CN106567118A - Method for preparing Ni-SiC composite coating on inner surface of hollow workpiece - Google Patents
Method for preparing Ni-SiC composite coating on inner surface of hollow workpiece Download PDFInfo
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- CN106567118A CN106567118A CN201610870899.1A CN201610870899A CN106567118A CN 106567118 A CN106567118 A CN 106567118A CN 201610870899 A CN201610870899 A CN 201610870899A CN 106567118 A CN106567118 A CN 106567118A
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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
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/12—Electroplating: Baths therefor from solutions of 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
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/02—Electroplating of selected surface areas
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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
- C25D5/18—Electroplating using modulated, pulsed or reversing current
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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
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
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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
- C25D5/48—After-treatment of electroplated surfaces
- C25D5/50—After-treatment of electroplated surfaces by heat-treatment
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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
- C25D7/00—Electroplating characterised by the article coated
- C25D7/04—Tubes; Rings; Hollow bodies
Abstract
The invention provides a method for preparing a Ni-SiC composite coating on the inner surface of a hollow workpiece. By means of a cyclic electroplating solution code position technology, an electroplating solution only makes contact with the inner surface of the hollow workpiece, and only the composite coating is deposited on the inner surface of the hollow workpiece without affecting the status of the outer surface of the hollow workpiece. The SiC content of the composite coating prepared in the composite electroplating solution with the SiC concentration being 20 g/L reaches up to 18.8%vol, and the utilization rate of SiC is effectively increased. The deposition rate of the Ni-SiC composite coating reaches up to 83 microns per 30min. Compared with a pure nickel coating, the Ni-SiC composite coating is low in surface roughness, uniform and compact and has the characteristics of high hardness, high abrasion resistance and high corrosion resistance. Through the method, the problem of concentration polarization of a composite electroplating solution in an immersion type electroplating system is effectively solved.
Description
Technical field
It is the present invention relates to metal surface properties modification technology and apparatus field, specifically a kind of for the table in the hollow work-piece
The method that face prepares Ni-SiC composite deposites.
Background technology
The metal-based compound coating characteristic such as have low cost, efficiency high and coating performance good, thus be subject to it is widely studied simultaneously
Successfully commercial applications are in automobile industry and aviation field.The performance of metal-based compound coating is with granule content in coating by straight
Connect relation.Content of the granule in metal matrix is higher, is distributed more uniform, the mechanical performance of composite deposite, wearability, corrosion resistance
It is better with non-oxidizability.In metal matrix granule content not only with electro-deposition parameter such as electroplate liquid composition, pH value, additive, electricity
Deposition current type and size are relevant, also have much relations with the selection of codeposition technique.
《Effect of particle size and co-deposition technique on hardness and
corrosion properties of Ni-Co/SiC composite coatings》In point out, traditional codeposition technique is
Refer to that negative electrode is parallel to horizontal plane with anode and parallel just to placing in composite plating solution, keep microgranule to exist using continuous stirring
Suspended state in composite plating solution.And precipitate codeposition technique and refer to that negative electrode and anode are perpendicular to water in composite plating solution
Plane and parallel just to placing, makes granule be suspended in electroplate liquid using intermittent stirring, is subsequently gradually deposited on negative electrode and quilt
Bury and overlay in coating.When preparing composite deposite using precipitation codeposition technique, action of gravity is conducive to granule coprecipitated with metal
Product.《Investigation on the corrosion and oxidation resistance of Ni-Al2O3nano-
composite coatings prepared by sediment co-deposition》In point out, using traditional electro-deposition skill
Art, prepares metal/micron order and nano level inorganic inert granule such as SiC, ZrO2、Al2O3、Si3N4、TiO2、CeO2, nanometer gold
The technique of the composite deposite such as hard rock and CNT is subject to widely studied.Using precipitation codeposition technique, research metal and micron
Grade particles such as graphite, Al, Si3N4、SiC、TiO2、MoS2、WS2, the co-deposition such as PTFE and diamond the existing many reports of technique
Road, but the technique that research metal is co-deposited with nano-scale particle is but rarely reported.《Electrodeposition of
graphite-bronze composite coatings and study of electroplating
characteristics》In be respectively adopted traditional codeposition technique and precipitation codeposition technique prepare G-Cu (Sn) composite deposite.
As a result show, low content graphite can be uniformly distributed in composite deposite prepared by two kinds of technologies, but work as graphite in composite deposite
When content is higher, graphite granule all occurs the phenomenon of particle agglomeration in two kinds of composite deposites, and the uniformity of composite deposite is reduced,
And the surface roughness increase of composite deposite.
Compared with traditional codeposition technique, there is precipitation codeposition technique feature to be can be from the relatively low compound electric of granule density
Obtain in plating solution and be co-deposited the high composite deposite of granule content, and co-deposition dispersibility of the granule in metal matrix is higher.
But using precipitation codeposition technique prepare composite deposite when, due to cathode parallel in horizontal plane place and be located at anode just under
Side, the such as earth of positive pole of the other impurities in composite plating solution in addition to granule can also be deposited in cathode surface, cause composite deposite table
Face it is coarse it is loose, easily there is dross tissue, the problems such as be easily mingled with.
Most importantly, traditional codeposition technique and precipitation codeposition technique are to be fully immersed in again negative electrode and anode
Carry out in closing electroplate liquid, therefore, non-working surface inevitably can be had composite deposite by low corrosion to a certain extent or deposition.
For outer surface has specific function only to allow in the hollow work-piece such as cylinder that inner surface deposits composite deposite, this two
Plant codeposition technique not optimal choice.In addition, the sedimentation rate of two kinds of codeposition techniques needs further to be improved.
Therefore, study densification that is a kind of high in one layer of granule content of hollow work-piece inner surface high speed deposition and being evenly distributed multiple
Coating is closed, while the electro-deposition techniques of hollow work-piece appearance surface state are not affected, it is significant.
The content of the invention
To overcome, the surface roughness of composite deposite present in prior art is big, composite deposite rough surface is loose, easy
There is dross tissue, be easily mingled with, and non-working surface inevitably there can be Composite Coatings by low corrosion to a certain extent or deposition
The deficiency of layer, the present invention propose a kind of method for preparing hollow work-piece inner surface Ni-SiC composite deposites.
The present invention detailed process be：
Step 1：Prepare composite plating solution.
It is that deionized water is formulated with composite plating solution stock solution to prepare composite plating solution.Prepare the desired amount of compound electric
During plating solution, in proportion deionized water is mixed with composite plating solution stock solution, and carry out air stirring；The air stirring persistent period is
12～24h.PH acidity regulators and pH alkalescence regulators is adopted to combine and make the pH value of mixed liquor for 4.0 ± 0.1.It is combined
Electroplate liquid.
