CN102115898A - Electro-deposition method for preparing bulk nano ferro-nickel alloy crystalline - Google Patents
Electro-deposition method for preparing bulk nano ferro-nickel alloy crystalline Download PDFInfo
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Abstract
The invention provides an electro-deposition method for preparing bulk nano-crystalline ferro-nickel alloy. Electro-deposition equipment capable of circularly filtering, stirring, temperature control and cathode movement is adopted; 1g/l to 3g/l of additive A and 0.25g/l to 0.75g/l of additive B are adopted; and the bulk nano ferro nickel alloy is acquired under the technological parameters that the electroplating solution temperature is 55 DEG C to 65 DEG C, the pH (hydrogen ion concentration) value is 3.2 to 3.8, and the cathode current density is 2A/dm2 to 8A/dm2. The invention has the characteristics of simple and easy-to-control technological process, steady product quality, small crystallite dimension, even structure, high purity, little environmental pollution, low production cost, and the like.
Description
Technical field
The present invention relates to a kind of method for preparing the block nanometer Metallic Solids, particularly relate to a kind of method for preparing large volume block nanometer metal alloy crystal.
Background technology
Nanocrystal has physical propertiess such as high strength that other common crystal do not have, high-ductility, wear resistance, ductility, hardness, resistance, chemical property and special sound, electricity, magnetic, heat, light, and application prospect is more and more wide.Because the nanometer crystal alloy material volume of most methods preparation is little, contain defectives such as hole, tiny crack, can't carry out performance tests such as mechanics.And adopt electro-deposition method to prepare the large volume nanometer crystal alloy now and also have very big difficulty.Therefore, large volume, high quality, preparation with real nanocrystalline structure alloy are current urgency problems to be solved.
Preparation large volume nano metal alloy crystalline technological difficulties are: the selection and the optimization of solution composition (main salt, complexing agent, stablizer, brightening agent etc.); The optimization of electro-deposition process parameter (cathode current density, anode-cathode relative moving speed, bath temperature, bath pH value etc.); The method that intermediate ion exchange of control deposition reaction process and ion are supplied with.The purpose of abovementioned technology is in order to increase nucleation rate to greatest extent, to suppress growth process, obtaining the high quality nano-crystal nickel ferroalloy materials that composition is even, crystallization crystal grain is tiny.
The present invention proposes the method for the large volume nano-crystal nickel iron alloy that a kind of prepared by electrodeposition composition is even, crystallization is careful.
Summary of the invention
The present invention need obtain large volume nano-crystal nickel ferroalloy materials on the cathode material surface by following processing method and processing condition: at first the anticathode material surface carries out clean, obtains cleaning, activating surface; Be nickel and iron level in the control large volume nano-crystal nickel iron alloy in galvanic deposit, it is anode material that the present invention adopts sheet nickel and pure iron plate; In galvanic deposit for making the careful internal stress little (or reduce internal stress) that do not produce of large volume nano-crystal nickel iron alloy crystallization, the present invention adds certain quantity of additive A and additive B in plating bath, wherein additive A can be selected BBI, propylene oxide, epoxy chloropropane, butynediol, this-sulfinic acid sodium, o-benzoic sulfimide etc., the perhaps combination of above-mentioned substance, additive B can be selected sodium laurylsulfonate, sodium lauryl sulphate, trisodium citrate etc., the perhaps combination of above-mentioned substance; For make large volume nanocrystalline can continuous growth in galvanic deposit, composition evenly, form no layered structure, the present invention adopts whole the stirring to plating bath, whipped form can adopt at the uniform velocity mechanical stirring or ultrasonic agitation, particularly adopts circulating filtration stirring or negative electrode to move the combination of stirring or above-mentioned stirring; The present invention through a large amount of experiments determine to be 3.2～3.8 at 55～65 ℃ of temperature of electroplating solution, pH, cathode current density is 2～8A/dm
2Processing condition under, can obtain the nano level Rhometal crystal of stable large volume.
