CN1044680A - Cobalt-nickel-phosphorus non-crystalline alloy plating bath and coating - Google Patents
Cobalt-nickel-phosphorus non-crystalline alloy plating bath and coating Download PDFInfo
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- CN1044680A CN1044680A CN 89108740 CN89108740A CN1044680A CN 1044680 A CN1044680 A CN 1044680A CN 89108740 CN89108740 CN 89108740 CN 89108740 A CN89108740 A CN 89108740A CN 1044680 A CN1044680 A CN 1044680A
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Abstract
A kind of cobalt-nickel-phosphorus non-crystalline alloy plating bath and coating is to use Co-Ni-P of the present invention on normal temperature condition
2Plating bath is with the method acquisition non-crystalline state brushing coating of conventional brush plating.At Co-Ni-P
2Contain the formation that the Nb additive can promote amorphous alloy coating significantly in the alloy electroplating bath.This plating bath and coating can be widely used in recovering the mechanical component wearing and tearing, strengthen mechanical surface, improve the wear resisting property and the antiseptic property of machinery, improve nearly one times of die life.The plating bath process for preparation is easy, and use range is wide.
Description
The present invention relates to a kind of manufacture method of cobalt nickel-phosphorus amorphous alloy plating bath, plating bath is used for brush plating, forms amorphous alloy coating on the metallic substance top layer.
Amorphous alloy is a kind of type material, and the distribution of atom is that long-range is unordered in the ideal non-crystalline material, the crystal boundary that does not have general crystalline material and had, macroscopic defectss such as dislocation.Non-crystaline amorphous metal has high-performances such as high strength, high rigidity, high wear resistance and high corrosion resistance.But also have many problems aspect production technique and the Materials science two, the non-crystalline material great majority that use at present obtain with the liquid quenching method, and the speed of cooling that the liquid method of quenching requires is up to 10
5-10
6℃/sec, so on production technique, there is certain difficulty, therefore also limited the use of non-crystalline material.Electro-deposition method obtained under certain condition liquid quench method the amorphous alloy film of some composition that can not obtain.But the bath temperature that this electro-deposition method uses requires more than 60 ℃, the deposition process conditions harshness.
The objective of the invention is to propose a kind of extraordinary plating bath, it can use the method for conventional brush plating to obtain amorphous alloy coating under normal temperature condition, thereby has simplified processing method greatly.
Invention is achieved in that a kind of cobalt-nickel-phosphorus non-crystalline alloy plating bath and coating, add the non-crystaline amorphous metal series that the 10-30% metalloid forms with magnesium-yttrium-transition metal cobalt, nickel, its plating bath is to be that base contains metalloid element phosphorus as main salt with cobalt, nickelalloy, it is the supply source of bivalent nickel ion and cobalt ion, simultaneously also be the conducting salt in the solution, with H
3PO
3As buffer reagent, auxiliary salt is as stablizer, and the aqueous solution of niobium additive; The standard potential difference of cobalt-nickel uses cobalt-nickel-phosphor alloy plating bath to carry out conventional brush plating under normal temperature condition less than 30mv, makes corresponding metal ion Co in the acidic aqueous solution
++, Ni
++P separates out on negative electrode jointly with the metalloid ion.Plating bath proportioning (weight ratio) is: NiSO
47H
2O10-25%, CoSO
4.7H
2O 2-18%, H
3PO
3: 1-2%, NiCl
26H
2O:2-6%, Na
3PO
412H
2O:2-10%, H
3PO
4: 3-6%, N
bAdditive: 1-3%, H
2O is some, and the plating bath pH value is 1.5, brushing plating voltage 11-13V.
Use plating bath of the present invention, under normal temperature condition, use the alloy layer that conventional brush plating method can obtain having amorphous structure.Its characteristics:
1, it is non-crystal structure under normal temperature condition, under higher temperature conditions since coating in grain refining, the stress that the surface crystallization layer produces the non-crystallized layer in inside and separate out second acting in conjunction that forms dispersion-strengthened mutually and produce one strengthening mechanism, make the microhardness of coating increase, thereby make coating have excellent high temperature resistance polishing machine, on hot-forging die and cold-punching mould, use, can receive good effect
2, co-based alloy coating is except that having high wear resistance, also has very low frictional coefficient, because cobalt-base alloy can reduce the solid mutual solubility of workpiece and pressing mold, in the time of 200 ℃, has only 5% dissolved ferric iron in cobalt, so can reduce adhesive attraction, the mould of coating cobalt-base alloy coating can twice the life.