The composite plating solution is by nickel sulfate, Nickel dichloride., boric acid, carborundum, saccharin sodium and cetyl trimethyl bromination
Ammonium is constituted；Nickel sulfate containing 350～450g/L, the Nickel dichloride. of 10～20g/L, 30～40g/ respectively in every liter of composite plating solution
The cetyl trimethylammonium bromide of the boric acid of L, the carborundum of 50～70g/L, the saccharin sodium of 2～3g/L and 0.4～0.8g/L.
When preparing composite plating solution stock solution, by the nickel sulfate for weighing, Nickel dichloride. and saccharin sodium and pour in reservoir, start
Air stirrer persistently carries out air stirring, is all dissolved as mixed liquor to nickel sulfate, Nickel dichloride. and saccharin sodium.In the mixing
The boric acid for weighing is added in liquid, mixed liquor is heated to into 75 DEG C by the heating rod in reservoir, while persistently entering to mixed liquor
Row air stirring, all dissolving to boric acid.The SiC microgranules and cetyl for weighing is added in the mixed liquor added with boric acid
Trimethylammonium bromide, mix homogeneously obtain composite plating solution stock solution.
Step 2：Prepare hollow work-piece.The preparation hollow work-piece is that hollow work-piece is first carried out stress relief annealing, then is beaten
Surface is milled to without rusty stain, antirust oil is coated, it is stand-by.The hollow work-piece is heated to into 550 DEG C with stove during stress relief annealing, is incubated
20min, cools to 30 DEG C with the furnace.
Step 3：Heat and stir composite plating solution.The heating to stir composite plating solution be the composite plating that will be obtained
Liquid is placed in reservoir, opens air stirring switch, 2～3h of air stirring is carried out to composite plating solution to starting to hollow work-piece
Carry out impactive nickel plating.During air stirring, air mass flow is 4～6m3/h.Start to open heater switch during stirring, to compound electric
Plating solution is heated, and heating-up temperature is 60 DEG C.
Step 4：Process electrode.With 400#The surface of the inner surface and anode conducting rod of liquid honing negative electrode conducting ring.
Step 5：Defat.The antirust oil on hollow work-piece surface is first cleaned with acetone, then carries out heat alkali liquid defat.The defat
When, hollow work-piece is placed in the alkali liquor of preparation and is reacted：The temperature of alkali liquor is 75～85 DEG C；Response time is 3～5min.
With 75～85 DEG C of hot water injection 2min；Deionized water rinses 2min.
Described alkali liquor is by 20～40g/LNaOH, 20～30g/LNa2CO3, 5～15g/LNa3PO4With 5～7mL/LOP
Emulsifying agent is configured to form.
Step 6：Corrode.Hollow work-piece after defat is placed in hydrochloric acid solution, by corroding the oxygen for removing metal surface
Change film and corrosion thing.The technological parameter of erosion is：30%HCl solution is prepared under room temperature, erosion time is 4～6min.Corrode
Cheng Hou, does not carry out deionized water rinsing, directly carries out next step activation processing.
Step 7：Activation.Hollow work-piece is placed in into the H that sulfuric acid concentration is 5%2SO4Activated in activated solution, to enter one
Step removes the oxide-film on hollow work-piece surface, makes the fresh matrix on hollow work-piece surface fully come out.Hollow work-piece is completed
Plating is carried out after activation processing.The technological parameter of activation is：Activation temperature≤25 DEG C, soak time is 2min, deionized water
Rinse 2min.
Step 8：Hollow work-piece is installed.Negative electrode conducting ring is enclosed within hollow work-piece, and will be cased with negative electrode conducting ring
Empty workpiece is placed between upper fixture and lower clamp, and adjustment upper fixture, hollow work-piece and lower clamp make the centrage of three overlap；
Nut on fastening leading screw, makes the contact face seal between hollow work-piece and upper fixture and lower clamp.
Opening plating rectifier power source makes hollow work-piece connect with power cathode, carries out cathodic protection to hollow work-piece.
Step 9：Prime coat is prepared in hollow work-piece inner surface.Bottoming is prepared in hollow work-piece inner surface by impactive nickel plating
Layer.Before impactive nickel plating, first close compressed air pump and stop stirring composite plating solution, make composite plating solution stand 20min, SiC
Microgranule free settling, in the composite plating solution of upper strata, SiC fraction of particle is low.When starting impactive nickel plating, by what is be connected with upper water-out mouth
Hand-operated valve is adjusted to maximum, and the hand-operated valve being connected with lower outlet is adjusted to minimum.Electromagnetic flowmeter is adjusted, makes to enter during impactive nickel plating
1.5 times of the volume flow of composite plating solution when the volume flow for entering the composite plating solution of plating chamber is Ni-SiC composite platings；
The time of the impactive nickel plating be 5min, during the Ni-SiC composite platings volume flow of composite plating solution be 1.6～
4.5m3/h.1.5 times of electric current when electric current when adjusting impactive nickel plating is Ni-SiC composite platings；The Ni-SiC composite platings
When electric current to the hollow work-piece inner surface electric current density be 8～12.5A/dm2.The temperature of impactive nickel plating is 50～70 DEG C,
The pH value of composite plating solution is 3.9～4.1, and plating time is 30min.
Step 10：Ni-SiC composite platings.The hand-operated valve that will be connected with lower outlet after completing impactive nickel plating is adjusted to most
Greatly, open compressed air pump.Electromagnetic flowmeter is adjusted, the volume flow for making composite plating solution into plating chamber is 1.6～
4.5m3/h；Electric current is adjusted, the electric current density for making hollow work-piece inner surface is 8～12.5A/dm2.The temperature of Ni-SiC composite platings
For 50～70 DEG C；PH value is 3.9～4.1；Plating time is 25min.
The impactive nickel plating and Ni-SiC composite platings it is total during, 50～83 μm of the sedimentation rate of composite plating solution/
30min。
Step 11：Dismounting hollow work-piece.
Step 12：Post processing.The hollow work-piece of composite plating is completed, surface of the work residual is washed off in deionized water
Composite plating solution, under ultrasound wave concussion cleaning 15min, drying.
The hollow work-piece of drying is put into and is heated in 150～200 DEG C of heating furnace and is incubated 1.5～2.5h；Insulation
Cool to room temperature after end with the furnace, obtaining inner surface has the hollow work-piece of composite deposite.Heat treatment after plating is conducive to dehydrogenation simultaneously
Coating internal stress is eliminated, coat binding strength is improved.
The present invention prepares Ni- using the hollow work-piece inner surface proposed in 201610810698.2 innovation and creation of Application No.