In sum, a kind of preparation large volume nanometer Rhometal crystalline electro-deposition method provided by the invention is characterized in that:
1) with the conducting metal being cathode material, is anode material with sheet nickel and pure iron plate;
2) electroplate liquid is the aqueous solution, and composition is made up of single nickel salt 200～250g/l, ferrous sulfate 10～20g/l, boric acid 40～45g/l, sodium-chlor 20～30g/l, Trisodium Citrate 15～20g/l, additive A 1～3g/l, additive B 0.25～0.75g/l;
3) the anticathode material carries out surface activation process;
4) in the ferro-nickel alloy electroplating process electroplate liquid being carried out integral body stirs;
5) temperature of electroplating solution is 55～65 ℃; PH is 3.2～3.8; Cathode current density is 2～8A/dm
2
Above-mentioned said additive A is one or both or the two or more mixing in the following material: BBI, propylene oxide, epoxy chloropropane, butynediol, this-sulfinic acid sodium, o-benzoic sulfimide.
Above-mentioned said additive B is one or both and the two or more mixing in the following material: sodium laurylsulfonate, sodium lauryl sulphate, trisodium citrate.
Above-mentionedly saidly electroplate liquid is carried out whole the stirring to circulating filtration stir or negative electrode moves stirring or the at the uniform velocity combination of mechanical stirring or ultrasonic agitation or above-mentioned stirring.
The invention has the advantages that:
1, in present method implementation process, adopt sulfate bath just can obtain the tiny densification of crystallization, the uniform large volume nano-crystal nickel of composition ferroalloy materials at cathode surface, all treatment soln of employing (pre-treatment, electroplate liquid) are little, the cheap regular solution of environmental pollution.And simple, the easy-operating characteristics of technology are arranged.
2, the gordian technique of acquisition nanometer crystal alloy material is to select additive, additive level and adding frequency and adding cycle.
3, by activation treatment, add additive and CONTROL PROCESS condition can obtain can continuous growth, composition is even, crystallization is careful, no layered structure, internal stress is little or the large volume nano-crystal nickel ferroalloy materials of internal stress free.The maximum ga(u)ge of the large volume nano-crystal nickel iron alloy that obtains is more than 7mm.
Description of drawings
Fig. 1 is the microtexture that adopts the nano-crystal nickel ferroalloy materials of the inventive method preparation.
Fig. 2 is the X-ray diffractogram that adopts the nano-crystal nickel ferroalloy materials of the inventive method preparation.
Embodiment:
1, embodiment one
Test adopts the soft steel sample as cathode material, and sheet nickel and pure iron plate are anode material, and wherein the sheet nickel area is 100mm * 100mm; The pure iron plate area is 100mm * 20mm.Electroplating power supply adopts silicon controlled rectification power source.Adopt cathode moving device and circulation filter in the electroplating process.The soft steel sample is carried out ferro-nickel alloy electroplating under circulation stirring and negative electrode mobile condition after through rust cleaning, oil removing, surface activation process, solution composition and plating condition see Table 1.Nano-crystal nickel ferroalloy materials microtexture that obtains and phase structure are as shown in Figure 1 and Figure 2.
2, embodiment two
After adopting above-mentioned soft steel sample through rust cleaning, oil removing, surface activation process, adopt anode material and electroplating device under the condition that circulating filtration and negative electrode move, to carry out ferro-nickel alloy electroplating.Its electroplate liquid formulation and processing condition see Table 2, also can obtain better result.
3, embodiment three
After adopting above-mentioned soft steel sample through rust cleaning, oil removing, surface activation process, adopt anode material and electroplating device under the condition that circulating filtration and negative electrode move, to carry out ferro-nickel alloy electroplating.Its electroplate liquid formulation and processing condition see Table 3, also can obtain better result.
Table 1 solution composition and plating condition
Table 2 solution composition and plating condition
Table 3 solution composition and plating condition
Claims (6)
1. one kind prepares large volume nanometer Rhometal crystalline electro-deposition method, it is characterized in that:
1) with the conducting metal being cathode material, is anode material with sheet nickel and pure iron plate;
2) electroplate liquid is the aqueous solution, and composition is made up of single nickel salt 200～250g/l, ferrous sulfate 10～20g/l, boric acid 40～45g/l, sodium-chlor 20～30g/l, Trisodium Citrate 15～20g/l, additive A 1～3g/l, additive B 0.25～0.75g/l;
3) the anticathode material carries out surface activation process;
4) in the ferro-nickel alloy electroplating process electroplate liquid being carried out integral body stirs;
5) temperature of electroplating solution is 55～65 ℃; PH is 3.2～3.8; Cathode current density is 2～8A/dm
2
Wherein: said additive A is one or both or the two or more mixing in the following material: BBI, propylene oxide, epoxy chloropropane, butynediol, this-sulfinic acid sodium, o-benzoic sulfimide; Said additive B is one or both and the two or more mixing in the following material: sodium laurylsulfonate, sodium lauryl sulphate, trisodium citrate.