3, when temperature is 500 ℃, the wear resisting property of amorphous alloy coating is 2.31 times of nickel-tungsten (50) alloy layer.
4, cobalt, nickel, phosphorus amorphous alloy coating; because its crystallization temperature is higher to be 323.4 ℃; in working temperature during in 300 ℃; can keep amorphous structure; so possess very good mechanical properties and the corrosion resistance that amorphous structure has under 300 ℃ of temperature condition being lower than; can be applied to the reparation of component easy to wear widely, suffer the corrosionproof protection of heavy corrosion parts.
Fig. 1: the differential thermal analysis curve (DAT curve) of cobalt-nickel-No. 1 amorphous alloy coating of phosphorus.
Fig. 2: the differential thermal analysis curve (in plating bath, mixing the niobium additive) of cobalt-nickel-No. 2 amorphous alloy coatings of phosphorus.
Fig. 3: the X-ray diffraction result of cobalt-nickel-No. 2 amorphous alloy coatings of phosphorus.
Fig. 3 a-thermal treatment temp is 150 ℃ X-ray diffraction result.
Fig. 3 b-thermal treatment temp is 300 ℃ X-ray diffraction result.
Fig. 3 c-thermal treatment temp is 400 ℃ X-ray diffraction result.
Fig. 3 d-thermal treatment temp is 450 ℃ X-ray diffraction result.
Fig. 3 e-thermal treatment temp is 500 ℃ X-ray diffraction result.
Fig. 3 f-thermal treatment temp is 600 ℃ X-ray diffraction result.
Fig. 4: cobalt-nickel-microhardness of No. 2 amorphous alloy coatings of phosphorus and the relation curve between the thermal treatment temp.
Fig. 5: the volume wear of Co-Ni-P2 amorphous alloy coating and the variation between the thermal treatment temp.
Fig. 6: under the different heat treatment temperature, Co-Ni-P2 amorphous alloy coating and Ni-W(50) relative wear resistance of alloy layer relatively.
Fig. 6 A-normal temperature condition;
Fig. 6 B-hot conditions.
Fig. 7: Co-Ni-P2 amorphous alloy coating and Ni-W(50) the SEI photo of alloy layer before high temperature wear.
Fig. 7 A: not the surface topography of the Co-Ni-P2 alloy layer of experience wear and vertical section (400 ℃, 500 ℃).
Fig. 7 B: (400 ℃ of the surface topography of the Co-Ni-P2 alloy layer after the wearing and tearing and vertical sections.500℃）。
Fig. 7 C: the Ni-W(50 of experience wear not) surface topography and vertical section (500 ℃) of alloy layer.
Fig. 7 D: the Ni-W(50 after the wearing and tearing) surface topography of alloy layer and vertical section (500 ℃)
Fig. 8: Co-Ni-P2 amorphous alloy coating and Ni-W(50) alloy layer high temperature wear surface topography.
Fig. 9: the surperficial composition of Co-Ni-P2 amorphous alloy coating.
Figure 10: Co-Ni-P2 number (no N
bAdditive) surface composition of mixed crystal alloy layer.
Figure 11: a brush plating embodiment of the present invention.
Now further narrate the excellent properties that uses alloy layer that plating bath of the present invention forms in conjunction with the accompanying drawings.
Referring to Fig. 1: the differential thermal analysis curve of Co-Ni-P1 alloy layer has three exothermic peaks, the temperature of temperature X-coordinate correspondence is respectively 251.8 ℃, 294.3 ℃ and 398.8 ℃, it is 216.8 ℃ that crystallization begins temperature, illustrates adding to pine for just reaching steady state after the Co-Ni-P1 amorphous alloy coating will experience three metastable phase transitions.
Referring to Fig. 2: the differential thermal analysis curve of Co-Ni-P2 alloy layer has two tangible exothermic peaks, corresponding temperature is respectively 331.9 ℃ and 421.5 ℃, it is 323.4 ℃ that crystallization begins temperature, explanation is in heat-processed, and the Co-Ni-P2 amorphous alloy coating just can reach steady state after will experiencing the secondary metastable phase transition.
Referring to Fig. 3: from Fig. 3 a, b as seen, thermal treatment temp is during from 150 ℃-300 ℃, coating is amorphous structure, and during according to c to 400 ℃ of Fig. 3, existing crystallization phases is separated out, can identify the fcc-Ni phase according to Fig. 3 f thermal treatment temp 600 ℃ the time, the structure of coating is fcc-Ni phase+unknown phase under this condition.