The device of SiC composite deposites is realized to hollow work piece inner surface plating.Composite plating solution is made to be in all the time by the electroplanting device
Flow regime, efficiently solves the problems, such as composite plating solution concentration polarization in immersion type electroplating system, can also make SiC microgranules abundant
Suspend, sedimentation rate is fast, and cathodic polarization is good, the composite deposite of the high Ni-based matter of nanoscale of SiC content of even compact can be prepared.
Therefore, based on the electroplanting device, the invention provides a kind of circulation electroplate liquid codeposition technique.
The operating parameter of this circulation electroplate liquid codeposition technique：Electric current density is 8～12.5A/dm2；Temperature is 50～70
℃；PH value is 3.9～4.1；2～3 μm/min of sedimentation rate；Composite plating solution volume flow is 1.6～4.5m3/h；During plating
Between 30min.
The method that the present invention provides cleaning workpiece after a kind of plating：Composite plating solution is stood, the outlet of bottom land is closed, is opened
Outlet in the middle part of groove, now the composite plating solution of input channel is the less supernatant of SiC content, adopts less flow velocity, keeps away
Exempt to stir the composite plating solution in reservoir, so as to the SiC that remains pipeline and surface of the work again flush clean is to compound electric
In plating solution, reduce carry-over loss.
Fig. 1 changes over figure for composite plating process parameter；Wherein：1. it is that electric current density changes over curve；2.
Volume flow changes over curve.In order to prepare the composite deposite being well combined with matrix, in the Ith stage of composite plating,
Impactive nickel plating is carried out with the electric current density and volume flow in 1.5 times of the IIth stage, one layer of transition zone, energy is deposited in matrix surface
Improve the adhesion of Ni-SiC composite deposites and matrix.
Fig. 2 is sampling explanation schematic diagram；Wherein, sampling angles of Fig. 2 a for integral macroscopic surface；Fig. 2 b are local macroscopic view
The sampling angle on surface；Sample position of Fig. 2 c for microscopic appearance.In figure, a represents the upper end of hollow work-piece, and b represents hollow work
The lower end of part, c represent and sample that d is represented in short transverse.Fig. 2 c are represented hollow work-piece along straight line
L launches after disconnecting, and X-axis represents circumferentially deploying direction, and Y-axis represents thickness direction, and Z axis represent short transverse.
As nickel anode has periodicity and symmetry, accordingly, the composite deposite of hollow work-piece inner surface is divided into into 12
The individual cycle.In order to study the uniformity of SiC content, thickness and microhardness in Ni-SiC composite deposites, respectively along height and week
C and d is chosen on direction to be analyzed, under an electron microscope, the microscopic appearance observed at c and d 10 Along ents of sample.
As shown in Figure 3.During using the nickel anode with poroid electroplate liquid flow channel, the surface of the composite deposite of acquisition goes out
It is in now the scraping decorative pattern of divergent shape, and decorative pattern is parallel just right with the electroplate liquid flow channel on nickel anode.According to hydromechanical
Knowable to equation of continuity, υPoroid electroplate liquid flow channel=υNickel anode*(SNickel anode/SPoroid electroplate liquid flow channel), S in formulaNickel anodeAnd SPoroid electroplate liquid flow channelRespectively
The gross area of nickel anode area of section and electroplate liquid flow channel, υNickel anodeAnd υPoroid electroplate liquid flow channelRespectively composite plating solution passes through nickel
The flow velocity of anode and poroid electroplate liquid flow channel.Due to SNickel anode＞ SPoroid electroplate liquid flow channel, then υPoroid electroplate liquid flow channelMore than υNickel anode.By hole
The composite plating solution of the entrainment hard SiC particulate that shape electroplate liquid flow channel sprays at a high speed, makees to the impact-scraping of composite deposite
There is the destruction with composite deposite surface is caused.
As shown in Figure 4.During using the nickel anode with strip electroplate liquid flow channel, the surface of the composite deposite of acquisition is complete
It is whole.This is because increasing the gross area of electroplate liquid flow channel, υStrip electroplate liquid flow channelReduce, sprayed by electroplate liquid flow channel
Impact-scraping effect of the composite plating solution to composite deposite reduces.
As shown in Figure 5.Can be seen that compared with nickel coating by low power surface topography, the surface of Ni-SiC composite deposites
Uniform ground, roughness are low.This is because SiC microgranules change the growth mechanism of Ni-based matter.SiC microgranules nickel metal surface with
Machine adsorbs, and reduces the growth rate of fast aufwuchsplate in nickel crystallization process so as to which the growth rate of each crystal plane reaches unanimity, most
Make the surface topography of composite deposite more smooth than nickel coating eventually.In high power surface topography map, nickel coating crystal grain is in born of the same parents' shape, brilliant
The hole of intergranular is high-visible；The surfacing of Ni-SiC composite deposites is fine and close, has no the poor platings such as hole, loose, dross
Tissue, the SiC particulate of black are evenly distributed on white Ni matrixes.Circulating for composite plating solution can promote SiC microgranules
It is dispersed, be conducive to improving the microgranule loading between the volume content of SiC microgranules in composite deposite and crystal boundary, reduce Composite Coatings
The porosity of layer, improves organizational structure, improves the hardness and wear resistance and corrosion resistance of coating.
As shown in Figure 6.Nickel coating and Ni-SiC composite deposites are well combined with matrix, and coating microstructure is continuously fine and close,
The harmful structure such as hole, loose is had no, SiC does not occur to reunite in being evenly distributed on Ni-based matter in Ni-SiC composite deposites.Pure nickel
The sedimentation rate of coating is 43 μm/30min, and the sedimentation rate of Ni-SiC composite deposites is up to 83 μm/30min.
As shown in Figure 7.The size of volume flow determines that composite plating solution and hard SiC microgranules are rushed to cathode inner surface
Brush and scraping intensity.On the one hand cathode inner surface can be adsorbed SiC microgranules or loose loosely with scraping action by this washing away
Composite deposite is taken back in composite plating solution, improves composite deposite quality；On the other hand coating can be destroyed, the table of composite deposite is reduced
Face quality, and volume flow is bigger, impact and scraping action are bigger, and surface quality is poorer.Carried out using less volume flow
During composite plating, impact and scraping action to cathode surface of composite plating solution and SiC microgranules is less, now composite plating solution
Main Function is the means of transport that SiC microgranules and nickel ion are conveyed to negative electrode, is conducive to improving the SiC content in composite deposite.
In composite deposite, SiC content is higher, and composite deposite hardness is bigger, and anti-cutting power is better, the Ni- complete so as to form surface
SiC composite deposites.When volume flow is 1.6m3During/h, composite plating solution can not be completely filled with composite plating chamber, in hollow work-piece
End does not deposit composite deposite.
