CN106381510A - Preparing technology of Ni-Fe-P alloy-based compound coating - Google Patents
Preparing technology of Ni-Fe-P alloy-based compound coating Download PDFInfo
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- CN106381510A CN106381510A CN201611109783.2A CN201611109783A CN106381510A CN 106381510 A CN106381510 A CN 106381510A CN 201611109783 A CN201611109783 A CN 201611109783A CN 106381510 A CN106381510 A CN 106381510A
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- composite deposite
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
- C25D3/562—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of iron or nickel or cobalt
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/04—Electroplating with moving electrodes
- C25D5/06—Brush or pad plating
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
- C25D5/36—Pretreatment of metallic surfaces to be electroplated of iron or steel
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/48—After-treatment of electroplated surfaces
- C25D5/50—After-treatment of electroplated surfaces by heat-treatment
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- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
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- Organic Chemistry (AREA)
- Electroplating Methods And Accessories (AREA)
- Electroplating And Plating Baths Therefor (AREA)
Abstract
The invention provides a preparing technology of a Ni-Fe-P alloy-based compound coating. The matrix material of the compound coating is amorphous/ nanocrystalline Ni-Fe-P alloy, the Ni content is 80-90wt% of the compound coating, the Fe content is 5-20wt% of the compound coating, and the P content is 5-15wt% of the compound coating. A second phase in the compound coating is a grain growth inhibitor, such as VC<1-x> and TiC, and the content of the second phase is 0-5wt% of the compound coating. The preparing technology of the compound coating comprises: 1, pretreating a metal plated surface; 2, activating second phase particles; 3, carrying out electric brushing plating on a Ni-Fe-P amorphous compound coating; and 4, carrying out partial crystallization transformation on the compound coating.
Description
Technical field
The present invention relates to a kind of electroplating process for surface and composite deposite, especially relate to one kind with amorphous/nanocrystalline Ni-
Fe-P alloy is the composite deposite preparation technology of matrix.
Background technology
Particularity (shortrange order) on non crystalline structure, so that non-crystalline material is compared with conventional metals, has excellent power
Learn the advantages of performance, resistance to corrosion, chemism.Non-crystalline material easily induction local Adiabatic Shear Bands in deformation at room temperature are formed
Substance shear fissure and unexpected fracture failure, hardly represent the plastic deformation feature of macroscopic view, this greatly limits amorphous material
Material is as the application of structural material.On the other hand, the construction featuress of amorphous determine that it is in thermodynamic (al) metastable state, and this also limits
Make use under higher temperature occasion for the non-crystalline material.Therefore, using the second phase principle of strengthening and toughening, using complex technique,
Add high rigidity particle in amorphous alloy material（Or fiber）, so that macroscopical plasticity of non-crystaline amorphous metal, impact flexibility is improved,
Achieved with certain achievement in some non-crystalline materials.
Composite plating is to make metal using electrochemical method（Or alloy）With solid particle（Or fiber）Codeposition, in coating
Hardly there are diffusing phenomenon between parent metal and the solid particle of interpolation, therefore have the comprehensive of parent metal and solid particle concurrently
Close performance.The adaptability of technology of composite plating and practicality are broad, have stronger transmutability and operability, application will increasingly
Extensively.The ultimate principle of Brush Plating is identical with plating, without coating bath.Make during brush plating to be saturated with the plated pen of plating solution with certain relative fortune
Dynamic speed moves on plated surface, and keeps certain pressure, so that metal ion deposition is in plated material surface.Brush
Plating has that equipment is simple, process is simple, low cost, deposition velocity are fast, applied widely the features such as, be widely used to parts
Surface peening and reparation.Therefore, amorphous/nanocrystalline composite deposite is prepared using Brush Plating, give full play to non-crystaline amorphous metal matrix
With the excellent properties of nanoparticle, improve the wearability of coating, save material, there is important practical implementation and be worth.
