CN104975326A - Preparation method for surface-electrodeposited nano rare earth modified cobalt-based composite plating layer - Google Patents
Preparation method for surface-electrodeposited nano rare earth modified cobalt-based composite plating layer Download PDFInfo
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Abstract
The invention relates to a process method for a surface-electrodeposited nano rare earth modified cobalt-based composite plating layer, wherein the method comprises the main process technology: a cobalt plate is used as an anode, and a deposited material is used as a cathode; before electroplating, firstly, the material is subjected to surface levelling, subjected to ultrasonic cleaning and oil removal in acetone and the like, and dried; a selected electroplating solution comprises the basic components of CoCl2.6H2O, H3BO3, NaCl2H25SO4 and the like; a Y2O3 nanoscale power is added to the basic electroplating solution and is subjected to dispersion treatment by magnetic stirring; in the electroplating, the current density is in a range of 200-600 mA/cm<2>, the temperature is 25-35 DEG C, and the time is 5-10 min; and finally, the nano Y2O3 modified cobalt-based composite plating layer with the thickness of 2-10 [mu]m is obtained on the material surface. In addition, the nano cobalt-based composite plating layer is continued to be treated for a certain time at the temperature of 800 DEG C, and the problem of Cr element volatilization of the composite plating layer in a water vapor environment is effectively inhibited. The method is suitable for surface treatment of parts having certain requirements on hardness, wear resistance, corrosion resistance and high temperature resistance.
Description
Technical field
The present invention relates to the surfacecti proteon of metallic substance, be specifically related to a kind of technological method of surface electrical depositing nano rare-earth modified Co base composite cladding, the object of its nano compound electroplating is mainly used in the high temperature oxidation resistance of the surface of stainless steel at raising 800 DEG C of temperature after oxide treatment, and the over-all properties such as its hardness, wear resistance, solidity to corrosion and electroconductibility, play the object of protection.
Background technology
Along with the fast development of aerospace, chemical industry, machinery and the industrial circle such as metallurgical, the requirement for material is more and more higher.But the inefficacy of material is inevitable often in the industrial production.The part surface of the work of a large amount of mechanical means and instrument or itself break down or even scrap is all caused by the frictional wear because it is in use subjected to, corrosion and fatigue or oxidation.Therefore, the structure and fuction material of development of new can, in high-parameters (as high speed, high temperature and high pressure) and the more severe medium-term and long-term steady running of Working environment, be an important direction of scientific rersearch in present material scientific domain.But consider economic factors, in most cases, can meet material that is overall and surface requirements and be difficult to find, therefore, the surface protection of research material and intensifying technology, improve life-span and the over-all properties of material, have great importance simultaneously.
Composite plating is also known as dispersion plating, that solid insoluble solid particulate homogenous is dispersed in electroplating solution, make aaerosol solution to electroplate, make solid particulate and matrix metal codeposition, thus on matrix, obtain the composite deposite of even dispersion distributed granule structure on matrix metal.In recent years, composite plating technology development is very rapid, at present in exploration with widen composite plating technology Application Areas and have very large innovation and breakthrough.Rare earth element is as the important strategic resource of one, China, and it also receives much concern at the investigation and application of field of surface technology.Rare earth element is introduced in electroplating solution and can improve plating solution performance, promotion galvanic deposit greatly and improve coating performance.The nano-composite plate prepared of electro-deposition method is adopted to have high rigidity, the advantage such as wear-resistant, corrosion-resistant and high temperature resistant.Thus on the basis of composite plating, Development of Nano-composite Plating Technoloyg has become the study hotspot in coating surface field in recent years, at present about the application of nano rare earth particle in Composite Coatings is also progressively launching.
This patent adopts composite plating technology to carry out surface modification to stainless material, has prepared the Co-Y with high rigidity, excellent abrasive resistance, solidity to corrosion, electroconductibility and high temperature oxidation resistance
2o
3nano-composite plate.In addition, stainless steel surface can be made to obtain the multifunctional membrane with thermotolerance and low-friction coefficient by this surface modifying treatment, expand the range of application of stainless material, stainless material is rised in value, has broad application prospects.Simultaneously, the cobalt-based composite deposite of the nano rare earth modification of invention can be used as the coated material of Solid Oxide Fuel Cell (SOFC) metal connector, other kinds metallic surface can also be applied to, as metallic copper, to improve the hardness of material, wear resistance, electroconductibility and high temperature oxidation resistance.