Referring to Fig. 4: the Changing Pattern that the hardness of general plating bath brushing coating raises with working temperature mostly be strengthen → strengthen again → softening, hardness has trend of rising when being heated to 100-200 ℃, when if Heating temperature surpasses 200 ℃, then coating hardness reduces, and is ruckbildung.The microhardness of Co-Ni-P2 amorphous alloy coating changes with the variation of thermal treatment temp, and thermal treatment all is incubated 30 minutes, and when temperature was lower than 300 ℃, the microhardness value of coating changed slowly.Thermal treatment temp is to crystallization temperature T
XCrystallization appears during 323.4 ℃ of ≈, further rising with temperature, the crystalline number of dies increases in the coating, grain refining, simultaneously, the coating crystallization process from the surface progressively to inner crystallization, because the surface crystallization layer has higher density (density of non-crystaline amorphous metal is than the little 1-3% of corresponding crystal alloy), can produce stress to the lower non-crystallized part of coating internal density, the effect of these two kinds of factors makes coating of the present invention that big hardness value all be arranged in the time of 400 ℃.When thermal treatment temp was higher than 500 ℃, the recrystallize of coating played a major role, and the hardness of coating reduces.
Referring to Fig. 5: with the rising of thermal treatment temp, begin slow increase during the volume wear to 250 of coating ℃, volume wear maximum in the time of 300 ℃, begin slow decline afterwards again, begin rapid increase once more after in the time of 400 ℃, reaching mnm., between its Changing Pattern and the microhardness shown in Figure 4 good corresponding relation is arranged.
Referring to Fig. 6,8: as Fig. 6 A under normal temperature condition, Co-Ni-P2 non-crystaline amorphous metal brushing coating is than Ni-W(50) the alloy brushing coating has superior wear resisting property, in the time of 400 ℃, the wear resistance of Co-Ni-P2 amorphous alloy coating is far superior to Ni-W(50) alloy layer, when thermal treatment temp is higher than 500 ℃, the wear resistance of Co-Ni-P2 amorphous alloy coating descends, not as good as Ni-W(50) alloy layer.As Fig. 6 b, the Co-Ni-P2 amorphous alloy coating also has under hot conditions than high-wearing feature, and when temperature was 500 ℃, the wear resistance of Co-Ni-P2 amorphous alloy coating was Ni-W(50) 2.31 times of alloy layer.
Referring to Fig. 7: the Co-Ni-P2 amorphous alloy coating has typical potato shape surface topography, the cross section tissue of tree ring and undulatory vertical section tissue.
Referring to Fig. 9,10: from the diagram experimental result as can be seen: the Co-Ni-P2 amorphous alloy coating (contains N
bAdditive) phosphorus content and uses the phosphorus content of the mixed crystal coating that Co-Ni-P2 plating bath (not containing the N additive) forms only to be 5.51wt% more than 6wt%, contains N in the plating bath
bThe adding of additive has influence on H significantly
3PO
3Reduction rate, make that the phosphorus content in the coating obviously improves, so that coating is changed to amorphous structure by the duplex grain structure of non-crystalline state and crystallite attitude.
Now sketch formulating of recipe of the present invention:
1, nickel salt (Ni) and cobalt salt (Co) are the main salt in the plating bath, it is the supply source of bivalent nickel ion and cobalt ion, it simultaneously also is the conducting salt in the solution, in plating bath, add muriate, the electricity that has improved plating bath is led and has been increased the spread coefficient of nickel, cobalt ion in the plating bath, makes that the limit current density value obtains improving in the electrodeposition process.
2, mineral acid is the adjustment agent of plating bath PH, also is the stablizer of plating bath pH value with advancing.
Auxiliary salt is a kind of salt of weak acid, and except the stable and buffering effect to pH value, auxiliary salt can ionization go out N in the aqueous solution, and therefore the electricity of solution being led also has certain contribution.
3, complexing agent: for d such as nickelous, cobalt, iron
3-d
8The metal ion of configuration, profit uses water as complexing agent, and the overvoltage of hydration complex ion discharge is higher, can obtain the coating of careful light.
4, additive: contain niobium (N
b) additive forms in the amorphous process at alloy electroplating bath and play an important role, it possesses thermodynamic condition in acidic aqueous solution on the one hand, might participate in certain electro-reduction process on electrode; On the other hand, contain N
bAdditive can be stablized non-crystal structure and the amorphous metal film is formed.