Content of the invention
Ni-Fe-P non-crystaline amorphous metal has high-strength, the good excellent properties such as wear-resisting and anti-corrosion, and preparation technology more becomes
Ripe, it is the preferable matrix material of composite deposite, VC1-x, the grain growth inhibitor such as TiC, there is the spies such as very high intensity, hardness
Point, can suppress the formation of noncrystal substrate height local shear band, and can suppress the coarsening rate of crystal grain during crystallization change, reduce plus
The sensitivity to non-crystaline amorphous metal matrix crystallization change for the hot time, improves grasping of Ni-Fe-P amorphous/nanocrystalline matrix preparation technology
The property made.The technical problem to be solved is to provide one kind with amorphous/nanocrystalline Ni-Fe-P alloy as matrix, adds brilliant
The big inhibitor of grain length is as the composite deposite preparation technology of the second phase.
A kind of preparation technology of Ni-Fe-P alloy base composite cladding, be employed technical scheme comprise that：The matrix of composite deposite
Material is amorphous/nanocrystalline Ni-Fe-P alloy, and Ni content is the 80-90wt% of composite deposite, and Fe content is the 5- of composite deposite
20wt%（Preferably 8-12wt%）, P content is the 5-15wt% of composite deposite（Preferably 8-12wt%）, the second phase in described composite deposite
For VC1-x, the grain growth inhibitor such as TiC, content is the 0-5wt% of composite deposite（Preferably 0.5-2wt%）.
The preparation technology of the composite deposite of the present invention, comprises the following steps：
（1）The pretreatment on the plated surface of metal；
（2）The activation of second phase particles；
（3）Brush Plating Ni-Fe-P amorphous composite deposite；
（4）The partially-crystallized transformation of composite deposite.
The plated surface preparation of described metal includes rust cleaning, defat, activation process, can be using chemistry or electrochemical method；
Described technique of brush plating parameter is：The electric current density of electrode is 0.2-1.2A/mm2, electrode speed of related movement is 5-
20m/min（Preferably 8-15m/min）, plating temperature be 30-60 DEG C, plating solution Ph value 0.5-1.5；
Described brush composite plating solution consists of；Soluble nickel salt 2-4mol/L, ferrous salt 0.2-1mol/L, carboxylic acid 0.2-
0.6mol/L, boric acid 15-40g/L, second phase particles 5-25g/L, sodium hypophosphite or phosphorous acid 0.1-0.5mol/L, chelating agent
0.5-5g/L, reducing agent 0.5-2g/L；
Described soluble nickel salt includes：Nickel sulfate, Nickel dichloride.；
Described ferrous salt includes：Ferrous sulfate, ferrous chloride；
Described carboxylic acid includes：Acetic acid, formic acid, oxalic acid, citric acid etc.；
Described chelating agent includes：Tartaric acid, dodecylbenzene sodium sulfonate, sodium lauryl sulphate etc.；
The technological parameter of described partially-crystallized transformation is：300-330 DEG C of transition temperature, heat time heating time 0.2-0.5h.
Compared with prior art, the present invention has advantages below：
1., compared with preparing non-crystalline material with methods such as vacuum plating method, liquisol quenching methods, galvanoplastic have that equipment investment is few, plating solution becomes
Point simple, stability is high, lasts a long time, the features such as utilization rate of raw materials is high, and with surface crack method（Casting class）Prepare amorphous
Composite is compared, energy resource consumption is less, tissue evenly；
2., for comparing conventional plating, in plating solution, metal ion content is higher, has relative telemechanical simultaneously therefore allow to make between two electrodes
With higher electric current density, deposition rate of metal is fast；
3. when utilizing contour hard, the high high inhibition non-crystaline amorphous metal of VC, TiC to deform, the sliding of single shear band, promotes multiple shear bands
Generation and sliding, improve macroscopical plasticity of amorphous composite deposite and impact flexibility, also can strengthen the wear-resisting of composite deposite simultaneously
Property；VC, TiC etc. are also a kind of efficient grain growth inhibitor simultaneously, can suppress crystallization change when crystal grain coarsening rate,
Reduce the sensitivity to crystallization change for the acid extraction, improve operability and the controllability of its crystallization change technique；
4. pass through to adjust the concentration proportioning of electroplate liquid main component, the composite deposite of heterogeneity can be obtained, meet different occasions
Performance requirement；
5. pass through crystallization change, make life in Ni-Fe-P non-crystaline amorphous metal be changed into amorphous/chemical machining nano Ni-Fe-P alloy, improve non-
Between crystalline substance/nanostructured mutually coordinated with mate, make composite deposite internal stress reduce, the height office of amorphous can be suppressed further
The formation of domain shear band, improves impact flexibility and the combination property of composite deposite；
6. can obtain, by adjusting the technological parameter of crystallization change, the Ni-Fe-P being made up of different amorphous/nanocrystalline proportion of composing
Alloy substrate, thus adjusting the performance of composite deposite, meets the performance requirement of different occasions；
7. this plating solution formula does not contain the noxious substance such as cyanide, Cr VI, cadmium thus reducing the one-tenth of electroplate liquid recycling
Basis and difficulty, achievable green production；
8. Brush Plating has equipment and technology simply, does not disintegrate reparation with more real particularly with large-scale, precision equipment scene
With being worth.Brush Plating can adopt the plated pen of different model, and be furnished with shape insoluble anode different, not of uniform size, to various not
All can repair with geometry and baroque parts.
