CN1152631A - Al-Ti alloy plating and making method thereof - Google Patents

Al-Ti alloy plating and making method thereof Download PDF

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Publication number
CN1152631A
CN1152631A CN 95119521 CN95119521A CN1152631A CN 1152631 A CN1152631 A CN 1152631A CN 95119521 CN95119521 CN 95119521 CN 95119521 A CN95119521 A CN 95119521A CN 1152631 A CN1152631 A CN 1152631A
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alloy plating
nacl
electroplating
plating
content
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CN1048042C (en
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郭乃名
过家驹
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Institute of Process Engineering of CAS
University of Science and Technology Beijing USTB
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University of Science and Technology Beijing USTB
Institute of Chemical Metallurgy CAS
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Abstract

The present invention relates to a kind of Al-Ti alloy electroplated layer material containing 50% Ti content and possessing excellent high-temp. oxidation resistance and resistance to corrosion. Its preparation method uses a fused-salt electroplating process, and its electroplating temp. is 130-250 deg.C, and an AlCl3-NaCl-KCl or AlCl3-NaCl fused salt system is adopted, and TiCl3, NaCl(KCl).TiCln (n=2,3) or TiCl4 can be directly added in the fused salt for addition of Ti ions. When electroplating, metal Al or metal Al and metal Ti or graphite can be used as positive electrode. Said invention possesses the advantages of saving energy, low cost, high electric efficiency, excellent electroplate layer properties, no damaging plated metal base material properties and easily-controlled plated layer thickness.