As shown in Figure 8.The SiC content and thickness of coating of the composite deposite prepared under different volumes flow circumferentially uniform one
Cause.Volume flow is bigger, and in composite deposite, SiC content is lower, and thickness is less.Think, composite plating solution is with suitable body
When product flow is circulated, be not only advantageous to nickel ion and SiC microgranules be conveyed to negative electrode, reduce concentration polarization, improve coating
Sedimentation rate, moreover it is possible to promote the suspended dispersed of SiC microgranules, increases the collision frequency of SiC microgranules and cathode surface, thinning negative electrode table
The thickness of face electric double layer, makes SiC microgranules be more easy to into electric double layer adsorb in cathode surface, and adsorbs micro- in the SiC of cathode surface
Grain can shorten nucleated time, the sedimentation rate increase of coating as the nonuniformity nucleating center of nickel ion deposition.But increase volume
During flow, the flowing velocity and stirring capacity of composite plating solution increase therewith, and composite plating solution increases to the impulsive force of cathode surface
Greatly, cause to be in weakly stable state or do not buried the SiC microgranules for covering completely by nickel matrix metal in cathode surface to be washed, and it is multiple
The kinetic energy increase of the SiC in electroplate liquid being closed, absorption being difficult in cathode surface, these processes are unfavorable for entering for composite codeposition
OK.Therefore, during composite electrodeposition, the SiC content and sedimentation rate of composite deposite is as the increase of volume flow is in
The trend of reduction.
As shown in Figure 9.The microhardness of the composite deposite prepared under different volumes flow circumferentially uniformity, and with
The increase of volume flow and reduce, it is consistent with the regularity of distribution circumferentially of SiC content in coating.The hardness of this explanation composite deposite
Relevant with the content of the SiC microgranules in coating, SiC content is higher, and the hardness of coating is bigger.
As shown in Figure 10.In composite deposite, SiC fraction of particle is more or less the same in the height direction, only the coating of upper and lower ends
Middle SiC content is higher, and this is concentrated in regional areas such as edge tips due to electric current density, the increase of nickel ion sedimentation rate, contracting
Short SiC microgranules are buried completely by nickel metal the time covered, i.e. the increasing number of the SiC microgranules of unit interval IT, thus are gone out
The composite deposite SiC content height at existing two ends and the big phenomenon of thickness of coating.
As shown in figure 11.Ni-SiC composite deposites fluctuate near the 620HV along the hardness of short transverse, upper and lower ends it is hard
Higher than mid portion, this is that SiC content is higher than mid portion in composite deposite by upper and lower ends causes degree.
As shown in figure 12.The anode of Q235 matrixes, nickel coating and Ni-SiC composite deposites in the NaCl solution of 0.5M
Polarization curve all experienced the activation-passivation transition process of anode polarization.Relative to pure Ni coating and Q235 matrixes, Ni-SiC is multiple
The corrosion potential for closing coating occurs substantially to shuffle.Q235 matrixes, nickel coating and Ni- are calculated respectively according to three polarization curves
The corrosion potential and corrosion current i of SiC composite depositescorr, as shown in table 2.The corrosion potential ratio of Ni-SiC composite deposites
The corrigendum of nickel coating and Q235 matrixes, the corrosion current of composite deposite are minimum.Test result indicate that, the corrosion resistance of composite deposite is excellent
In nickel coating, effective protection can be provided for Q235 matrixes as cathodic electrodeposition coating.This conclusion can be by the analysis of impedance curve
As a result it is confirmed.
As shown in figure 13.The impedance curve of Q235, nickel coating and Ni-SiC composite deposites in the NaCl solution of 0.5M exists
Have differences in size, but shape is similar, the corrosion process of this explanation Q235, nickel coating and Ni-SiC composite deposites follows identical
Corrosion mechanism.The semicircle arc radius of contrast impedance curve can show that the semicircle arc radius of Ni-SiC composite deposites are maximum, nickel
Coating secondly, the minimum of Q235 matrixes.This is because the SiC microgranules being deposited in composite deposite change the structure of Ni-based matter,
The germinating of etch pit can be stopped and grown up as physical barriers in the SiC microgranules of coating surface, to the passivated of nickel matrix metal
Journey has facilitation, so as to improve the corrosion resistance of composite deposite.
As shown in figure 14.When starting insulation at 200 DEG C, there is atomic rearrangement in Ni-SiC composite deposites on an atomic scale
Or nickel-silicon compound in structural relaxation, and coating, is separated out, distortion of lattice aggravation, hardness are raised；During insulation 3h, tiny is nickel suicide
Compound amount of precipitation is maximum, and disperse effect is the most obvious, and coating hardness is increased to maximum；When continuing insulation, nickel-silicon compound is long
Greatly, disperse decreased effectiveness, coating hardness decline.Heat treatment temperature is higher, and the crystallite dimension of nickel-silicon compound is bigger, disperse effect
It is weaker, and the crystal grain of Ni-based matter grows up also with the rising of temperature, the crystal boundary and phase boundary in composite deposite is reduced, and coating is soft
Change.Therefore, the coating hardness after carrying out heat treatment at 400 DEG C is minimum.
As shown in figure 15.Wherein, first 3 groups be Ni-SiC composite deposites respectively with GCr15 balls, Al2O3Ball and ZrO balls are to mill
The quality wear rate of generation, experiment condition are load 15N under room temperature, speed 4.222m/min, experimental period 30min；2 groups are afterwards
The Ni-SiC composite deposites being incubated at 200 DEG C or 300 DEG C after 3h and Al2O3The quality wear rate that ball is produced to mill, experiment condition
For load 15N under room temperature, speed 4.222m/min, experimental period 30min.Jing after 300 DEG C × 3h heat treatments, Ni-SiC Composite Coatings
The quality wear rate of layer is minimum.Compared to not thermally treated composite deposite, the equal energy of heat treatment is carried out at 200 DEG C or 300 DEG C
The wearability of Ni-SiC composite deposites is improved, and composite deposite, Jing after the heat treatment of 300 DEG C × 3h, its hardness and adhesion reach
Good cooperation, wearability are optimal.Possibly Jing after 200 DEG C × 3h heat treatments, coating hardness is high, while coating internal stress is not yet
It is completely eliminated, the mass loss rate of coating is big.
Description of the drawings
Fig. 1 changes over figure for composite plating process parameter；Wherein：1. it is that electric current density changes over curve；2.
Volume flow changes over curve.