In the electrodeposition process of cobalt, nickel and phosphorus, cobalt and nickel cathode reductive electrode process divided for three steps carried out:
M
+++H
2O ()/() MOH
++H
+……（1）
MOH
++e (RDS)/() MOH……（2）
MOH+H
++e ()/() M+H
2O……（3）
M can replace with Ni or Co in the formula
Wherein second step was the controlled step of entire electrode process, and the cathodic reduction electrode process of phosphorous acid carries out in two steps:
H
3PO
3+2H
++2e (RDS)/() H
3PO
2+H
2O……（4）
H
3PO
2+H
++e ()/() P+2H
2O……（5）
Metal ion or their complex ion are reduced into the process of metal on negative electrode, be called metal electrodeposition, also there is the generation of Metallic Solids in it and grows up and form the process of metal plating, i.e. electrocrystallization process except the electrochemical reaction that metal ion or its complex ion take place on negative electrode.The fundamental prerequisite of the common discharge of several ions is that the deposition potential between them equates.And deposition potential is metal under this condition (metalloid) equilibrium potential and its overpotential sum, promptly
ε
Separate out=ε °+(RT)/(NF) Lna+n ... (6)
In the formula: ε °-standard potential; T-absolute temperature
The R-gas law constant; The F-faraday constant
N-participates in the electronic number a-activity of reaction; The n-overpotential
Therefore, standard potential ε °, ion(ic)activity a and overpotential n are three significant parameters of decision metal (metalloid) ion deposition potential.Co of the present invention and Ni standard potential difference are within 30mv, when they were separated out in acidic aqueous solution, both overpotentials were more approaching, changed its deposition potential by changing the suitable complexing agent of concentration and adding and a small amount of niobium additive, make it reach common discharge, realize codeposition.
Embodiment 1:Co-Ni-P
2(no N
bAdditive) alloy electroplating bath
NiSO
4·7H
2O 200-300g/l
CoSO
4·7H
2O 30-70g/l
H
3PO
320-50g/l
NiCl
26H
2O auxiliary salt 1 20-60g/l
Na
3PO
412H
2O auxiliary salt 2 100-150g/l
H
3PO
4Mineral acid 30-70g/l
Plating bath color: light green
PH 1.5
During 20 ℃ of temperature
The plating bath electricity is led 75m Ω
-1
Plating bath density: 1.287g/cm
3
Embodiment 2:Co-Ni-P
2Alloy electroplating bath on embodiment 2 bases, increases
N
bAdditive 18-20g/l
Plating bath color: grayish green
PH 1.5
During 20 ℃ of temperature
The plating bath electricity is led: 75m Ω
-1
Plating bath density: 1.297g/cm
3
Embodiment 3: referring to Figure 11, plating bath continuously flows into from tubing 1 in the cotton jacket 3 near workpiece to be plated 6, and this cotton jacket 3 is installed on the plating pen 4, contacts with the surface of workpiece to be plated 6, plating bath retrieving arrangement 5, adopt brush plating power supply, during work, workpiece to be plated 6 connects power cathode, plating pen 4 connects positive source, by tubing 1 plating bath is delivered between the graphite cathode 2 of cotton jacket 3 and plating pen 4,, obtained coating through the brush plating repeatedly of cotton jacket 3 with workpiece to be plated 6.
Claims (3)
1, a kind of cobalt-nickel-phosphorus non-crystalline alloy plating bath and coating adds the non-crystaline amorphous metal series that the 10--30% metalloid forms with magnesium-yttrium-transition metal cobalt, nickel, it is characterized in that:
A, being that base contains metalloid element phosphorus as main salt with cobalt, nickelalloy, is the supply source of bivalent nickel ion and cobalt ion, also is simultaneously the conducting salt in the solution, with H
3PO
3As buffer reagent, auxiliary salt is as stablizer, and the aqueous solution of niobium additive;
The standard potential difference of B, cobalt-nickel uses cobalt-nickel-phosphor alloy plating bath to carry out conventional brush plating under normal temperature condition less than 30mv, makes corresponding metal ion CO in the acidic aqueous solution
++, Ni
++P separates out on negative electrode jointly with the metalloid ion.
