CN109943872A - It is a kind of for melting the preparation method for the composite coating that stainless steel containing Cr in fluoride salt protects - Google Patents
It is a kind of for melting the preparation method for the composite coating that stainless steel containing Cr in fluoride salt protects Download PDFInfo
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Abstract
The invention discloses a kind of for melting the preparation method for the composite coating that stainless steel containing Cr protects in fluoride salt, and this method comprises the following steps: 1) selecting stainless steel as cathode substrate, select nickel sheet as anode base material；2) anode and cathode substrate is placed in nano compound electroplating slot, and carries out nano combined pulse plating in stirring, prepare Ni (NiO) transition zone；3) above-mentioned substrate is stirred nickel plating in bright nickel plating slot；4) above-mentioned substrate is placed into the container full of inert gas shielding and is heat-treated, 850~900 DEG C of the temperature of heat treatment, time 8h react the Cr in substrate with the NiO in transition zone, and then surface in situ grows Cr2O3Diffusion barrier.The method of the present invention is easy to operate, and coating controllability is high, favorable anti-corrosion effect, reduces electroplating time, and the additive of plating solution is few, facilitates to reduce the pollution to environment while reducing cost, and the coating compactness and binding force that prepare are good.
Description
Technical field
It is specifically a kind of stainless containing Cr in fluoride salt for melting the invention belongs to technical field of metal material surface treatment
The preparation method of the composite coating of steel protection.
Background technique
Melting fluoride salt is that a kind of new type high temperature and high heat flux density pass heat storage medium, has high heat capacity, high-melting-point, high fever
Unique ermal physics and the thermochemistries such as conductance, high irradiation stability, low neutron-capture cross section, low saturated vapor pressure and low viscosity
Matter is now widely used for hot industry field.However, molten fluoride has very strong corrosivity at high temperature.It is using
When relevant device or system, the activity that metallic element easily occurs in the fluoride of high-temperature molten-state for metallic based structures material is molten
Solution, significantly reduces the service life of material, this is also one of the major obstacle of industrial applications for restricting melting fluoride salt.In recent years
Come, with the development of the technologies such as fused salt pile, spentnuclear fuel post-processing, fuse salt heat accumulating, molten fluoride etching problem by
To extensive concern.It is Ni-based for the low Cr containing Mo of representative with Hastelloy N alloy (main component is Ni-7Cr-16Mo-5Fe)
Alloy is typically considered to have preferable anti-fluoride corrosion performance, but due to active element selective corrosion when longtime running,
Such alloy still not can avoid to form Cr depletion zone and hole.
Currently, the general Cr inhibited in matrix alloy using the method for applying diffusion barrier between Ni coating and matrix alloy
Equal elements external diffusion, is remarkably improved the resist melt fluoride corrosion performance of Ni coating.Ceramic diffusion barrier is extended out in inhibition element
Dissipating aspect has some superiority.Oxide ceramics diffusion barrier generally using pre-oxidize the methods of thermally grown method, in situ synthesis into
Row preparation.Existing research personnel are prepared for oxide diffusion barrier using in situ synthesis between cold spraying coating and matrix, but
It finds that the binding force between the coating and matrix under cold spray process is poor again, causes the diffusion barrier microdefect of subsequent preparation can not
It avoids, element counterdiffusion cannot be stopped completely during coating long service.
Summary of the invention
It is answered technical problem to be solved by the invention is to provide a kind of for melt that stainless steel containing Cr in fluoride salt protects
Close coating preparation method, this method using pulse composite plating prepare Ni (NiO) transition zone, subsequent pulse plating Ni coating,
Handling finally by high-temperature vacuum appropriate makes matrix alloy surface in situ grow Cr2O3Diffusion barrier, finally obtain it is continuous fine and close and
The Cr being well combined with matrix2O3/ Ni composite coating.
