CN103806076A - Method for asymmetric alternating current-direct current plating of Fe-nano ZrO2 composite coating - Google Patents
Method for asymmetric alternating current-direct current plating of Fe-nano ZrO2 composite coating Download PDFInfo
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- CN103806076A CN103806076A CN201210451167.0A CN201210451167A CN103806076A CN 103806076 A CN103806076 A CN 103806076A CN 201210451167 A CN201210451167 A CN 201210451167A CN 103806076 A CN103806076 A CN 103806076A
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Abstract
The invention relates to a method for asymmetric alternating current-direct current plating of a Fe-nano ZrO2 composite coating. The method comprises the following steps: (1) adding 300-450g of molysite to each liter of distilled water, adjusting the pH value to 0.5-2.0 after dissolving, and then adding 10-20g of sodium chloride, 10-60g of nano ZrO2, 1-3g of ascorbic acid, 1-5g of saccharin and 0.05-2.0g of lauryl sodium sulfate; (2) pouring the solution obtained in the step (1) into a coating bath, keeping the temperature of the solution at 20-50 DEG C, and putting the coating bath into a magnetic field; and (3) adopting a asymmetric alternating current-direct current mode, wherein the asymmetric alternating current-direct current plating mode comprises three processes of plating, transition plating and direct current plating. By adopting the method, the Fe-nano ZrO2 composite coating is obtained by adding the nano ZrO2 and improving the components and the electroplate deposition condition of an electroplate liquid, and has extremely low internal stress, and excellent hardness and wear-resisting property.
Description
Technical field
The present invention relates to metal material field, be specifically related to a kind of method of preparing nano iron plating by electro-deposition.
Background technology
Cause more than 70% discharge of environmental pollution from production.For reducing as far as possible the harm of a large amount of waste products to environment, maximally utilise the added value of waste product, then manufacturing engineering is arisen at the historic moment in the world.Manufacturing engineering can extend work-ing life, improving product performance, save energy, the protection of the environment of product again, meets the strategy of sustainable development.Nano surface work is as the gordian technique of manufacturing engineering again, applying of manufacturing engineering again had to important effect, it not only can recover piece surface size, can also significantly improve surface property, reaches the object of the desired recovery of manufacturing engineering or upgrading performance again.
The reasons such as physical abuse mainly comes from wearing and tearing, scuffing, fatigue damage, damages, insufficient lubrication.Iron is as cheap metal, in the earth's crust, reserves are abundant, plating iron technology is a kind of restorative procedure of component of machine, owing to thering is the features such as sedimentation velocity is fast, current efficiency is high, technique is simple, production cost is low, substantially pollution-free, the mechanical wear part of industry or the reparations of processing error part such as communications and transportation, mining equiment, machinofacture are successfully used to, and obtained good economic benefit and social benefit, can and obtain good economic benefit in the more huge effect of performance in manufacturing engineering again to its nanometer.
CN101386999A discloses a kind of method of preparing nano iron plating by electro-deposition, as follows: in every liter of distilled water, add 300～450g molysite, after dissolving, regulate pH value to 0.5～2.0; Every liter is added 1～5g asccharin and 0.05～0.2g sodium lauryl sulphate again; Above-mentioned solution is poured in coating bath, and solution temperature remains on 20～50 ℃, and coating bath is placed in to magnetic field; Adopt dipulse system, the dutycycle of direct impulse is 25～75%, the dutycycle of reverse impulse is 5～20%, positive and negative pulse frequency 10～50Hz, peak current density 10～the 30A/dm of both forward and reverse directions pulse ↑, direct impulse current duration compares 20:1 with reverse impulse current duration.The preparing nano iron plating by electro-deposition method that the method provides has easy and simple to handle, easy control, production efficiency advantages of higher, is applicable to recover manufacturing engineering and the material protection again such as piece surface size, raising surface property.
But the coating that the method obtains can't meet some requirement of production application at aspect of performances such as hardness, wear resistance, resistance to high temperature oxidation.