Summary of the invention
The present invention adopts cobalt as matrix metal, and cobalt coat has that high temperature oxidation resistance is good, hardness is high and the good characteristics such as wear resistance is good; Adopting novel rare-earth nano material---yttrium oxide nano particle, as rare earth nanometer particle, has excellent high light transmittance, thermotolerance, erosion resistance and high-temperature stability.By Y
2o
3nano particle is incorporated in composite plating, and Means of Electrodeposition can prepare the Co-Y of excellent combination property
2o
3nano-composite plate.
The object of the invention is the composite plating solution by providing a kind of nano rare earth modification, preparing one and there is high rigidity, low-friction coefficient, wear-resistant, corrosion-resistant and resistant to elevated temperatures composite deposite.For realizing this object, the technical solution used in the present invention detailed process is as follows:
First stainless steel sample wire is cut into the size of 1cm × 1cm × 0.5cm, on pre-mill after buffing work-piece surface removal zone of oxidation in acetone, ethanol ultrasonic cleaning, dry for standby.
Then configure base electroplate liquid, plating solution consists of: CoCl
26H
2o:100-150gL
-1, H
3bO
3: 30-60gL
-1, NaC
12h
25sO
4: 0.1-0.3gL
-1.Weigh good above material, first carry out the heating for dissolving of boric acid, then add CoCL2 6H2O and sodium lauryl sulphate, utilize magnetic stirrer to make it mix, precipitation is dissolved completely.
Then in the electroplate liquid configured, Y is added
2o
3nanometer powder (granularity is 10-40nm), utilizes magnetic stirrer 1h, nanometer powder is fully mixed, dispersed, forms aaerosol solution.
Finally adopt the parallel apparatus for placing of two electrodes to carry out galvanic deposit, cobalt plate is as anode (cobalt plate purity is greater than 99.9%), and stainless steel is as negative electrode, and while plating piece puts into electroplating solution, opening power carries out direct current electrode position immediately.In scattered plating solution, adopt constant current process to control power supply electroplate, and set corresponding time (5-10min) and current density (200-600mA/cm
2), control temperature (25-35 DEG C) in water bath equipment.The pH value scope of plating solution is 4.5-4.9, adopts the pH value of 10%HCl solution and 3.5%NaOH solution adjustment solution.After certain electroplating technology, obtain nanometer Y at stainless steel surface
2o
3the cobalt-based composite deposite of modification, thickness is 2-10 μm of scope.After having deposited, stainless steel is taken out; clean with distilled water; under 800 DEG C of argon shields, 2 hours are processed after oven dry; effectively improve coating and the stainless bonding force of matrix; and improve the performances such as the dispersion of nano particle in coating, effectively can suppress the Cr volatilization problems of matrix stainless material in water vapor.Carry out follow-up 800 DEG C of high temperature oxidations experiment, mainly for SS430 ferritic stainless steel, its composition is roughly: carbon (C) :≤0.12%, silicon (Si) :≤0.75%, manganese (Mn) :≤1.00%, phosphorus (P) :≤0.04%, sulphur (S) :≤0.03%, chromium (Cr): 16.0 ~ 18.0%.
The technology of the present invention method carries out modification to stainless steel surface, in cobalt plating solution, add Y
2o
3nano particle, by composite electric plating method at its surface electrical deposition Co-Y
2o
3nano-composite plate, has equipment simple, and operating procedure is convenient, and cost is low, power consumption is few, the advantages such as utilization rate of raw materials is higher, good process repeatability.Stainless steel surface Y after modification
2o
3nano particle distribution is comparatively even, and cohesive force is better.Y after 800 DEG C of high temperature oxidation experiments
2o
3particle and matrix metal Co are combined therebetween closely, and the defect such as Interface Crack, hole is less.Through the stainless steel of surface modification treatment, its nano surface composite deposite can provide permanently effective protection to matrix, suppresses Cr element to external diffusion, improves its high temperature oxidation resistance.