The present invention solves above-mentioned technical problem with following technical solution:
The present invention is a kind of for melting the preparation method for the composite coating that stainless steel containing Cr in fluoride salt protects, including following
Step:
1) substrate pre-processes: selecting stainless steel as cathode substrate, nickel sheet is anode base material, the size and stainless steel of nickel sheet
The sizableness of cathode substrate, and cathode and anode base material are pre-processed, pretreatment refers to substrate surface polishing, falls
Angle, oil removing, washing, activation, again washing process；
2) nano compound electroplating prepares Ni (NiO) transition zone: pretreated anode and cathode substrate being placed on nano combined
In electroplating bath, and carry out nano combined pulse plating Ni (NiO) transition zone in stirring, in the every 1L of required electroplate liquid containing with
Lower component: hydration nickel sulfate 250g, hydrated nickel chloride 40g, boric acid 40g, lauryl sodium sulfate 0.3g, nickel oxide powder 20~
100g, remaining is deionized water；Pulse plating condition are as follows: average current density is 6~8A/dm2, plating solution pH is 3.5, when plating
Temperature be 50~55 DEG C, frequency be 100~500Hz, total duty ratio be 70~80%, electroplating time 300s；
3) outer layer nickel is electroplated: by it is above-mentioned through nano compound electroplating Ni (NiO) transition zone treated substrate in bright nickel plating
It is stirred nickel plating in slot, contains following components in the every 1L of required plating solution: hydration nickel sulfate 250g, hydrated nickel chloride 40g, boron
Sour 40g, lauryl sodium sulfate 0.3g, saccharin sodium 1g, remaining is deionized water；Plating conditions: average current density is
3.5A/dm2, plating solution pH is 4.5, and temperature when plating is 45 DEG C, frequency 50Hz, and total duty ratio is 40%, and wherein forward direction accounts for
Sky is than being 36%, electroplating time 300s；
4) be heat-treated: by above-mentioned electroplated outer layer nickel, treated that substrate is placed into the container of inert gas shielding carries out
The temperature of heat treatment, heat treatment is 850~900 DEG C, time 8h, reacts the Cr in substrate with the NiO in transition zone, Jin Erbiao
Face growth in situ goes out Cr2O3Diffusion barrier is to get to for melting the Cr that stainless steel containing Cr protects in fluoride salt2O3The compound painting of/Ni
Layer.
In step 1), the stainless steel selects 316L stainless steel, and is cut into the thin slice of 15 × 10 × 2mm.
In step 1), the oil removing in the pretreatment is to be put into substrate in acetone soln and surpass in ultrasonic cleaner
Sound 3~5 minutes, the temperature of ultrasonic cleaning was room temperature.
In step 1), the activating solution of use is activated in the pretreatment by hydrochloric acid, sulfuric acid and deionized water by quality
Than being mixed for 2:4:2, activation temperature uses room temperature, and activation time is 15 seconds, and the substrate after activation uses deionized water again
Cleaning, is then quickly put into electroplating bath.
In step 1), 150 mesh and 600 mesh sand paper are respectively adopted in polishing and chamfering in the pretreatment.
In step 2), the partial size of nickel oxide powder employed in the nano compound electroplating is 50nm.
In step 2), for the inert gas used in the heat treatment process for high-purity argon gas, container is quartz ampoule.
In step 2), the agitating mode used in the nano compound electroplating is magnetic agitation mode, revolving speed 550rpm.
In step 2), after the electroplate liquid preparation for 24 hours through ultrasonic disperse, to obtain the more uniform nano-powder plating of dispersion
Liquid.
The method of the present invention has the following beneficial effects:
1) NiO nano particle is used in composite plating plating solution of the invention, which is added in electroplating solution
With metal co-deposition, Ni (NiO) composite deposite has been obtained.Since pulse plating is to the higher controllability of coating, form thin
Crystal structure reduces plating layer porosity, the smooth densification of coating surface；And electroplating time while reaching required thickness of coating
It is greatly reduced.
2) when the method for the present invention uses bright nickel plating technique, additive types are less, reduce manual operation intensity, and be electroplated
Time is short, improves production efficiency, while reducing the pollution to environment to a certain extent, has reached the mesh of green production
's.