Fig. 2 is sampling explanation schematic diagram；Wherein, sampling angles of Fig. 2 a for integral macroscopic surface；Fig. 2 b are local macroscopic view
The sampling angle on surface；Sample position of Fig. 2 c for microscopic appearance.In figure, a represents the upper end of hollow work-piece, and b represents hollow work
The lower end of part, c represent and sample that d is represented in short transverse.Fig. 7 c are represented hollow work-piece along straight line
L launches after disconnecting, and X-axis represents circumferentially deploying direction, and Y-axis represents thickness direction, and Z axis represent short transverse.
The macro surface shape of the composite deposite that Fig. 3 is obtained when being using the nickel anode with poroid electroplate liquid flow channel
Looks；Wherein, integral macroscopic surfaces of Fig. 3 a for hollow work-piece；Fig. 3 b are hollow work-piece local macro surface.
The macro surface shape of the composite deposite that Fig. 4 is obtained when being using the nickel anode with gap-like electroplate liquid flow channel
Looks；Wherein, Fig. 4 a are integral macroscopic surface topography；Fig. 4 b are local macro surface pattern.
Fig. 5 is the micromorphology of nickel coating and Ni-SiC composite deposites；Wherein, Fig. 5 a are nickel coating under low power
Micromorphology；Fig. 5 b are the micromorphology of Ni-SiC composite deposites under low power；Fig. 5 c are nickel coating under high power
Micromorphology；Fig. 5 b are the micromorphology of Ni-SiC composite deposites under high power.
Fig. 6 is the microscopic cross pattern of nickel coating and Ni-SiC composite deposites；Wherein, microcosmic of Fig. 6 a for nickel coating
Cross Section Morphology；Microscopic cross patterns of Fig. 6 b for Ni-SiC composite deposites.
Fig. 7 is the macro surface pattern of Ni-SiC composite deposites under different volumes flow；Wherein, Fig. 7 a are that volume flow is
1.665m3The macro surface pattern of Ni-SiC composite deposites during/h；It is 2.174m that Fig. 7 b are volume flows3During/h, Ni-SiC is combined
The macro surface pattern of coating；It is 2.462m that Fig. 7 c are volume flows3The macro surface pattern of Ni-SiC composite deposites during/h；Figure
It is 3.208m that 7d is volume flow3The macro surface pattern of Ni-SiC composite deposites during/h；It is 4.587m that Fig. 7 e are volume flows3/
The macro surface pattern of Ni-SiC composite deposites during h.
Fig. 8 is cutting at 10 Along ents in Ni-SiC composite deposites under different volumes flow circumferentially direction unit period
Face pattern；Wherein, Fig. 8 a are that volume flow is 1.665m3During/h, Ni-SiC composite deposites are circumferentially on direction 10 in unit period
Cross Section Morphology at individual Along ent；It is 2.174m that Fig. 8 b are volume flows3During/h, Ni-SiC composite deposites are circumferentially single on direction
Cross Section Morphology in bit period at 10 Along ents；It is 2.462m that Fig. 8 c are volume flows3During/h, Ni-SiC composite deposites are along week
Cross Section Morphology on direction in unit period at 10 Along ents.
Fig. 9 is Ni-SiC composite deposites hardness profile circumferentially under different volumes flow；In figure：3 is Q235 bases
The hardness profile of body；4 is nickel coating hardness profile circumferentially；5 is that volume flow is 3.209m3Prepare during/h
Composite deposite hardness profile circumferentially；6 is that volume flow is 2.462m3The composite deposite for preparing during/h is circumferentially
Hardness profile；7 is that volume flow is 2.174m3The composite deposite prepared during/h hardness profile circumferentially；8 is body
Product flow is 1.665m3The composite deposite prepared during/h hardness profile circumferentially.
Figure 10 is the distribution curve of the SiC content and thickness of coating of Ni-SiC composite deposites in short transverse；In figure：9
It is distribution curve of the SiC content of Ni-SiC composite deposites in short transverse；10 is the thickness edge height of Ni-SiC composite deposites
Distribution curve on degree direction.
Figure 11 is hardness profile of the Ni-SiC composite deposites in short transverse.
Figure 12 is that the anode polarization of Q235 matrixes, nickel coating and Ni-SiC composite deposites in the NaCl solution of 0.5M is bent
Line；In figure：11 is the anodic polarization curves of Q235 matrixes；12 is the anodic polarization curves of nickel coating；13 is that Ni-SiC is combined
The anodic polarization curves of coating.
Figure 13 is the impedance curve of Q235, nickel coating and composite deposite in the NaCl solution of 0.5M；In figure：14 is Q235
The impedance curve of matrix；15 is the impedance curve of nickel coating；16 is the impedance curve of Ni-SiC composite deposites.
Figure 14 be different heat treatment at a temperature of composite deposite hardness with temperature retention time change curve；In figure：17 is 200
The hardness of composite deposite during heat treatment is carried out at DEG C with temperature retention time change curve；18 is that heat treatment recurrence of disease at the same time next year is carried out at 300 DEG C
The hardness of coating is closed with temperature retention time change curve；19 is the hardness of composite deposite when heat treatment is carried out at 400 DEG C with insulation
Time changing curve.
Figure 15 is the quality wear rate of Ni-SiC composite deposites under different abrasive conditions.
Figure 16 is the flow chart of the present invention.
Specific embodiment
The present invention is with Q235 steel revolving body as hollow work-piece to be plated.The present invention is that a kind of employing circulates electroplanting device hollow
The preparation method of work piece inner surface Ni-SiC composite deposites, is a kind of method of circulation electroplate liquid co-deposition.
The present invention propose in utilizing the innovation and creation of Application No. 201610810698.2 for preparing in hollow work-piece
The device of surface Ni-SiC composite deposites is realized to hollow work piece inner surface plating.
The device for preparing hollow work-piece inner surface Ni-SiC composite deposites, including the circulation of reservoir, electroplate liquid
Pump, compressed air pump, electromagnetic flowmeter, compressed air pump and sealing plating station.
The lower discharging tube and upper water-out pipe being parallel to each other is placed with the reservoir, and is located at the upper water-out pipe
At the 3/4 of electroplate liquid liquid level, lower discharging tube is located at the lowest point of electroplate liquid liquid level；The port of export of the lower discharging tube is stored up with being located at
The entrance connection of the electroplate liquid circulating pump outside liquid bath；The port of export of the upper water-out pipe is connected with lower discharging tube outside reservoir.
The outlet of the electroplate liquid circulating pump is connected with the entrance of the electromagnetic flowmeter in reservoir by pipeline；Institute
The outlet for stating electromagnetic flowmeter is connected with the plating chamber water inlet of lower clamp by pipeline；Flow out from upper water-out pipe with lower discharging tube
Electroplate liquid converge after, under the driving force of electroplate liquid circulating pump, flow direction sealing plating station, adjust electromagnetic flowmeter control flow direction
The electroplate liquid volume flow of sealing plating station；After composite plating is completed in sealing plating station, electroplate liquid returns to liquid storage by loop
In groove.