2. electro-deposition method as claimed in claim 1 is characterized in that: in the said ferro-nickel alloy electroplating process electroplate liquid is carried out whole the stirring to circulating filtration and stir or negative electrode moves stirring or the at the uniform velocity combination of mechanical stirring or ultrasonic agitation or above-mentioned stirring.
3. electro-deposition method as claimed in claim 1 is characterized in that: said electroplating bath components is made up of single nickel salt 225～245g/l, ferrous sulfate 15～18g/l, boric acid 40～42g/l, sodium-chlor 25～28g/l, Trisodium Citrate 15～18g/l, additive A 1.5～2.5g/l, additive B 0.35～0.55g/l;
4. electro-deposition method as claimed in claim 1 is characterized in that: said additive A is BBI or butynediol or both combinations.
5. electro-deposition method as claimed in claim 1 is characterized in that: said additive B is sodium laurylsulfonate or sodium lauryl sulphate or both combinations.
6. electro-deposition method as claimed in claim 1 is characterized in that: 58～62 ℃ of said temperature of electroplating solution; Said pH is 3.5～3.8; Said cathode current density is 4～6A/dm
2
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104034457A (en) * | 2014-04-30 | 2014-09-10 | 江西师范大学 | Method of testing electrodeposition stress |
| CN106498451A (en) * | 2016-10-31 | 2017-03-15 | 华北理工大学 | A kind of iron-nickel alloy low-carbon (LC) steel composite material and preparation method thereof |
| CN107737948A (en) * | 2017-10-20 | 2018-02-27 | 成都理工大学 | The preparation method of the Fe@Ni nanocrystals of cube structure |
| CN108559915A (en) * | 2018-05-16 | 2018-09-21 | 河南工程学院 | A kind of dilval and preparation method thereof |
| CN110067011A (en) * | 2019-03-28 | 2019-07-30 | 上海大学 | Prepare the method and electric deposition device of bulk nano-crystalline nickel |
| CN111333473A (en) * | 2020-03-10 | 2020-06-26 | 攀枝花学院 | High and low temperature resistant emulsion explosive and preparation method thereof |
-
2009
- 2009-12-31 CN CN2009102181532A patent/CN102115898A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104034457A (en) * | 2014-04-30 | 2014-09-10 | 江西师范大学 | Method of testing electrodeposition stress |
| CN104034457B (en) * | 2014-04-30 | 2016-08-24 | 江西师范大学 | A kind of method testing electro-deposition stress |
| CN106498451A (en) * | 2016-10-31 | 2017-03-15 | 华北理工大学 | A kind of iron-nickel alloy low-carbon (LC) steel composite material and preparation method thereof |
| CN106498451B (en) * | 2016-10-31 | 2018-09-04 | 华北理工大学 | A kind of iron-nickel alloy-mild steel composite material and preparation method |
| CN107737948A (en) * | 2017-10-20 | 2018-02-27 | 成都理工大学 | The preparation method of the Fe@Ni nanocrystals of cube structure |
| CN107737948B (en) * | 2017-10-20 | 2019-05-10 | 成都理工大学 | The preparation method of the Fe@Ni nanocrystal of cube structure |
| CN108559915A (en) * | 2018-05-16 | 2018-09-21 | 河南工程学院 | A kind of dilval and preparation method thereof |
| CN108559915B (en) * | 2018-05-16 | 2019-10-11 | 河南工程学院 | A kind of dilval and preparation method thereof |
| CN110067011A (en) * | 2019-03-28 | 2019-07-30 | 上海大学 | Prepare the method and electric deposition device of bulk nano-crystalline nickel |
| CN111333473A (en) * | 2020-03-10 | 2020-06-26 | 攀枝花学院 | High and low temperature resistant emulsion explosive and preparation method thereof |
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Application publication date: 20110706 |