3) the reverse impulse composite plating technology that the present invention uses, deposition efficiency is high, sedimentary even compact and internal stress
It is low, it can be prepared under low temperature and normal pressure, it is easy to operate.It, can be by adjusting pulse when carrying out nano-composite plate plating
Deposition parameter accurately controls the microstructure of coating and nickel layer, object phase constituent and thickness etc..When carrying out nickel plating, can also adopt
With higher current density, plating efficiencies are improved, obtain the better coating of performance.
4) high current density for the pulse composite plating that the present invention uses accelerates deposition velocity, simultaneously as duty ratio
In the presence of it is namely certain open, the disconnected time, provide the particle of abundance for cathode, nickel deposition velocity and nanoparticle on cathode
Deposition velocity it is suitable, it is available have even compact, the tiny Ni-NiO composite deposite of particle.
5) Ni (NiO) Pulse composite coating prepared by the present invention passes through subsequent heat treatment technique, can occur with substrate in situ
Reaction, makes growth in situ between substrate and Ni coating go out Cr2O3Diffusion barrier, the composite coating and basal body binding force of this method preparation
It is good.
Detailed description of the invention
Fig. 1 is the surface scan electron microscope of the composite coating of the embodiment of the present invention 1.
Fig. 2 is the surface scan electron microscope of the composite coating of the embodiment of the present invention 2.
Specific embodiment
Technical solution of the present invention is described in further detail with reference to the accompanying drawing.
The present invention is a kind of for melting the preparation method for the composite coating that stainless steel containing Cr protects in fluoride salt, concrete technology
Process is as follows:
1) substrate pre-processes: selecting stainless steel as cathode substrate, nickel sheet is anode base material, the size and stainless steel of nickel sheet
The sizableness of cathode substrate, and cathode and anode base material are pre-processed, pretreatment refers to substrate surface polishing, falls
Angle, oil removing, washing, activation, again washing process.
The stainless steel selects 316L stainless steel, and is cut into the thin slice of 15 × 10 × 2mm.
Polishing and chamfering are carried out to substrate using 150 mesh and 600 mesh sand paper, to obtain the substrate surface of continuous formation,
The binding force between substrate and coating can be improved when subsequent plating.
The activating solution used is activated in the pretreatment by hydrochloric acid, sulfuric acid and deionized water in mass ratio for 2:4:2
It is mixed, activation temperature uses room temperature, and activation time is 15 seconds, and the substrate after activation is cleaned with deionized water again, then
Quickly it is put into electroplating bath.
Oil removing in the pretreatment be substrate is put into acetone soln and in ultrasonic cleaner ultrasound 3~5 points
Clock, the temperature of ultrasonic cleaning are room temperature.
2) nano compound electroplating Ni (NiO) transition zone: yin-yang the two poles of the earth material is fixed in electroplating bath, and the two is put in parallel
It sets, apart from moderate, electroplating bath can be replaced with the beaker of 200ml, and nano combined pulse plating is then carried out in stirring, required
Contain following components in the every 1L of electroplate liquid: hydration nickel sulfate 250g, hydrated nickel chloride 40g, boric acid 40g, lauryl sodium sulfate
0.3g, 20~100g of nickel oxide powder, remaining is deionized water；Pulse plating condition are as follows: average current density is 6~8A/dm2,
Plating solution pH is 3.5, and temperature when plating is 50~55 DEG C, and frequency is 100~500Hz, and total duty ratio is 70~80%, plating
Time is 300s.
The partial size of nickel oxide powder employed in the nano compound electroplating is 50nm, the uniqueness that nano-powder has by it
Physicochemical property, the performance of composite deposite can be substantially improved.
The agitating mode used in the nano compound electroplating is magnetic agitation mode, and revolving speed 550rpm not only guarantees
Nano particle is evenly dispersed in the plating solution when plating, also ensures uniform deposition of the nano particle in coating.