Summary of the invention
For the deficiencies in the prior art, one of object of the present invention is to provide a kind of asymmetric AC-DC electroplating Fe-nanometer ZrO
2the method of composite deposite.Described method is by adding nanometer ZrO
2with component and the electroplating deposition condition of improving electroplate liquid, obtain Fe-nanometer ZrO
2composite deposite, it has extremely low internal stress, fabulous hardness and wear resisting property.
Technical problem to be solved by this invention is to provide a kind of method of preparing nano iron plating by electro-deposition.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows:
A kind of asymmetric AC-DC electroplating Fe-nanometer ZrO
2the method of composite deposite, the method comprises the steps:
(1) in every liter of distilled water, add 300～450g molysite, after dissolving, regulate pH value to 0.5～2.0; Every liter is added sodium-chlor 10-20g, nanometer ZrO again
210-60g, xitix 1-3g, 1～5g asccharin and 0.05～0.2g sodium lauryl sulphate;
(2) solution step (1) being obtained is poured in coating bath, and solution temperature remains on 20～50 ℃, and coating bath is placed in to magnetic field;
(3) adopt asymmetrical alternating current-direct current mode: asymmetric AC-DC electroplating comprises plating, transition plating and 3 processes of DC plating; In the plating stage, positive and negative two halves Bob β value is got 1.1-1.4, and watt current density is got 1-3A/dm2, stops 3-7min, is transformed into transition plating; In the transition plating stage, first in 7min, make anodal current density rise to 8-10A/dm2, cathodal current density is down to 0.5-1A/dm2, then stop 3-8min, after transition has been plated, in 1min, adjust anodal current density to 15-30A/dm2, cathodal current density, to 0A/dm2, is transformed into DC plating; DC plating current density is 15-30A/dm2.
In step (1), described molysite is ferrous salt, preferably FeCl
24H
2o.
In step (1), described coating bath is take pure iron sheet as anode, take plating metal workpiece as negative electrode.
In step (2), described magnetic field is produced by current coil, and electric current is 5～20A.
In step (2), described magnetic field, the direction that in the direction of its magnetic induction density and coating bath, negatively charged ion moves is perpendicular or parallel, hereinafter to be referred as vertical magnetic field or parallel magnetic field, preferred parallel magnetic field, most preferably parallel magnetic field in the same way.
The present invention has following beneficial effect:
(1) method of preparing nano iron plating by electro-deposition of the present invention, owing to having adopted suitable solution and solution parameter, makes the grain fineness number of settled layer reach nanometer scale; Adding of adding of additive asccharin and sodium lauryl sulphate, particularly asccharin can obviously reduce grain-size, improves the toughness of settled layer; Magnetic field is improved Solution Dispersion ability and current efficiency, and parallel equidirectional magnetic field significantly declines settled layer grain fineness number; Use two pulse, be conducive to further reducing of settled layer grain fineness number, the present invention can make the settled layer that grain fineness number is 15～100nm.Preparing nano iron plating by electro-deposition method provided by the invention has easy and simple to handle, easy control, production efficiency advantages of higher, is applicable to recover manufacturing engineering and the material protection again such as piece surface size, raising surface property.
(2) the present invention adopts asymmetric AC-DC electroplating method can obtain that internal stress is little, the composite deposite of smooth densification, effectively reduces the generation of coating crackle.
Embodiment
For ease of understanding the present invention, it is as follows that the present invention enumerates embodiment.Those skilled in the art should understand, described embodiment helps to understand the present invention, should not be considered as concrete restriction of the present invention.
Following examples, need make coating bath with synthetic glass, and self-control coil produces foreign field, first pure iron sheet (plating metal workpiece) are eliminated rust, oil removal treatment, then carry out galvanic deposit and make nano iron plating.
Embodiment 1:
Solution parameter is: FeCl
24H
2o concentration is 400g/L, and solution temperature is 30 ℃, and pH value 1.0 is added sodium-chlor 10g/L, nanometer ZrO
210g/L, xitix 1g/L, 1g asccharin and 0.05g/L sodium lauryl sulphate/L.