2, by the described cobalt-nickel of claim 1-phosphorus non-crystalline alloy plating bath and coating, it is characterized in that: plating bath proportioning (weight ratio) is:
NiSO
4·7H
2O 10-25%
CoSO
4·7H
2O 2-18%
H
3PO
31-2%
NiCl
2·6H
2O 2-6%
Na
3PO
4.12H
2O 2-10%
H
3PO
33-6%
N
6Additive 1-3%
H
2O is some
3, by claim 1 or 2 described cobalt-nickel-phosphorus non-crystalline alloy plating bath and coating, it is characterized in that: the plating bath pH value is 1.5, brushing plating voltage 11-13V.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89108740 CN1025056C (en) | 1989-11-24 | 1989-11-24 | Cobalt-nickel-phosphorus non-crystalline alloy plating solution and coat |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89108740 CN1025056C (en) | 1989-11-24 | 1989-11-24 | Cobalt-nickel-phosphorus non-crystalline alloy plating solution and coat |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1044680A true CN1044680A (en) | 1990-08-15 |
| CN1025056C CN1025056C (en) | 1994-06-15 |
Family
ID=4857711
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 89108740 Expired - Fee Related CN1025056C (en) | 1989-11-24 | 1989-11-24 | Cobalt-nickel-phosphorus non-crystalline alloy plating solution and coat |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1025056C (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102233698A (en) * | 2010-04-23 | 2011-11-09 | 鸿富锦精密工业（深圳）有限公司 | Surface strengthening matrix and preparation method thereof |
| CN102363341A (en) * | 2011-11-01 | 2012-02-29 | 黄光洁 | Medicinal capsule mold and making technology thereof |
| CN103074649A (en) * | 2013-01-21 | 2013-05-01 | 四川重汽王牌兴城液压件有限公司 | Method for improving corrosion resistance of cylinder barrel of mine single hydraulic prop |
| CN103911638A (en) * | 2014-04-18 | 2014-07-09 | 合鸿新材科技有限公司 | Cobalt nickel phosphorus-silicon carbide electroplating solution and electroplating method |
| CN104532304A (en) * | 2014-12-16 | 2015-04-22 | 安徽工业大学 | Welding method of metal glass |
| CN108256288A (en) * | 2018-01-18 | 2018-07-06 | 安徽工业大学 | A kind of method of Local Structure in identification non-crystaline amorphous metal |
| CN108977844A (en) * | 2017-05-31 | 2018-12-11 | 刘志红 | A kind of cobalt base amorphous alloy catalysis electrode and preparation method thereof |
| CN109023464A (en) * | 2018-07-27 | 2018-12-18 | 淮阴工学院 | Ni-based chalcogenide film of amorphous cobalt and its preparation method and application |
| CN109136889A (en) * | 2017-06-27 | 2019-01-04 | 罗奕兵 | A kind of cobalt-nickel-phosphor catalytic reactor and production method |
| CN110029376A (en) * | 2018-01-11 | 2019-07-19 | 泰科电子(上海)有限公司 | Alloy layer, workpiece and electroplate liquid |
-
1989
- 1989-11-24 CN CN 89108740 patent/CN1025056C/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102233698A (en) * | 2010-04-23 | 2011-11-09 | 鸿富锦精密工业（深圳）有限公司 | Surface strengthening matrix and preparation method thereof |
| CN102233698B (en) * | 2010-04-23 | 2014-12-10 | 鸿富锦精密工业（深圳）有限公司 | Surface strengthening matrix and preparation method thereof |
| CN102363341A (en) * | 2011-11-01 | 2012-02-29 | 黄光洁 | Medicinal capsule mold and making technology thereof |
| CN103074649A (en) * | 2013-01-21 | 2013-05-01 | 四川重汽王牌兴城液压件有限公司 | Method for improving corrosion resistance of cylinder barrel of mine single hydraulic prop |
| CN103911638A (en) * | 2014-04-18 | 2014-07-09 | 合鸿新材科技有限公司 | Cobalt nickel phosphorus-silicon carbide electroplating solution and electroplating method |
| CN104532304A (en) * | 2014-12-16 | 2015-04-22 | 安徽工业大学 | Welding method of metal glass |
| CN108977844A (en) * | 2017-05-31 | 2018-12-11 | 刘志红 | A kind of cobalt base amorphous alloy catalysis electrode and preparation method thereof |
| CN109136889A (en) * | 2017-06-27 | 2019-01-04 | 罗奕兵 | A kind of cobalt-nickel-phosphor catalytic reactor and production method |
| CN110029376A (en) * | 2018-01-11 | 2019-07-19 | 泰科电子(上海)有限公司 | Alloy layer, workpiece and electroplate liquid |
| CN108256288A (en) * | 2018-01-18 | 2018-07-06 | 安徽工业大学 | A kind of method of Local Structure in identification non-crystaline amorphous metal |
| CN109023464A (en) * | 2018-07-27 | 2018-12-18 | 淮阴工学院 | Ni-based chalcogenide film of amorphous cobalt and its preparation method and application |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1025056C (en) | 1994-06-15 |
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