The electroplate liquid needs after preparing through ultrasonic disperse for 24 hours, disperses more uniform nano-powder plating solution to obtain.
3) outer layer nickel is electroplated: by it is above-mentioned through nano compound electroplating Ni (NiO) transition zone treated substrate in bright nickel plating
It is stirred nickel plating in slot, contains following components in the every 1L of required plating solution: hydration nickel sulfate 250g, hydrated nickel chloride 40g, boron
Sour 40g, lauryl sodium sulfate 0.3g, saccharin sodium 1g, remaining is deionized water；Plating conditions: average current density is
3.5A/dm2, plating solution pH is 4.5, and temperature when plating is 45 DEG C, frequency 50Hz, and total duty ratio is 40%, and wherein forward direction accounts for
Sky is than being 36%, electroplating time 300s；
At the end of plating with deionized water rinse coating, after flushing electricity consumption blowing drying (blown with cold wind, will not be in coating table
Face leaves water stain), to obtain clean coating surface.
4) it is heat-treated: treated the substrate sealing of above-mentioned electroplated outer layer nickel is placed into the container of inert gas shielding
It is interior, it is subsequently placed at Muffle furnace and is heat-treated, or be put into vacuum tube furnace, carry out hot place after being subsequently passed inert gas
The temperature of reason, heat treatment is 850~900 DEG C, time 8h, and substrate surface is made to grow Cr2O3Diffusion barrier is to get to for melting
The composite coating that stainless steel containing Cr protects in fluoride salt.
For the inert gas used in the heat treatment process for high-purity argon gas, the container is quartz ampoule.
Stainless steel surface prepare one layer it is continuous fine and close, with matrix alloy and the anti-corrosion good diffusion of Ni layers of binding performance
Barrier is the key that prepare the coating of resistance to molten fluoride, and the chemical bonding between oxide coating and matrix can significantly improve oxide
With matrix adhesiveness.The present invention prepares Ni-NiO transition zone, subsequent pulse plating Ni coating using pulse composite plating, and passes through
High-temperature vacuum processing appropriate makes matrix alloy surface in situ grow Cr2O3Diffusion barrier, finally obtain it is continuous fine and close and with matrix knot
Close good Cr2O3/ Ni composite coating.
It is the embodiment of the present invention below:
Embodiment 1
The stainless steel (ingredient is shown in Table one) for being about 16wt.% with amount containing Cr cuts stainless steel cathode substrate for cathode substrate
It is cut into 15 × 10 × 2mm thin slice, using nickel sheet as anode base material, the size of nickel sheet and the sizableness of stainless steel cathode substrate, and
Cathode and anode base material are pre-processed, i.e., it is sour again after deionized water cleaning with acetone ultrasound oil removing after polishing, chamfering
Change, is finally rinsed again.Scattered plating solution (plating solution containing NiO nano particle (50nm) is put it into later
Contain following components in every 1L: hydration nickel sulfate 250g, hydrated nickel chloride 40g, boric acid 40g, lauryl sodium sulfate 0.3g, oxygen
Change nickel powder 20g, remaining is deionized water) in be electroplated.Power supply be adjustable dual-pulse power supply, the pulse frequency used for
100Hz, average current density 6A/dm2, bath temperature is 50 DEG C, and total duty ratio is 70%, the mixing speed in electroplating process
It is 3.5 for 550rpm, plating solution pH, electroplating time 300s.There is the sample of 1 micron of thick nano-composite plate to be put into electro-deposition
Carry out plating outer layer Ni in plating Ni liquid, contain following components in the every 1L of the plating solution: hydration nickel sulfate 250g, hydrated nickel chloride 40g,
Boric acid 40g, lauryl sodium sulfate 0.3g, saccharin sodium 1g, remaining is deionized water.Power supply is adjustable dual-pulse power supply, is used
Average current density be 3.5A/dm2, plating solution pH is 4.5, and temperature when plating is 45 DEG C, frequency 50Hz, and total duty ratio is
40%, wherein positive duty ratio is 36%, electroplating time 300s.The sample wash that plating is completed completely dries up later, connects
Sample is sealed in the quartz ampoule full of high-purity argon gas again, then put it into Muffle furnace, through 900 DEG C, 8h heat at
Reason process is obtained containing Cr2O3Diffusion barrier and anti-corrosion Ni layers of oxide composite coating.Obtained oxide diffusion barrier Cross Section Morphology is such as
Shown in Fig. 1.Outer boundary disappears in anticorrosion layer after heat treatment, and generating continuous, average thickness at interior outer boundary is about 1
The oxide of micron.Sample is scanned using power spectrum, the main component of obtained oxide composite coating is shown in Table two (Fig. 1
Middle mark part).It can be obtained in conjunction with elemental line scan and element distribution analysis result, oxide diffusion barrier is mainly by rich Cr oxide
Composition.