Specific embodiment
The invention will be further described with reference to embodiments.
The preparation of embodiment 1 amorphous/nanocrystalline Ni-Fe-P alloy/VC composite deposite
Amorphous/nanocrystalline Ni-Fe-P alloy/VC composite deposite, basic material is amorphous/nanocrystalline Ni-Fe-P alloy, Ni content
For the 83.4wt% of composite deposite, Fe content is the 10.6wt% of composite deposite, and P content is the 5.3wt% of composite deposite, VC content
0.7wt% for composite deposite.
Its electroplating technology, comprises the following steps：
（1）The pretreatment on plated metal surface：No. 45 steel plates selected by plating material, and plated surface is successively machined, then super
Sound wave cleaning machine adopts 20wt% sodium hydroxide solution with degreasing, finally, removes plated surface using 12wt% hydrochloric acid solution
Oxide-film, activated metal surface；
（2）The activation processing of solid particle：400 mesh VC microgranules are added to the hydrochloric acid solution cleaning of 15wt%, standby；
（3）Composite plating solution consists of：Nickel dichloride. 0.2 mol/L, nickel sulfate 1.8mol/L, ferrous sulfate 0.3mol/L, boric acid
20g/L, dodecylbenzene sodium sulfonate 1g/L, tartaric acid 0.5g/L, acetic acid 0.3mol/L, VC5g/L, sodium hypophosphite 0.24 mol/
L, potassium iodide 0.5g/L, titration hydrochloric acid to pH value to 1；
（4）The preparation of composite deposite：Anode adopts plate graphite, and the electric current density of electrode is 0.45 A/mm2, electrode fortune relatively
Dynamic speed is 8 m/min, and plating temperature is 40 DEG C；
（5）The post processing of composite deposite：0.2 h will be incubated at 320 DEG C of temperature by plated product, make amorphous Ni-Fe-P alloy-based
Body is changed into amorphous/nanocrystalline Ni-Fe-P alloy substrate.
Embodiment 2
The amorphous/nanocrystalline Ni-Fe-P alloy of the present embodiment //TiC composite deposite, basic material is amorphous/nanocrystalline Ni-Fe-
P alloy, Ni content is the 82.6wt% of composite deposite, and Fe content is the 8.1wt% of composite deposite, and P content is composite deposite
7.2wt%, TiC content is the 2.1wt% of composite deposite.
Its electroplating technology, comprises the following steps：
（1）The pretreatment of plate surface：Q235 steel plate selected by plating material, first through milling, mill, the plated surface of attrition process, then,
Degreasing is cleaned using 20wt% sodium hydroxide solution, finally, removes the oxide-film on plated surface using 12wt% hydrochloric acid solution, live
Change metal surface；
（2）The activation processing of microgranule：The TiC microgranule of 400 mesh is added in the hydrochloric acid solution of 25wt%, is heated to 65 DEG C of process
30min, is cleaned with distilled water 3 times, standby；
（3）Composite plating solution forms：Nickel sulfate 2.5mol/L, ferrous sulfate 0.2mol/L, oxalic acid 0.4mol/L, boric acid 15g/L,
Dodecylbenzene sodium sulfonate 0.8g/L, TiC15g/L, sodium hypophosphite 0.4mol/L, potassium iodide 0.5g/L, add hydrochloric acid and adjust
PH value is to 1.5；
（4）The preparation of composite deposite：Anode adopts plate graphite, and electrode plate current density is 0.6A/mm2, plating temperature is 45
℃；
（5）The post processing of composite deposite：0.3 h will be incubated at 310 DEG C of temperature by plated product, make amorphous Ni-P alloy substrate
It is changed into amorphous/nanocrystalline Ni-Fe-P alloy substrate.