In addition, the present invention also can be applicable to the research of Solid Oxide Fuel Cell (SOFC) metal connector top coat.Adding of rare-earth yttrium element; the growth velocity of surface film oxide can not only be reduced, greatly improve the antioxidant property of metal connector alloy, the microdefect in chromic oxide protective membrane can also be made up; greatly strengthen the adsorptive power of protective membrane, and reach the effect of crystal grain thinning.
Accompanying drawing explanation
Fig. 1 is electrochemical principle schematic diagram.
Fig. 2 is SS 430 ferritic stainless steel surface modification technology schema.
Fig. 3 is the SEM surface picture (Y of direct supply nano composite galvanized coating
2o
3the addition of nano particle is 20gL
-1).
Specific implementation method:
A kind of preparation method's specific implementation process of rare-earth element modified cobalt-based nano composite galvanized coating is as follows:
Embodiment 1:
(1) SS430 ferritic stainless steel sample wire is cut into the size of 1cm × 1cm × 0.5cm, pre-mill uses 180-2000
#siC sand paper to polish step by step removal oxide layer on stainless steel surface, the then each 10min of ultrasonic cleaning in acetone, ethanol, dry for standby.
(2) configure electroplate liquid, plating solution consists of: CoCl
26H
2o:100-150gL
-1, H
3bO
3: 30-60gL
-1, NaC
12h
25sO
4: 0.1-0.3gL
-1.Weigh good above material, boric acid fully dissolves in the distilled water of boiling, and after its cooling, add CoCL2 6H2O and sodium lauryl sulphate, utilize magnetic stirrer that above material is mixed, precipitation is dissolved completely.10gL is added in the electroplate liquid configured
-1y
2o
3(granularity is 40nm to nanometer powder.And utilize magnetic stirrer 1h, make it mix, form aaerosol solution.
(3) the parallel apparatus for placing of two electrodes is adopted to carry out galvanic deposit, wherein cobalt plate is as anode (cobalt plate purity is greater than 99.9%), stainless steel is as negative electrode, in scattered plating solution, adopt constant current process to control power supply (DPS15V5A, cumulative science and technology) carry out direct current electrode position, and set corresponding time 8min and current density 400mA/cm
2, control temperature 25 DEG C in water bath equipment).The pH value scope of plating solution is 4.5, adopts 10%HCl to adjust the pH value of solution.After certain electroplating technology, obtain nanometer Y at stainless steel surface
2o
3the cobalt-based composite deposite of modification, thickness is 6 μm of scopes.After having deposited, stainless steel plating piece is taken out, with distilled water cleaning, the Co-Y that bonding force is good, be evenly distributed after oven dry, can be obtained
2o
3nano-composite plate.
(4) composite deposite of the nano rare earth modification obtained is continued to process 2 hours under 800 DEG C of argon shields; effectively improve coating and the stainless bonding force of matrix; and improve the performances such as the dispersion of nano particle in coating, effectively can suppress the Cr volatilization problems of matrix stainless material in water vapor.The high temperature oxidation experiment at 800 DEG C of temperature is carried out subsequently in high temperature process furnances.
Embodiment 2:
(1) SS430 ferritic stainless steel sample wire is cut into the size of 1cm × 1cm × 0.5cm, pre-mill uses 180-2000
#siC sand paper to polish step by step removal oxide layer on stainless steel surface, the then each 10min of ultrasonic cleaning in acetone, ethanol, dry for standby.
(2) configure electroplate liquid, plating solution consists of: CoCl
26H
2o:100-150gL
-1, H
3bO
3: 30-60gL
-1, NaC
12h
25sO
4: 0.1-0.3gL
-1.Weigh good above material, boric acid fully dissolves in the distilled water of boiling, and after its cooling, add CoCL2 6H2O and sodium lauryl sulphate, utilize magnetic stirrer that above material is mixed, precipitation is dissolved completely.20gL is added in the electroplate liquid configured
-1y
2o
3(granularity is 40nm to nanometer powder.And utilize magnetic stirrer 1h, make it mix, form aaerosol solution.