Table one
Table two
Embodiment 2
The stainless steel (ingredient is shown in Table one) for being about 16wt.% with amount containing Cr cuts stainless steel cathode substrate for cathode substrate
It is cut into 15 × 10 × 2mm thin slice, using nickel sheet as anode base material, the size of nickel sheet and the sizableness of stainless steel cathode substrate, and
Cathode and anode base material are pre-processed, i.e., after polishing, chamfering, acetone ultrasound oil removing is acidified again after deionized water cleaning,
Finally it is rinsed again.Scattered plating solution (the every 1L of the plating solution containing NiO nano particle (50nm) is put it into later
In contain following components: hydration nickel sulfate 250g, hydrated nickel chloride 40g, boric acid 40g, lauryl sodium sulfate 0.3g, nickel oxide
Powder 100g, remaining is deionized water) in be electroplated.Power supply be adjustable dual-pulse power supply, the pulse frequency used for 500Hz,
Average current density is 8A/dm2, bath temperature is 55 DEG C, and total duty ratio is 80%, and the mixing speed in electroplating process is
550rpm, plating solution pH are 3.5, electroplating time 300s.The sample that electro-deposition there are 2 microns of thick nano-composite plates is put into plating
It carries out containing following components in plating outer layer Ni, the every 1L of the plating solution in Ni liquid: hydration nickel sulfate 250g, hydrated nickel chloride 40g, boron
Sour 40g, lauryl sodium sulfate 0.3g, saccharin sodium 1g, remaining is deionized water.Power supply is adjustable dual-pulse power supply, use
Average current density is 3.5A/dm2, plating solution pH is 4.5, and temperature when plating is 45 DEG C, frequency 50Hz, and total duty ratio is
40%, wherein positive duty ratio is 36%, electroplating time 300s.The sample wash that plating is completed completely dries up later, connects
Sample is placed in vacuum tube furnace again, after being subsequently passed inert gas, the heat treatment process through 850 DEG C, 8h is contained
Cr2O3Diffusion barrier and anti-corrosion Ni layers of oxide composite coating.Obtained oxide diffusion barrier Cross Section Morphology is as shown in Figure 2.Through heat
Outer boundary disappears in treated anticorrosion layer, and the oxidation that continuous, average thickness is about 1 micron is generated at interior outer boundary
Object.Sample is scanned using power spectrum, the main component of obtained oxide composite coating is shown in Table three (marking part in Fig. 2
Point).It can be obtained in conjunction with element Surface scan and element distribution analysis result, oxide diffusion barrier is mainly made of rich Cr oxide.