Vertical magnetic field, in externally-applied magnetic field coil, electric current is 5A.
Asymmetrical alternating current-direct current mode: asymmetric AC-DC electroplating comprises plating, transition plating and 3 processes of DC plating; In the plating stage, positive and negative two halves Bob β value gets 1.1, and watt current density is got 1A/dm2, stops 3min, is transformed into transition plating; In the transition plating stage, first in 7min, make anodal current density rise to 8A/dm2, cathodal current density is down to 0.5A/dm2, then stop 3min, after transition has been plated, in 1min, adjust anodal current density to 15A/dm2, cathodal current density, to 0A/dm2, is transformed into DC plating; DC plating current density is 15A/dm2.
Embodiment 2:
Solution parameter is: FeCl
24H
2o concentration is 350g/L, and solution temperature is 20 ℃, and pH value 1.5 is added sodium-chlor 20g/L, nanometer ZrO
260g/L, xitix 3g/L, 5g asccharin and 0.02g/L sodium lauryl sulphate;
Parallel magnetic field in the same way, in externally-applied magnetic field coil, electric current is 20A;
Asymmetrical alternating current-direct current mode: asymmetric AC-DC electroplating comprises plating, transition plating and 3 processes of DC plating; In the plating stage, positive and negative two halves Bob β value gets 1.4, and watt current density is got 3A/dm2, stops 7min, is transformed into transition plating; In the transition plating stage, first in 7min, make anodal current density rise to 10A/dm2, cathodal current density is down to 1A/dm2, then stop 8min, after transition has been plated, in 1min, adjust anodal current density to 30A/dm2, cathodal current density, to 0A/dm2, is transformed into DC plating; DC plating current density is 30A/dm2.
Embodiment 3
Solution parameter is: FeCl
24H
2o concentration is 450g/L, and solution temperature is 50 ℃, and pH value 2.0 is added sodium-chlor 15g/L, nanometer ZrO
235g/L, xitix 2g/L, 3g asccharin and 0.1g/L sodium lauryl sulphate/L.
Vertical magnetic field, in externally-applied magnetic field coil, electric current is 10A.
Asymmetrical alternating current-direct current mode: asymmetric AC-DC electroplating comprises plating, transition plating and 3 processes of DC plating; In the plating stage, positive and negative two halves Bob β value gets 1.3, and watt current density is got 2A/dm2, stops 5min, is transformed into transition plating; In the transition plating stage, first in 7min, make anodal current density rise to 9A/dm2, cathodal current density is down to 0.75A/dm2, then stop 5min, after transition has been plated, in 1min, adjust anodal current density to 20A/dm2, cathodal current density, to 0A/dm2, is transformed into DC plating; DC plating current density is 20A/dm2.
Applicant's statement, the present invention illustrates detailed process equipment and process flow process of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned detailed process equipment and process flow process, do not mean that the present invention must rely on above-mentioned detailed process equipment and process flow process and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, and the selections of the equivalence replacement to the each raw material of product of the present invention and the interpolation of ancillary component, concrete mode etc., within all dropping on protection scope of the present invention and open scope.
Claims (7)
1. an asymmetric AC-DC electroplating Fe-nanometer ZrO
2the method of composite deposite, is characterized in that the method comprises the steps:
(1) in every liter of distilled water, add 300～450g molysite, after dissolving, regulate pH value to 0.5～2.0; Every liter is added sodium-chlor 10-20g, nanometer ZrO again
210-60g, xitix 1-3g, 1～5g asccharin and 0.05～0.2g sodium lauryl sulphate;
(2) solution step (1) being obtained is poured in coating bath, and solution temperature remains on 20～50 ℃, and coating bath is placed in to magnetic field;
(3) adopt asymmetrical alternating current-direct current mode: asymmetric AC-DC electroplating comprises plating, transition plating and 3 processes of DC plating; In the plating stage, positive and negative two halves Bob β value is got 1.1-1.4, and watt current density is got 1-3A/dm2, stops 3-7min, is transformed into transition plating; In the transition plating stage, first in 7min, make anodal current density rise to 8-10A/dm2, cathodal current density is down to 0.5-1A/dm2, then stop 3-8min, after transition has been plated, in 1min, adjust anodal current density to 15-30A/dm2, cathodal current density, to 0A/dm2, is transformed into DC plating; DC plating current density is 15-30A/dm2.