The compressed air pump is located at the outer opposite side of reservoir；The outlet of the compressed air pump is connected to electromagnetic flowmeter and goes out
On pipeline between mouth and electroplate liquid circulating pump；There is air exhaust duct on the export pipeline of the compressed air pump；The sky
The pipe level at gas exhaust outlet end is placed in the reservoir inner bottom surface, and is located in reservoir in the air exhaust duct
There are two steam vents on the tube wall that a section of basal surface, what two steam vent was symmetrical is distributed under the air exhaust duct circumferential surface
Side；Angle α between the centrage of two steam vent is 90 °.
Make composite plating solution all the time in flow regime by the electroplanting device, efficiently solve in immersion type electroplating system
The problem of composite plating solution concentration polarization, can also make SiC microgranules fully suspend, and sedimentation rate is fast, and cathodic polarization is good, can prepare
The composite deposite of the high Ni-based matter of nanoscale of even fine and close SiC content.
The present invention will describe its detailed process in detail by 5 embodiments.
The preparation process of the hollow work-piece surface Ni-SiC composite deposites is as follows：
Step 1：Prepare composite plating solution.
It is that deionized water is formulated with composite plating solution stock solution to prepare composite plating solution.Prepare the desired amount of compound electric
During plating solution, in proportion deionized water is mixed with composite plating solution stock solution, and carry out air stirring；The air stirring persistent period is
12～24h.PH acidity regulators and pH alkalescence regulators is adopted to combine and make the pH value of mixed liquor for 4.0 ± 0.1.It is combined
Electroplate liquid.
The composite plating solution is by nickel sulfate, Nickel dichloride., boric acid, carborundum, saccharin sodium and cetyl trimethyl bromination
Ammonium is constituted；Nickel sulfate containing 350～450g/L, the Nickel dichloride. of 10～20g/L, 30～40g/ respectively in every liter of composite plating solution
The cetyl trimethylammonium bromide of the boric acid of L, the carborundum of 50～70g/L, the saccharin sodium of 2～3g/L and 0.4～0.8g/L.
When preparing composite plating solution stock solution, by the nickel sulfate for weighing, Nickel dichloride. and saccharin sodium and pour in reservoir, start
Air stirrer persistently carries out air stirring, is all dissolved as mixed liquor to nickel sulfate, Nickel dichloride. and saccharin sodium.In the mixing
The boric acid for weighing is added in liquid, mixed liquor is heated to into 75 DEG C by the heating rod in reservoir, while persistently entering to mixed liquor
Row air stirring, all dissolving to boric acid.The SiC microgranules and cetyl for weighing is added in the mixed liquor added with boric acid
Trimethylammonium bromide, mix homogeneously obtain composite plating solution stock solution.
The present embodiment is by taking the composite plating solution for preparing 100L as an example.Nickel sulfate, the chlorine of 15g/L of 350g/L are weighed in proportion
Change the cetyl trimethylammonium bromide of nickel, the boric acid of 30g/L, the carborundum of 70g/L, the saccharin sodium of 3g/L and 0.6g/L.
70L deionized waters are added in reservoir.By the nickel sulfate for weighing, Nickel dichloride. and saccharin sodium and pour in reservoir, start air
Agitating device persistently carries out air stirring to mixed liquor, all dissolving to nickel sulfate, Nickel dichloride. and saccharin sodium.In mixed liquor
It is middle to add the boric acid for weighing, mixed liquor is heated to into 75 DEG C by the heating rod in reservoir, while persistently carrying out to mixed liquor
Air stirring, all dissolving to boric acid.The SiC microgranules and cetyl trimethyl for weighing is added in the mixed liquor for obtaining
Ammonium bromide, obtains composite plating solution stock solution.Deionized water is added in the composite plating solution stock solution for obtaining, and total amount is obtained for 100L
Mixed liquor.Groove lid is covered, continuation carries out air stirring to mixed liquor, and the persistent period is 18h.Using pH acidity regulators and pH
Alkaline regulator combine make mixed liquor pH value be 4.0 ± 0.1.Obtain composite plating solution.
Step 2：Prepare hollow work-piece.To eliminate machining stress and reducing the stress of hollow work-piece itself, by hollow work-piece
Stress relief annealing is first carried out, then surface is polishing to without rusty stain, coat antirust oil, it is stand-by.Stress relief annealing technique is with stove heat
To 550 DEG C, 20min is incubated, 30 DEG C are cooled to the furnace.
Step 3：Composite plating solution prepared by heating whipping step 1.The composite plating solution for obtaining is placed in reservoir,
Air stirring switch is opened, and 2～3h of air stirring is carried out to composite plating solution to starting impactive nickel plating to be carried out to hollow work-piece.It is empty
During gas agitating, air mass flow is 4～6m3/h.Start heater switch to be opened during stirring, composite plating solution is heated, plus
Hot temperature is 60 DEG C.
Step 4：Process electrode.In order that electrodes conduct is good, before plating first with 400#Liquid honing negative electrode is conductive
The inner surface of ring.Negative electrode conducting ring is aluminum alloy material, and surface is easily passivated the passivating film for generating poorly conductive.Need to be beaten with waterproof abrasive paper
Mill, destroys surface passivated membrane, makes fresh metal exposed out, so that having good conduction between negative electrode conducting ring and negative electrode
Property.Same grinding process anode conducting rod, makes have good electric conductivity between conductive anode rod and nickel anode.
Step 5：Acetone oil removing, heat alkali liquid defat.The antirust oil on hollow work-piece surface is first cleaned with acetone, then carries out thermokalite
Loss of thick fluid fat.
Hollow work-piece is placed in the alkali liquor of preparation and is reacted：The alkali liquor of preparation is heated to into 75～85 DEG C；During reaction
Between be 3～5min.Then with 75～85 DEG C of hot water injection 2min, then deionized water rinses 2min.
Described alkali liquor is by 20～40g/LNaOH, 20～30g/LNa2CO3, 5～15g/LNa3PO4With 5～7mL/LOP
Emulsifying agent is configured to form.
Step 6：Corrode.Pickling can remove the oxide-film of metal surface and corrosion thing.Hydrochloric acid to metal-oxide with compared with
Strong solvability, dissolves relatively slow to metallic matrix, and the excessive erosion harm to matrix is little.The technological parameter of erosion is：Under room temperature,
30%HCl solution is prepared, erosion time is 4～6min.After the completion of erosion, deionized water rinsing is not carried out, directly carried out next
Step activation processing.Do not wash after corroding in 30%HCl and activated in being directly entered dilute sulfuric acid, more preferably, this is its effect
Because micro hydrochloric acid plays etching catalytic action in dilute sulfuric acid, activation effect is more preferable.