(3) the parallel apparatus for placing of two electrodes is adopted to carry out galvanic deposit, wherein cobalt plate is as anode (cobalt plate purity is greater than 99.9%), stainless steel is as negative electrode, in scattered plating solution, adopt constant current process to control power supply (DPS15V5A, cumulative science and technology) carry out direct current electrode position, and set corresponding time 10min and current density 600mA/cm
2, control temperature 35 DEG C in water bath equipment.The pH value scope of plating solution is 4.9, adopts 10%HCl to adjust the pH value of solution.After certain electroplating technology, obtain nanometer Y at stainless steel surface
2o
3the cobalt-based composite deposite of modification, thickness is 10 μm of scopes.After having deposited, stainless steel plating piece is taken out, with distilled water cleaning, the Co-Y that bonding force is good, be evenly distributed after oven dry, can be obtained
2o
3nano-composite plate.
(4) composite deposite of the nano rare earth modification obtained is continued to process 2 hours under 800 DEG C of argon shields; effectively improve coating and the stainless bonding force of matrix; and improve the performances such as the dispersion of nano particle in coating, effectively can suppress the Cr volatilization problems of matrix stainless material in water vapor.The high temperature oxidation experiment at 800 DEG C of temperature is carried out subsequently in high temperature process furnances.
Embodiment 3:
(1) SS430 ferritic stainless steel sample wire is cut into the size of 1cm × 1cm × 0.5cm, pre-mill uses 180-2000
#siC sand paper to polish step by step removal oxide layer on stainless steel surface, the then each 10min of ultrasonic cleaning in acetone, ethanol, dry for standby.
(2) configure electroplate liquid, plating solution consists of: CoCl
26H
2o:100-150gL
-1, H
3bO
3: 30-60gL
-1, NaC
12h
25sO
4: 0.1-0.3gL
-1.Weigh good above material, boric acid fully dissolves in the distilled water of boiling, and after its cooling, add CoCL2 6H2O and sodium lauryl sulphate, utilize magnetic stirrer that above material is mixed, precipitation is dissolved completely.30gL is added in the electroplate liquid configured
-1y
2o
3nanometer powder (granularity is 10-40nm).And utilize magnetic stirrer 1h, make it mix, form aaerosol solution.
(3) the parallel apparatus for placing of two electrodes is adopted to carry out galvanic deposit, wherein cobalt plate is as anode (cobalt plate purity is greater than 99.9%), stainless steel is as negative electrode, in scattered plating solution, adopt constant current process to control power supply (DPS15V5A, cumulative science and technology) carry out direct current electrode position, and set corresponding time (5min) and current density (200mA/cm
2), control temperature (25 DEG C) in water bath equipment.The pH value scope of plating solution is 4.5-4.9, adopts 10%HCl to adjust the pH value of solution.After certain electroplating technology, obtain nanometer Y at stainless steel surface
2o
3the cobalt-based composite deposite of modification, thickness is 3 μm of scopes.After having deposited, stainless steel plating piece is taken out, with distilled water cleaning, the Co-Y that bonding force is good, be evenly distributed after oven dry, can be obtained
2o
3nano-composite plate.
(4) composite deposite of the nano rare earth modification obtained is continued to process 2 hours under 800 DEG C of argon shields; effectively improve coating and the stainless bonding force of matrix; and improve the performances such as the dispersion of nano particle in coating, effectively can suppress the Cr volatilization problems of matrix stainless material in water vapor.The high temperature oxidation experiment at 800 DEG C of temperature is carried out subsequently in high temperature process furnances.
Embodiment 4:
(1) SS430 ferritic stainless steel sample wire is cut into the size of 1cm × 1cm × 0.5cm, pre-mill uses 180-2000
#siC sand paper to polish step by step removal oxide layer on stainless steel surface, the then each 10min of ultrasonic cleaning in acetone, ethanol, dry for standby.
(2) configure electroplate liquid, plating solution consists of: CoCl
26H
2o:100-150gL
-1, H
3bO
3: 30-60gL
-1, NaC
12h
25sO
4: 0.1-0.3gL
-1.Weigh good above material, boric acid fully dissolves in the distilled water of boiling, and after its cooling, add CoCL2 6H2O and sodium lauryl sulphate, utilize magnetic stirrer that above material is mixed, precipitation is dissolved completely.40gL is added in the electroplate liquid configured
-1y
2o
3nanometer powder (granularity is 10-40nm).And utilize magnetic stirrer 1h, make it mix, form aaerosol solution.