Description

Al-Ti alloy plating and method for making thereof
The invention relates to a kind of novel galvanization coating material and manufacture method thereof, belong to molten salt electrochemistry and field of metal surface treatment technology.
As everyone knows, premium properties such as that aluminium, titanium and alloy thereof have is corrosion-resistant, resistance to high temperature oxidation, specific tenacity height is metal ideal composite surface materials such as iron and steel, can be widely used in aspects such as oil, chemical industry, boats and ships, automobile, machinery, metallurgy.But because the sedimentation potential of aluminium, titanium is more negative than the deposition potential of hydrogen, therefore this coating can not be produced with common aqueous solution electro-plating method.Electroplate Al and AL-Ti alloy and become a urgent important technological problems to be solved.
The present aluminum-plated component of using mainly is to adopt following two kinds of methods to produce:
1, hot dip process method: [J.A.Mock, Materials Engineering, 1972, VOl.75, p.48-51.] No.2 promptly is being immersed in the Al liquid of fusing by the plating parts, this method is to be raw material with pure metal Al, carries out under the high temperature more than 700 ℃.Therefore not only cost height, energy consumption are big, and substrate performance is worsened, and the Al-Fe alloy layer that is generated also causes plating material processing characteristics to descend, and also have shortcomings such as thickness of coating is wayward.
2, vacuum evaporation and hot spray process: be that to adopt pure metal Al and Al powder be raw material, vaporising under vacuum or carry out thermospray, production cost height, coating be difficult for evenly and bonding force poor, be easy to take place pitting in the use.
Also have the method for in the organic solution medium, electroplating Al in addition, then because of costing an arm and a leg, the organic solution poorly conductive, problem such as inflammable is difficult to use in actual production.
In recent years abroad begun one's study and adopted fused salt electrolysis method to carry out Al and Al-Mn alloy plating [Li Qingfeng, H.A.Hjuler, et al.J.Electrochem.Soc.1990VOl.137, No.2, p.593-598], thereby avoided the shortcoming of hot dip coating method, but the high temperature oxidation resisting of Al and Al-Mn alloy layer and solidity to corrosion etc. can't satisfy the service requirements under the harsh corrosive environment.Ti and Al-Ti alloy have very good thermotolerance and corrosion resistance nature, carry out the Al-Ti coelectrodeposition in low-temperature molten salt, are expected to make the new A l-Ti alloy layer of thermotolerance and excellent corrosion-proof performance.
The Al-Ti alloy plating that the purpose of this invention is to provide a kind of high temperature oxidation resisting and excellent corrosion-proof performance, and low-temperature molten salt is electroplated the method for Al-Ti alloy.The concrete solution and the technology contents of invention are:
The invention provides a kind of plating Al-Ti alloy plated layer.Base material is metallic substance such as iron, carbon steel, copper, stainless steel, aluminium, nickel, and its coating is characterized as: coating contains the Ti amount and is 0.1-50 (wt) % (surplus is Al content), and the coating adhesion amount is 1-100g/M 2Ti in the Al alloy layer of the present invention can suppress stripping and the oxidation of Al in the coating, and increases the compactness of coating.Coating contains the Ti amount and is lower than 0.1 (wt) %, then is difficult to form fine and close anti-corrosion coating, and coating contains Ti to be measured when being higher than 50 (wt) %, and the coating apparent mass is poor.The coating adhesion amount is less than 1g/M 2, solidity to corrosion deficiency then, the coating adhesion amount is greater than 100g/M 2, the coating processing characteristics worsens.
The invention provides a kind of manufacture method of Al-Ti alloy plating, is to have adopted in low temperature (130 ℃-250 ℃) fused salt Al-Ti coelectrodeposition to produce the method for Al-Ti alloy layer.This preparation method is characterised in that:
1. adopt AlCl 3-NaCl-KCl molten salt system or AlCl 3-NaCl molten salt system, wherein AlCl 3Content is at 50.1mol%-99mol%,, NaCl, the ratio between the KCl can be selected arbitrarily, and the fused salt for preparing is put into plating tank, is heated to fusing.The adding mode of titanium ion in the fused salt can directly add TiCl 3, or MaCl (KCl) TiCl n(n=2,3) salt, or directly add TiCl 4It adds Ti ionic amount is 10ppm to 2 (wt) %.
2. adopt metal A l or metal A l and metal Ti when electroplating, or graphite is as anode.
Anode shape can adopt ring-type, cylindric or tabular.The anode number can be one or more.
3. electroplating temperature is between 130 ℃-250 ℃.
4. electroplating the cathode current density that adopts is 0.01A/cm 2-1.2A/cm 2
In the plating time slot fused salt velocity of flow at 0.05M/sec-5M/sec.
6. also can feed N in the plating tank 2Or protection of inert gas such as Ar.
7. use usual method degreasing, pickling, washing before the plating of metal plating piece, after thorough drying, put into fused salt and electroplate, electroplate back plating piece water flushing, oven dry.
Advantage of the present invention and positively effect:
1. adopt fused salt as electroplating medium, make the plating of Al-Ti alloy become possibility.
2. adopt low-temperature molten salt (below 250 ℃) to electroplate, therefore not only energy-conservation, and do not damage by the metallizing substrate performance.
3. adopt cheap chloride system fused salt, with low cost.
4. adopt fused salt to electroplate, so it is high to have the electricity effect, metal plating is in conjunction with firm, and thickness of coating is easy to control.
5. the Al-Ti alloy layer of Huo Deing has excellent thermotolerance and solidity to corrosion.
Solidity to corrosion, the stable on heating comparison test of the present invention's resulting Al-Ti alloy plated layer sample and control sample the results are shown in table 1.As shown in table 1, Al-Ti alloy plating of the present invention has excellent solidity to corrosion and thermotolerance.
Different coating material thermotolerances of table 1 and corrosion proof comparison
Sample type Base material Coating is formed Adhesion amount g/M Solidity to corrosion Thermotolerance Remarks
????1 Carbon steel (A3) Al-3Ti ????30 ????O ????O Example of the present invention
????2 Carbon steel (A3) Al-10Ti ????30 ????O ????O Example of the present invention
????3 Carbon steel (A3) Al-40Ti ????30 ????O ????O Example of the present invention
????4 Carbon steel (A3) Al-10Mn ????35 ????△ ????△ Reference examples
????5 Carbon steel (A3) Zn ????70 ????× ????× Reference examples
????6 The 1Cr13 stainless steel - ????- ????※ ????※ Reference examples
Annotate: solidity to corrosion evaluation method: cyclic wetting and drying test.Sample soaked 1 hour in 5%NaCl solution after, take out in 50 ℃ of dryings 0.5 hour round-robin test 600 times.Produce red rust area by it and estimate its solidity to corrosion, 0 be＜5%, and △ is 5-20%, and ※ is 20-70% * be＞70%.
Thermotolerance evaluation method: sample was heated 24 hours down in 800 ℃, by its surrosion (mg/cm 2) estimate its thermotolerance.O is＜1mg/cm 2, △ is 1-5mg/cm 2, ※ is 5-30mg/cm 2, * be＞30mg/cm 2
Provide specific embodiment of the present invention below, the Al-Ti alloy plated layer performance that each embodiment makes, meet table 1 shown in the result.
Embodiment 1:
Workpiece to be plated is a cold-rolled steel sheet, with usual method degreasing, pickling, washing, drying.
1, adopt AlCl 3-NaCl-KCl fused salt (wherein mol ratio is 80: 15: 5), adding Ti ionic amount in fused salt is 100ppm.
2, anode adopts Graphite Electrodes.
3, ionogen (fused salt) flow velocity is 0.8m/sec.
4,140 ℃ of electroplating temperatures.
5, cathode current density is 0.8A/cm 2
6, feed N in the plating tank 2Protection.
7, electroplating time is 4 minutes.
8, electroplate back sample water flushing, oven dry.
Plating makes that to contain Ti amount in the Al-Ti alloy layer be 2.25%, and Al content is 97.75%.
Embodiment 2:
Workpiece to be plated is a copper, after usual method degreasing, pickling, washing, drying, with electroplated.
1, adopt AlCl 3-NaCl (its mol ratio is 57: 43) fused salt.Adding Ti ionic amount in fused salt is 0.6 (wt) %.
2, anode adopts metal A l plate and metallic titanium plate.
3, electrolyte flow rate is 0.2m/sec.
4, electroplating temperature is at 230 ℃.
5, cathode current density is 0.05A/cm 2
6, electroplating time is 15 minutes.
7, electroplate back sample water flushing, oven dry.
Plating makes that the titaniferous amount is 40% in the Al-Ti alloy layer, and aluminum content is 60%.
Embodiment 3:
Workpiece to be plated is a technically pure iron, after usual method degreasing, pickling, washing, drying, with electroplated.
1, adopt AlCl 3-NaCl-KCl fused salt (mol ratio is 60: 21: 19).Adding Ti ionic amount in the fused salt is 800ppm.
2, with pure metal Al orificed anode.
3, electrolyte flow rate is 1.5m/sec.
4, electroplating temperature is 180 ℃.
5, cathode current density is 0.1A/cm 2
6, feed the Ar protection in the plating tank.
7, electroplating time is 8 minutes.
8, electroplate back sample water flushing, oven dry.
Plating makes that to contain Ti amount in the Al-Ti alloy layer be 18%, and aluminium content is 82%.