Claims (2)
1. a kind of preparation technology of Ni-Fe-P alloy base composite cladding it is characterised in that：The basic material of composite deposite is non-
Crystalline substance/nanometer crystalline Ni-Fe-P alloy, Ni content is the 80-90wt% of composite deposite, and Fe content is the 5-20wt% of composite deposite（Excellent
Select 8-12wt%）, P content is the 5-15wt% of composite deposite（Preferably 8-12wt%）, in described composite deposite, second is mutually VC1-x、
The grain growth inhibitors such as TiC, content is the 0-5wt% of composite deposite（Preferably 0.5-2wt%）.
2. composite deposite preparation technology it is characterised in that：（1）The pretreatment on the plated surface of metal；（2）The work of second phase particles
Change；（3）Brush Plating Ni-Fe-P amorphous composite deposite；（4）The partially-crystallized transformation of composite deposite；
The plated surface preparation of described metal includes rust cleaning, defat, activation process, can be using chemistry or electrochemical method；
Described technique of brush plating parameter is：The electric current density of electrode is 0.2-1.2A/mm2, electrode speed of related movement is 5-
20m/min（Preferably 8-15m/min）, plating temperature be 30-60 DEG C, plating solution Ph value 0.5-1.5；
Described brush composite plating solution consists of；Soluble nickel salt 2-4mol/L, ferrous salt 0.2-1mol/L, carboxylic acid 0.2-
0.6mol/L, boric acid 15-40g/L, second phase particles 5-25g/L, sodium hypophosphite or phosphorous acid 0.1-0.5mol/L, chelating agent
0.5-5g/L, reducing agent 0.5-2g/L；
Described soluble nickel salt includes：Nickel sulfate, Nickel dichloride.；
Described ferrous salt includes：Ferrous sulfate, ferrous chloride；
Described carboxylic acid includes：Acetic acid, formic acid, oxalic acid, citric acid etc.；
Described chelating agent includes：Tartaric acid, dodecylbenzene sodium sulfonate, sodium lauryl sulphate etc.；
The technological parameter of described partially-crystallized transformation is：300-330 DEG C of transition temperature, heat time heating time 0.2-0.5h.
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107937945A (en) * | 2017-12-29 | 2018-04-20 | 刘志红 | A kind of galvanoplastic prepare Ni Fe P amorphous powder techniques |
| CN108060440A (en) * | 2017-12-30 | 2018-05-22 | 罗奕兵 | A kind of brush plating production method of iron-nickel-phosphor powder |
| CN108103538A (en) * | 2017-12-27 | 2018-06-01 | 刘志红 | A kind of cobalt-nickel-phosphor amorphous alloy powder preparation process |
| CN108103539A (en) * | 2017-12-29 | 2018-06-01 | 刘志红 | A kind of Ni-Fe-phosphorus amorphous powder production method |
| CN108145148A (en) * | 2017-12-28 | 2018-06-12 | 刘志红 | A kind of production technology based on brush nickel plating alloy amorphous powder |
| CN108165899A (en) * | 2017-12-27 | 2018-06-15 | 刘志红 | A kind of production method of Co-Fe-Ni-P powder |
| CN108179366A (en) * | 2017-12-28 | 2018-06-19 | 刘志红 | A kind of production method of the alloy amorphous state powder of Ni |
| CN108179365A (en) * | 2017-12-28 | 2018-06-19 | 刘志红 | A kind of production technology of brush plating method Ni-Co-P amorphous powders |
| CN108977845A (en) * | 2017-05-31 | 2018-12-11 | 刘志红 | A kind of Fe-based amorphous alloy catalysis electrode and preparation method thereof |