(3) the parallel apparatus for placing of two electrodes is adopted to carry out galvanic deposit, wherein cobalt plate is as anode (cobalt plate purity is greater than 99.9%), stainless steel is as negative electrode, in scattered plating solution, adopt constant current process to control power supply (DPS15V5A, cumulative science and technology) carry out direct current electrode position, and set corresponding time (7min) and current density (500mA/cm
2), control temperature (30 DEG C) in water bath equipment.The pH value scope of plating solution is 4.7, adopts the pH value of 10%HCl solution and 3.5%NaOH solution adjustment solution.After certain electroplating technology, obtain nanometer Y at stainless steel surface
2o
3the cobalt-based composite deposite of modification, thickness is 7 μm of scopes.After having deposited, stainless steel plating piece is taken out, with distilled water cleaning, the Co-Y that bonding force is good, be evenly distributed after oven dry, can be obtained
2o
3nano-composite plate.
The composite deposite of the nano rare earth modification obtained is continued to process 2 hours under 800 DEG C of argon shields; effectively improve coating and the stainless bonding force of matrix; and improve the performances such as the dispersion of nano particle in coating, effectively can suppress the Cr volatilization problems of matrix stainless material in water vapor.The high temperature oxidation experiment at 800 DEG C of temperature is carried out subsequently in high temperature process furnances.
Claims (8)
1. the present invention is about a kind of preparation method of surface electrical depositing nano rare-earth modified Co base composite cladding, and its processing step is:
Step 1: size stainless steel sample wire being cut into 1cm × 1cm × 0.5cm, on pre-mill after buffing work-piece surface removal zone of oxidation in acetone, ethanol ultrasonic cleaning, dry for standby.
Step 2: configure base electroplate liquid, plating solution consists of: CoCl
26H
2o:100-150gL
-1; H
3bO
3: 30-60gL
-1; NaC
12h
25sO
4: 0.1-0.3gL
-1.Weigh good above material, first carry out the heating for dissolving of boric acid, then add CoCL2 6H2O and sodium lauryl sulphate, utilize magnetic stirrer to make it be uniformly dispersed, precipitation is dissolved completely.
Step 3: add proper amount of nano Y in the basic electroplate liquid configured
2o
3utilize magnetic stirrer 1h after powder, nanometer powder fully mixed, dispersed, form aaerosol solution.
Step 4: adopt the parallel apparatus for placing of two electrodes to carry out galvanic deposit, wherein cobalt plate is as anode (cobalt plate purity is greater than 99.9%), stainless steel is as negative electrode, in scattered plating solution, adopt constant current process to control power supply electroplate, and set corresponding time (5-10min) and current density (200-600mA/cm
2), control temperature (25-35 DEG C) in water bath equipment.After certain electroplating technology, obtain nanometer Y at stainless steel surface
2o
3the cobalt-based composite deposite of modification, thickness is 2-10 μm of scope.
Step 5: the composite deposite of the nano rare earth modification obtained in step 4 is continued to process 2 hours under 800 DEG C of argon shields; effectively improve coating and the stainless bonding force of matrix; and improve the performances such as the dispersion of nano particle in coating, effectively can suppress the Cr volatilization problems of matrix stainless material in water vapor.
2. according to the preparation method of the surface electrical depositing nano rare-earth modified Co base composite cladding described in claims 1, it is characterized in that: carry out galvanic deposit mainly for SS430 ferritic stainless steel, the stainless composition of its SS430 is roughly: carbon (C) :≤0.12%, silicon (Si) :≤0.75%, manganese (Mn) :≤1.00%, phosphorus (P) :≤0.04%, sulphur (S) :≤0.03%, chromium (Cr): 16.0 ~ 18.0%.
3. according to the preparation method of the surface electrical depositing nano rare-earth modified Co base composite cladding described in claims 1, it is characterized in that: in step 1, the first Linear cut of stainless steel sample becomes the size of 1cm × 1cm × 0.5cm, and pre-mill passes through 180-2000
#sand papering to workpiece surface removes zone of oxidation and light, after ultrasonic cleaning after 10 minutes in acetone, then after the greasy dirt continuing to remove surface after EtOH Sonicate ripple cleans 10 minutes, drying for standby.