Claims (8)

1, a kind of Al-Ti alloy plating is characterized in that:
(1) wherein the content of Ti is 0.1-50 (wt) %, and all the other are Al content;
(2) the coating adhesion amount is 1-100g/M 2
(3) base material is a metallic substance.
2, Al-Ti alloy plating as claimed in claim 1 is characterized in that said substrate metal material is carbon steel, iron, copper, stainless steel, aluminium, nickel.
3, Al-Ti alloy plating as claimed in claim 1 is characterized in that preferable Ti content proportioning is 6 (wt) %-42 (wt) %.
4, a kind of method for making of Al-Ti alloy plating is characterized in that:
(1) adopts AlCl 3-NaCl-KCl molten salt system or AlCl 3-NaCl molten salt system, wherein AlCl 3Content is 50.1mol-99mol%, and the ratio between NaCl and the KCl can be selected arbitrarily; The add-on of titanium ion is 10ppm to 2 (wt) % in the fused salt;
(2) electroplating temperature is between 130 ℃-250 ℃;
Adopt metallic aluminium or metallic aluminium and metal titanium when (3) electroplating, or graphite is as anode;
(4) electroplating the cathode current density that adopts is 0.01A/cm 2-1.2A/cm 2
(5) the fused salt velocity of flow is 0.05 meter per second-5 meter per second in the plating time slot.
5, the method for making of Al-Ti alloy plating as claimed in claim 4 is characterized in that the adding method of said titanium ion is, can directly add TiCl 3, or NaCl (KCl) TiCln (n=2,3) salt, or directly add TiCl 4
6, the method for making of Al-Ti alloy plating as claimed in claim 4 is characterized in that also can feeding shielding gas nitrogen or argon gas in the plating tank.
7, the method for making of Al-Ti alloy plating as claimed in claim 4 is characterized in that anodic is shaped as ring-type, cylindric or tabular, and the anode number is one or more.
8, the method for making of Al-Ti alloy plating as claimed in claim 4 is characterized in that optimal components ratio and condition are: AlCl 3Content is at 55mol%-80mol%, and current density is 0.03A/cm 2-0.3A/cm 2, electroplating temperature is that 150 ℃ of-200 ℃ of electrolyte flow rate are at 0.5M/sec-4M/sec.
CN95119521A 1995-12-19 1995-12-19 Al-Ti alloy plating and making method thereof Expired - Fee Related CN1048042C (en)

