, 35 ± 2 ℃ of test temperatures are tested 144 hours not show rust, and conclusion (of pressure testing): salt spray resistance improves more than 2 times than hot-dip galvanizing steel wire.
Claims (2)
1, novel rare-earth zinc aluminum alloy coating material or immersion, comprising: with steel wire to be plated through degrease, washing, pickling, use the rare earth composite salt to help the plating solvent treatment, enter and carry out plating in the coating bath of the liquid rear earth zinc-aluminium alloy plating bath of 470 ± 5 ℃ be built-in with and handle, after steel are drawn crystallization, through the air naturally cooling, on roll up or send strand; It is NH that wherein said rare earth composite salt helps the plating solvent composition
4Cl=280--300g/L, ZnCl
2=200-220g/L, ReCl
3=180-220g/L, NH
4The aqueous solution of F=40-60g/L; Wherein said liquid rear earth zinc-aluminium alloy plating bath consists of Re≤1.0%, Al≤0.5%, and surplus is Zn, and total impurities is not more than 0.060%; Wherein said steel wire travelling speed is 11.0m/min.
2, novel rare-earth zinc aluminum alloy coating material and or immersion thereof, it can be used for preparing the base steel material that novel plating has rear earth zinc-aluminium alloy, and wherein to become top layer be Re to base steel material structural group
2O
3+ Al
2O
3The composite membrane thickness that is constituted is 10nm-40nm, inferior top layer is rear earth zinc-aluminium alloy (Re-Zn-Al) alloy, composition and content are: Al＞25%, La=0.3%, Ce=0.5% (atomic percent), internal layer is essentially pure zinc layer, with the matrix transition layer be plasticity iron zinc-aluminium ternary alloy preferably.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 96120984 CN1161383A (en) | 1996-12-10 | 1996-12-10 | Rare-earth, zinc and aluminium alloy coating material, and art for hot-dip plating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 96120984 CN1161383A (en) | 1996-12-10 | 1996-12-10 | Rare-earth, zinc and aluminium alloy coating material, and art for hot-dip plating |
Publications (1)
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|---|---|
| CN1161383A true CN1161383A (en) | 1997-10-08 |
Family
ID=5126716
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|---|---|---|---|
| CN 96120984 Pending CN1161383A (en) | 1996-12-10 | 1996-12-10 | Rare-earth, zinc and aluminium alloy coating material, and art for hot-dip plating |
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| CN102121087A (en) * | 2011-01-28 | 2011-07-13 | 浙江永丰钢业有限公司 | Formula of strip steel rare-earth zinc aluminum alloy coating |
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- 1996-12-10 CN CN 96120984 patent/CN1161383A/en active Pending
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| CN102560312B (en) * | 2010-12-16 | 2013-12-18 | 贵州华科铝材料工程技术研究有限公司 | Seven-combination modified low-zinc aluminum alloy plating material for hot-dip plating and preparation method thereof |
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