| CN108977843A (en) * | 2017-05-31 | 2018-12-11 | 刘志红 | A kind of ni-based amorphous alloy catalysis electrode and preparation method thereof |
| CN109137487A (en) * | 2017-06-18 | 2019-01-04 | 罗奕兵 | A kind of Ni-Fe-phosphorus non-crystalline alloy composite fibre and preparation method |
| CN109136889A (en) * | 2017-06-27 | 2019-01-04 | 罗奕兵 | A kind of cobalt-nickel-phosphor catalytic reactor and production method |
| CN109126656A (en) * | 2017-06-27 | 2019-01-04 | 罗奕兵 | A kind of Ni-Fe-phosphorus non-crystalline alloy catalytic reactor production method |
| CN110029379A (en) * | 2019-05-05 | 2019-07-19 | 东莞市康圣精密合金材料有限公司 | Ultra-wide stainless steel materials nickel plating appearance optimization technique |
| CN110029377A (en) * | 2019-05-15 | 2019-07-19 | 东南大学 | A kind of long-wave band blacker-than-black is composite porous and preparation method thereof |
| CN110829132A (en) * | 2019-10-18 | 2020-02-21 | 捷和电机制品(深圳)有限公司 | Carbon brush spring and direct current motor |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108977845A (en) * | 2017-05-31 | 2018-12-11 | 刘志红 | A kind of Fe-based amorphous alloy catalysis electrode and preparation method thereof |
| CN108977843A (en) * | 2017-05-31 | 2018-12-11 | 刘志红 | A kind of ni-based amorphous alloy catalysis electrode and preparation method thereof |
| CN109137487A (en) * | 2017-06-18 | 2019-01-04 | 罗奕兵 | A kind of Ni-Fe-phosphorus non-crystalline alloy composite fibre and preparation method |
| CN109126656A (en) * | 2017-06-27 | 2019-01-04 | 罗奕兵 | A kind of Ni-Fe-phosphorus non-crystalline alloy catalytic reactor production method |
| CN109136889A (en) * | 2017-06-27 | 2019-01-04 | 罗奕兵 | A kind of cobalt-nickel-phosphor catalytic reactor and production method |
| CN108165899A (en) * | 2017-12-27 | 2018-06-15 | 刘志红 | A kind of production method of Co-Fe-Ni-P powder |
| CN108103538A (en) * | 2017-12-27 | 2018-06-01 | 刘志红 | A kind of cobalt-nickel-phosphor amorphous alloy powder preparation process |
| CN108145148A (en) * | 2017-12-28 | 2018-06-12 | 刘志红 | A kind of production technology based on brush nickel plating alloy amorphous powder |
| CN108179366A (en) * | 2017-12-28 | 2018-06-19 | 刘志红 | A kind of production method of the alloy amorphous state powder of Ni |
| CN108179365A (en) * | 2017-12-28 | 2018-06-19 | 刘志红 | A kind of production technology of brush plating method Ni-Co-P amorphous powders |
| CN108103539A (en) * | 2017-12-29 | 2018-06-01 | 刘志红 | A kind of Ni-Fe-phosphorus amorphous powder production method |
| CN107937945A (en) * | 2017-12-29 | 2018-04-20 | 刘志红 | A kind of galvanoplastic prepare Ni Fe P amorphous powder techniques |
| CN108060440A (en) * | 2017-12-30 | 2018-05-22 | 罗奕兵 | A kind of brush plating production method of iron-nickel-phosphor powder |
| CN110029379A (en) * | 2019-05-05 | 2019-07-19 | 东莞市康圣精密合金材料有限公司 | Ultra-wide stainless steel materials nickel plating appearance optimization technique |
| CN110029377A (en) * | 2019-05-15 | 2019-07-19 | 东南大学 | A kind of long-wave band blacker-than-black is composite porous and preparation method thereof |
| CN110829132A (en) * | 2019-10-18 | 2020-02-21 | 捷和电机制品(深圳)有限公司 | Carbon brush spring and direct current motor |
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Application publication date: 20170208 |