Step 7：Activation.Hollow work-piece is placed in into the H that sulfuric acid concentration is 5%2SO4Activated in activated solution, to enter one
Step removes the oxide-film on hollow work-piece surface, makes the fresh matrix on hollow work-piece surface fully come out.Hollow work-piece is completed
Plating is carried out after activation processing.The technological parameter of activation is：Activation temperature≤25 DEG C, soak time is 2min, deionized water
Rinse 2min.
Step 8：Hollow work-piece is installed.Negative electrode conducting ring is enclosed within hollow work-piece, and will be cased with negative electrode conducting ring
Empty workpiece is placed between upper fixture and lower clamp, adjustment upper fixture, hollow work-piece and lower clamp, makes the centrage weight of three
Close, fasten the nut on leading screw, make the contact face seal between hollow work-piece and upper fixture and lower clamp.To prevent hollow work-piece molten
Solution, pollutes composite plating solution, and the present invention adopts powered plating technology.
The powered plating technology is that, before composite plating solution contact hollow work-piece, first opening plating rectifier power source makes hollow
Workpiece is connected with power cathode, carries out cathodic protection to hollow work-piece.
Step 9：Prime coat is prepared in hollow work-piece inner surface.Bottoming is prepared in hollow work-piece inner surface by impactive nickel plating
Layer.Before impactive nickel plating, first close compressed air pump and stop stirring composite plating solution, make composite plating solution stand 20min, SiC
Microgranule free settling, in the composite plating solution of upper strata, SiC fraction of particle is low.When starting impactive nickel plating, by what is be connected with upper water-out mouth
Hand-operated valve is adjusted to maximum, and the hand-operated valve being connected with lower outlet is adjusted to minimum.Electromagnetic flowmeter is adjusted, makes to enter during impactive nickel plating
1.5 times of the volume flow of composite plating solution when the volume flow for entering the composite plating solution of plating chamber is Ni-SiC composite platings；
The time of the impactive nickel plating be 5min, during the Ni-SiC composite platings volume flow of composite plating solution be 1.6～
4.5m3/h.1.5 times of electric current when electric current when adjusting impactive nickel plating is Ni-SiC composite platings；The Ni-SiC composite platings
When electric current to the hollow work-piece inner surface electric current density be 8～12.5A/dm2.The temperature of impactive nickel plating is 50～70 DEG C,
The pH value of composite plating solution is 3.9～4.1, and plating time is 30min.
When carrying out impactive nickel plating, in reservoir, SiC content low composite plating solution in upper strata is started the cycle over into pipeline, big
Impactive nickel plating under conditions of volume flow, high current density, obtains the tiny and fine and close prime coat of SiC content, crystal grain, improves multiple
Close the adhesion between coating and matrix.
Step 10：Ni-SiC composite platings.The hand-operated valve that will be connected with lower outlet after completing impactive nickel plating is adjusted to most
Greatly, open compressed air pump.Electromagnetic flowmeter is adjusted, the volume flow for making composite plating solution into plating chamber is 1.6～
4.5m3/h；Electric current is adjusted, the electric current density for making hollow work-piece inner surface is 8～12.5A/dm2.The temperature of Ni-SiC composite platings
For 50～70 DEG C；PH value is 3.9～4.1；Plating time is 25min.
The impactive nickel plating and Ni-SiC composite platings it is total during, 50～83 μm of the sedimentation rate of composite plating solution/
30min。
Step 11：Dismounting hollow work-piece.Compressed air pump and composite plating solution circulating pump are first closed, plating rectification is turned off
Power supply.Composite plating solution in sealing plating chamber is back in reservoir in the presence of self gravitation.Unclamp tight on leading screw
Gu nut, lifts upper fixture, negative electrode conducting ring is exited, take out hollow work-piece.
Step 12：Post processing.The hollow work-piece of composite plating is completed, surface of the work residual is washed off in deionized water
Composite plating solution, under ultrasound wave concussion cleaning 15min, drying.
The hollow work-piece of drying is put into and is heated in 150～200 DEG C of heating furnace and is incubated 1.5～2.5h；Insulation
Cool to room temperature after end with the furnace, obtain the hollow work-piece of composite deposite.Heat treatment after plating is conducive to dehydrogenation and eliminates plating
Layer internal stress, improves coat binding strength.
Using circulation electroplate liquid codeposition technique, can realize that electroplate liquid only contacts hollow work-piece inner surface, only in hollow work
Part inner surface deposits composite deposite, and does not affect hollow work-piece appearance surface state.In the composite plating solution that SiC concentration is 20g/L
In the composite deposite of middle preparation, SiC content is up to 18.8%vol, and the utilization rate of SiC is effectively improved.Ni-SiC composite deposites it is heavy
Product speed is up to 83 μm/30min.Compared with nickel coating, Ni-SiC composite deposites show that roughness is low, even compact, performance
Go out the corrosion proof feature of hard high-wearing feature.
The concrete preparation process of 5 embodiments proposed by the present invention is identical, and difference is the technique in each embodiment
Parameter is different.Table 1 is the technological parameter of each embodiment.