2. the method for preparing nano iron plating by electro-deposition according to claim 1, is characterized in that the molysite described in step (1) is ferrous salt.
3. the method for preparing nano iron plating by electro-deposition according to claim 2, is characterized in that the molysite described in step (1) is FeCl
24H
2o.
4. the method for preparing nano iron plating by electro-deposition according to claim 1, is characterized in that the coating bath described in step (2) is take pure iron sheet as anode, take plating metal workpiece as negative electrode.
5. the method for preparing nano iron plating by electro-deposition according to claim 1, is characterized in that the magnetic field described in step (2) is produced by current coil, and electric current is 5～20A.
6. the method for preparing nano iron plating by electro-deposition according to claim 1 or 5, is characterized in that the magnetic field described in step (2), and the direction that in the direction of its magnetic induction density and coating bath, negatively charged ion moves is perpendicular or parallel.
7. the method for preparing nano iron plating by electro-deposition according to claim 6, is characterized in that the magnetic field described in step (2), and the direction of its magnetic induction density is parallel with the direction that negatively charged ion in coating bath moves.
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|---|---|---|---|
| CN201210451167.0A CN103806076A (en) | 2012-11-12 | 2012-11-12 | Method for asymmetric alternating current-direct current plating of Fe-nano ZrO2 composite coating |
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| CN201210451167.0A CN103806076A (en) | 2012-11-12 | 2012-11-12 | Method for asymmetric alternating current-direct current plating of Fe-nano ZrO2 composite coating |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104947157A (en) * | 2015-05-14 | 2015-09-30 | 大连大学 | Electrodeposition-laser remelting strengthening technology for Fe-ZrO2 nano composite layer on 45# steel surface |
| CN105018971A (en) * | 2015-07-20 | 2015-11-04 | 哈尔滨工业大学 | Method for preparing functional micro-nano structure dendritic alpha-Fe-based material through iron |
| CN108221012A (en) * | 2018-01-03 | 2018-06-29 | 西北工业大学 | A kind of Fe-Ni/ZrO2The electro-deposition preparation method of nanocomposite |
| CN108754534A (en) * | 2018-05-25 | 2018-11-06 | 山东师范大学 | A kind of the iron-based non-precious metal catalyst and preparation method of electro-catalysis synthesis ammonia |
-
2012
- 2012-11-12 CN CN201210451167.0A patent/CN103806076A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104947157A (en) * | 2015-05-14 | 2015-09-30 | 大连大学 | Electrodeposition-laser remelting strengthening technology for Fe-ZrO2 nano composite layer on 45# steel surface |
| CN105018971A (en) * | 2015-07-20 | 2015-11-04 | 哈尔滨工业大学 | Method for preparing functional micro-nano structure dendritic alpha-Fe-based material through iron |
| CN105018971B (en) * | 2015-07-20 | 2017-09-12 | 哈尔滨工业大学 | A kind of method by the dendritic α Fe sills of iron standby functional micro-nano structure |
| CN108221012A (en) * | 2018-01-03 | 2018-06-29 | 西北工业大学 | A kind of Fe-Ni/ZrO2The electro-deposition preparation method of nanocomposite |
| CN108754534A (en) * | 2018-05-25 | 2018-11-06 | 山东师范大学 | A kind of the iron-based non-precious metal catalyst and preparation method of electro-catalysis synthesis ammonia |
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Application publication date: 20140521 |