Table three
Claims (9)
1. a kind of for melting the preparation method for the composite coating that stainless steel containing Cr protects in fluoride salt, which is characterized in that including
Following steps:
1) substrate pre-processes: selecting stainless steel as cathode substrate, nickel sheet is as anode base material, size and the stainless steel yin of nickel sheet
The sizableness of pole substrate, and cathode and anode base material surface are pre-processed, pretreatment refers to the polishing of its surface, falls
Angle, oil removing, washing, activation, again washing process；
2) nano compound electroplating Ni (NiO) transition zone: pretreated anode and cathode substrate is placed in nano compound electroplating slot,
And nano combined pulse plating is carried out in stirring, Ni (NiO) transition zone is prepared, is contained in the every 1L of required electroplate liquid with the following group
Point: hydration nickel sulfate 250g, hydrated nickel chloride 40g, boric acid 40g, lauryl sodium sulfate 0.3g, 20~100g of nickel oxide powder,
Remaining is deionized water；Pulse plating condition are as follows: average current density is 6~8A/dm2, plating solution pH is 3.5, temperature when plating
Degree is 50~55 DEG C, and frequency is 100~500Hz, and total duty ratio is 70~80%, electroplating time 300s；
3) outer layer nickel is electroplated: by it is above-mentioned through nano compound electroplating Ni (NiO) transition zone treated substrate in bright nickel plating slot
It is stirred nickel plating, contains following components in the every 1L of required plating solution: hydration nickel sulfate 250g, hydrated nickel chloride 40g, boric acid
40g, lauryl sodium sulfate 0.3g, saccharin sodium 1g, remaining is deionized water；Plating conditions: average current density 3.5A/
dm2, plating solution pH is 4.5, and temperature when plating is 45 DEG C, frequency 50Hz, and total duty ratio is 40%, wherein positive duty ratio is
36%, electroplating time 300s；
4) be heat-treated: by above-mentioned electroplated outer layer nickel, treated that substrate is placed into the container full of inert gas shielding carries out
The temperature of heat treatment, heat treatment is 850~900 DEG C, time 8h, reacts the Cr in substrate with the NiO in transition zone, Jin Erbiao
Face growth in situ goes out Cr2O3Diffusion barrier is to get to for melting the Cr that stainless steel containing Cr protects in fluoride salt2O3The compound painting of/Ni
Layer.
2. according to claim 1 for melting the preparation method for the composite coating that stainless steel containing Cr protects in fluoride salt,
It is characterized in that, in step 1), the stainless steel selects 316L stainless steel, and is cut into the thin slice of 15 × 10 × 2mm.
3. according to claim 1 for melting the preparation method for the composite coating that stainless steel containing Cr protects in fluoride salt,
It is characterized in that, in step 1), the oil removing in the pretreatment is that substrate is put into acetone soln and in ultrasonic cleaner
Ultrasound 3~5 minutes, the temperature of ultrasonic cleaning are room temperature.
4. according to claim 1 for melting the preparation method for the composite coating that stainless steel containing Cr protects in fluoride salt,
It is characterized in that, in step 1), the activating solution of use is activated in the pretreatment by hydrochloric acid, sulfuric acid and deionized water by quality
Than being mixed for 2:4:2, activation temperature uses room temperature, and activation time is 15 seconds.
5. according to claim 1 for melting the preparation method for the composite coating that stainless steel containing Cr protects in fluoride salt,
It is characterized in that, in step 1), 150 mesh and 600 mesh sand paper are respectively adopted in polishing and chamfering in the pretreatment.
6. according to claim 1 for melting the preparation method for the composite coating that stainless steel containing Cr protects in fluoride salt,
It is characterized in that, in step 2), the partial size of nickel oxide powder employed in the nano compound electroplating is 50nm.
7. according to claim 1 for melting the preparation method for the composite coating that stainless steel containing Cr protects in fluoride salt,
It is characterized in that, in step 2), for the inert gas used in the heat treatment process for high-purity argon gas, container is quartz ampoule.
8. according to claim 1 for melting the preparation method for the composite coating that stainless steel containing Cr protects in fluoride salt,
It is characterized in that, in step 2), the agitating mode used in the nano compound electroplating is magnetic agitation mode, and revolving speed is
550rpm。
9. according to claim 1 for melting the preparation method for the composite coating that stainless steel containing Cr protects in fluoride salt,
It is characterized in that, in step 2), after the electroplate liquid preparation for 24 hours through ultrasonic disperse, disperses more uniform nano-powder to obtain
Plating solution.
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