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CN101914791A (en) * 2010-09-15 2010-12-15 武汉钢铁(集团)公司 Method for electroplating corrosion resistant aluminum-manganese alloy layer
CN101065519B (en) * 2004-11-24 2011-04-20 住友电气工业株式会社 Molten salt bath, precipitate, and process for producing metal precipitate
CN102191519A (en) * 2011-04-28 2011-09-21 上海交通大学 Method for preparing molten salt electrodeposition aluminium membrane on surface of aluminium based composite material
CN102776416A (en) * 2012-07-11 2012-11-14 东莞市闻誉实业有限公司 Aluminum alloy electroplating coating and preparation method thereof
CN103409775A (en) * 2013-08-26 2013-11-27 江苏启迪合金有限公司 Method for producing aluminum-titanium alloy through electrolysis
CN105154922A (en) * 2015-08-12 2015-12-16 贵州盘县紫森源（集团）实业发展投资有限公司 Method for preparing aluminum-titanium alloy with coal gangue as raw materials
US20160268632A1 (en) * 2013-11-06 2016-09-15 Research Foundation Of The City University Of New York Ionic liquid comprising alkaline earth metal
CN107460502A (en) * 2017-09-21 2017-12-12 北京工业大学 A kind of method that fused salt electro-deposition for adding solid phase particle prepares alloy
CN109023431A (en) * 2018-09-30 2018-12-18 成都先进金属材料产业技术研究院有限公司 The method for preparing titanium-aluminium alloy
CN113897645A (en) * 2021-11-18 2022-01-07 中国兵器工业第五九研究所 Preparation method of corrosion-resistant decontamination coating

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Cited By (15)

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Publication number Priority date Publication date Assignee Title
CN101065519B (en) * 2004-11-24 2011-04-20 住友电气工业株式会社 Molten salt bath, precipitate, and process for producing metal precipitate
CN101914791B (en) * 2010-09-15 2012-08-22 武汉钢铁(集团)公司 Method for electroplating corrosion resistant aluminum-manganese alloy layer
CN101914791A (en) * 2010-09-15 2010-12-15 武汉钢铁(集团)公司 Method for electroplating corrosion resistant aluminum-manganese alloy layer
CN102191519B (en) * 2011-04-28 2014-08-06 上海交通大学 Method for preparing molten salt electrodeposition aluminium membrane on surface of aluminium based composite material
CN102191519A (en) * 2011-04-28 2011-09-21 上海交通大学 Method for preparing molten salt electrodeposition aluminium membrane on surface of aluminium based composite material
CN102776416A (en) * 2012-07-11 2012-11-14 东莞市闻誉实业有限公司 Aluminum alloy electroplating coating and preparation method thereof
CN103409775A (en) * 2013-08-26 2013-11-27 江苏启迪合金有限公司 Method for producing aluminum-titanium alloy through electrolysis
CN103409775B (en) * 2013-08-26 2015-11-11 江苏启迪合金有限公司 A kind of method of electrolysis production aluminum titanium alloy
US20160268632A1 (en) * 2013-11-06 2016-09-15 Research Foundation Of The City University Of New York Ionic liquid comprising alkaline earth metal
CN106463769A (en) * 2013-11-06 2017-02-22 纽约城市大学研究基金会 Ionic liquid comprising alkaline earth metal
CN105154922A (en) * 2015-08-12 2015-12-16 贵州盘县紫森源（集团）实业发展投资有限公司 Method for preparing aluminum-titanium alloy with coal gangue as raw materials
CN107460502A (en) * 2017-09-21 2017-12-12 北京工业大学 A kind of method that fused salt electro-deposition for adding solid phase particle prepares alloy
CN109023431A (en) * 2018-09-30 2018-12-18 成都先进金属材料产业技术研究院有限公司 The method for preparing titanium-aluminium alloy
CN109023431B (en) * 2018-09-30 2020-05-12 成都先进金属材料产业技术研究院有限公司 Method for preparing titanium-aluminum alloy
CN113897645A (en) * 2021-11-18 2022-01-07 中国兵器工业第五九研究所 Preparation method of corrosion-resistant decontamination coating

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