4., according to the preparation method of the surface electrical depositing nano rare-earth modified Co base composite cladding described in claims 1, it is characterized in that: in step 2, configure base electroplate liquid consists of: CoCl
26H
2o:100-150gL
-1; H
3bO
3: 30-60gL
-1; NaC
12h
25sO
4: 0.1-0.3gL
-1.Configure corresponding electroplate liquid composition, the heating for dissolving process of boric acid is first carried out after 10-15 minute in layoutprocedure, when solution presents aqueous solution feature, add CoCL2 6H2O and sodium lauryl sulphate more simultaneously, utilize magnetic stirrer to make it be uniformly dispersed, precipitation is dissolved completely.
5., according to the preparation method of the surface electrical depositing nano rare-earth modified Co base composite cladding described in claims 1, it is characterized in that: in step 3, in the basic electroplate liquid configured, add 10-40gL
-1nanometer Y
2o
3powder, nanometer Y
2o
3the granularity of powder is 10-40nm.And utilize magnetic stirrer 1h, and nanometer powder is fully mixed, dispersed, form aaerosol solution.After certain electroplating technology, obtain nanometer Y at stainless steel surface
2o
3the cobalt-based composite deposite of modification, thickness is 2-10 μm of scope.
6. according to the preparation method of the surface electrical depositing nano rare-earth modified Co base composite cladding described in claims 1, it is characterized in that: in step 4, adopt the parallel apparatus for placing of two electrodes to carry out galvanic deposit, wherein cobalt plate is as anode (cobalt plate purity is greater than 99.9%), and stainless steel is as negative electrode.
7. according to the preparation method of the surface electrical depositing nano rare-earth modified Co base composite cladding described in claims 1, it is characterized in that: in step 4, nano compound electroplating adopts digital power, in scattered plating solution, adopt constant current process to control power supply electroplate, and set corresponding time (5-10min) and current density (200-600mA/cm
2), control temperature (25-35 DEG C) in water bath equipment.The pH value scope of plating solution is 4.5-4.9, adopts the pH value of 10%HCl solution and 3.5%NaOH solution adjustment solution.
8. according to the preparation method of the surface electrical depositing nano rare-earth modified Co base composite cladding described in claims 1; it is characterized in that: the composite deposite of the nano rare earth modification obtained in step 5 continues to process 2 hours under 800 DEG C of argon shields; effectively improve coating and the stainless bonding force of matrix; and improve the performances such as the dispersion of nano particle in coating, effectively can suppress the Cr volatilization problems of matrix stainless material in water vapor.
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| CN105332010A (en) * | 2015-11-18 | 2016-02-17 | 常州大学 | Preparation method of pulse electrodeposition Co/Y2O3 nanometer composite plating layer |
| CN108411345A (en) * | 2018-04-28 | 2018-08-17 | 邹峰 | A kind of preparation method of high temperature resistant coating |
| CN112226805A (en) * | 2020-10-26 | 2021-01-15 | 矿冶科技集团有限公司 | Preparation method of electrodeposited cobalt-based composite coating |
| CN115110125A (en) * | 2022-06-21 | 2022-09-27 | 西安建筑科技大学 | A composition containing nanometer Y 2 O 3 Corrosion-resistant super-hydrophobic composite material of particles and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105332010A (en) * | 2015-11-18 | 2016-02-17 | 常州大学 | Preparation method of pulse electrodeposition Co/Y2O3 nanometer composite plating layer |
| CN108411345A (en) * | 2018-04-28 | 2018-08-17 | 邹峰 | A kind of preparation method of high temperature resistant coating |
| CN112226805A (en) * | 2020-10-26 | 2021-01-15 | 矿冶科技集团有限公司 | Preparation method of electrodeposited cobalt-based composite coating |
| CN115110125A (en) * | 2022-06-21 | 2022-09-27 | 西安建筑科技大学 | A composition containing nanometer Y 2 O 3 Corrosion-resistant super-hydrophobic composite material of particles and preparation method thereof |
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| CN104975326B (en) | 2017-10-24 |
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