Table 1
2 matrix of table, nickel coating are compared with the corrosion potential and corrosion current of Ni-SiC composite deposites prepared by embodiment 1
| Sample | Corrosion potential (mV) | Corrosion current (μ A/cm2) |
| Hollow work-piece matrix | -421.00 | 17.58 |
| Nickel coating | -314.24 | 0.72 |
| Ni-SiC composite deposites | -267.15 | 0.45 |
Claims (7)
1. a kind of method for preparing hollow work-piece inner surface Ni-SiC composite deposites, it is characterised in that detailed process is：
Step 1：Prepare composite plating solution；
It is that deionized water is formulated with composite plating solution stock solution to prepare composite plating solution；Prepare the desired amount of composite plating solution
When, in proportion deionized water is mixed with composite plating solution stock solution, and carries out air stirring；The air stirring persistent period be 12～
24h；PH acidity regulators and pH alkalescence regulators is adopted to combine and make the pH value of mixed liquor for 4.0 ± 0.1；Obtain composite plating
Liquid；
Step 2：Prepare hollow work-piece；
Step 3：Heat and stir composite plating solution；
Step 4：Process electrode；With 400#The surface of the inner surface and anode conducting rod of liquid honing negative electrode conducting ring；
Step 5：Defat；The antirust oil on hollow work-piece surface is first cleaned with acetone, then carries out heat alkali liquid defat；
Step 6：Corrode；Hollow work-piece after defat is placed in hydrochloric acid solution, by corroding the oxide-film for removing metal surface
With corrosion thing；
Step 7：Activation；Hollow work-piece is placed in into the H that sulfuric acid concentration is 5%2SO4Activated in activated solution, further to remove
The oxide-film on hollow work-piece surface is removed, makes the fresh matrix on hollow work-piece surface fully come out；Hollow work-piece completes activation
Plating is carried out after process；The technological parameter of activation is：Activation temperature≤25 DEG C, soak time is 2min, deionized water rinsing
2min；
Step 8：Hollow work-piece is installed；Negative electrode conducting ring is enclosed within hollow work-piece, and the hollow work of negative electrode conducting ring will be cased with
Part is placed between upper fixture and lower clamp, and adjustment upper fixture, hollow work-piece and lower clamp make the centrage of three overlap；Fastening
Nut on leading screw, makes the contact face seal between hollow work-piece and upper fixture and lower clamp；Opening plating rectifier power source makes hollow
Workpiece is connected with power cathode, carries out cathodic protection to hollow work-piece；
Step 9：Prime coat is prepared in hollow work-piece inner surface；Prime coat is prepared in hollow work-piece inner surface by impactive nickel plating；
Before impactive nickel plating, first close compressed air pump and stop stirring composite plating solution, make composite plating solution stand 20min, SiC microgranules
Free settling, in the composite plating solution of upper strata, SiC fraction of particle is low；When starting impactive nickel plating, will be manual with what upper water-out mouth was connected
Valve is adjusted to maximum, and the hand-operated valve being connected with lower outlet is adjusted to minimum；Electromagnetic flowmeter is adjusted, and makes electricity to be entered during impactive nickel plating
1.5 times of the volume flow of composite plating solution when the volume flow of the composite plating solution in plating chamber is Ni-SiC composite platings；It is described
The time of impactive nickel plating be 5min, during the Ni-SiC composite platings volume flow of composite plating solution be 1.665～
4.587m3/h；1.5 times of electric current when electric current when adjusting impactive nickel plating is Ni-SiC composite platings；The Ni-SiC compound electrics
The electric current density of electric current during plating to the hollow work-piece inner surface is 8～12.5A/dm2；The temperature of impactive nickel plating is 50～70
DEG C, the pH value of composite plating solution is 3.9～4.1；
Step 10：Ni-SiC composite platings；The hand-operated valve that will be connected with lower outlet after completing impactive nickel plating is adjusted to maximum, beats
Open compressed air pump；Electromagnetic flowmeter is adjusted, the volume flow for making composite plating solution into plating chamber is 1.665～
4.587m3/h；Electric current is adjusted, the electric current density for making hollow work-piece inner surface is 8～12.5A/dm2；The temperature of Ni-SiC composite platings
Spend for 50～70 DEG C；PH value is 3.9～4.1；Plating time is 25min；
Impactive nickel plating and Ni-SiC composite platings it is total during, the sedimentation rate of the composite plating solution is 50～83 μm/
30min；
Step 11：Dismounting hollow work-piece；
Step 12：Post processing；The hollow work-piece of composite plating is completed, answering for surface of the work residual is washed off in deionized water
Electroplate liquid is closed, concussion cleaning 15min, drying under ultrasound wave；
The hollow work-piece of drying is put into and is heated in 150～200 DEG C of heating furnace and is incubated 1.5～2.5h；Insulation terminates
After cool to room temperature with the furnace, obtaining inner surface has the hollow work-piece of composite deposite；Heat treatment after plating is conducive to dehydrogenation and eliminates
Coating internal stress, improves coat binding strength.
2. the method for preparing hollow work-piece inner surface Ni-SiC composite deposites as claimed in claim 1, it is characterised in that described multiple
Close electroplate liquid to be made up of nickel sulfate, Nickel dichloride., boric acid, carborundum, saccharin sodium and cetyl trimethylammonium bromide；Per liter is combined
In electroplate liquid respectively the nickel sulfate containing 350～450g/L, the Nickel dichloride. of 10～20g/L, the boric acid of 30～40g/L, 50～
The cetyl trimethylammonium bromide of the carborundum of 70g/L, the saccharin sodium of 2～3g/L and 0.4～0.8g/L；
When preparing composite plating solution stock solution, by the nickel sulfate for weighing, Nickel dichloride. and saccharin sodium and pour in reservoir, start air
Agitating device persistently carries out air stirring, is all dissolved as mixed liquor to nickel sulfate, Nickel dichloride. and saccharin sodium；
The boric acid for weighing is added in the mixed liquor, mixed liquor is heated to into 75 DEG C by the heating rod in reservoir, while holding
It is continuous that air stirring is carried out to mixed liquor, all dissolving to boric acid；In the mixed liquor added with boric acid, add the SiC for weighing micro-
Grain and cetyl trimethylammonium bromide, mix homogeneously, obtain composite plating solution stock solution.
3. the method for preparing hollow work-piece inner surface Ni-SiC composite deposites as claimed in claim 1, it is characterised in that prepare
The composite plating solution of 100L, detailed process are as follows：70L deionized waters are added in reservoir；Each material is weighed in proportion；To claim
The nickel sulfate, Nickel dichloride. and the saccharin sodium that take simultaneously are poured in reservoir, and starting air stirrer persistently carries out air to mixed liquor
Stirring, all dissolving to nickel sulfate, Nickel dichloride. and saccharin sodium；The boric acid for weighing is added in mixed liquor, by reservoir
In heating rod mixed liquor is heated to into 75 DEG C, while persistently carry out air stirring to mixed liquor, all dissolving to boric acid；
The SiC microgranules and cetyl trimethylammonium bromide for weighing is added in the mixed liquor for obtaining, composite plating solution stock solution is obtained；
Deionized water is added in the composite plating solution stock solution for obtaining, the mixed liquor that total amount is 100L is obtained；Groove lid is covered, is continued to mixing
Liquid carries out air stirring, and the persistent period is 12～24h；Combine and make mixed liquor using pH acidity regulators and pH alkalescence regulators
PH value be 4.0 ± 0.1；Obtain composite plating solution.
4. the method for preparing hollow work-piece inner surface Ni-SiC composite deposites as claimed in claim 1, it is characterised in that the standard
Standby hollow work-piece is that hollow work-piece is first carried out stress relief annealing, then is polishing to surface without rusty stain, coats antirust oil, stand-by；Go
The hollow work-piece is heated to into 550 DEG C with stove during stress annealing, 20min is incubated, is cooled to 30 DEG C with the furnace.
5. the method for preparing hollow work-piece inner surface Ni-SiC composite deposites as claimed in claim 1, it is characterised in that described to add
Heat to stir composite plating solution be that the composite plating solution that will be obtained is placed in reservoir, opens air stirring switch, to compound electric
Plating solution carries out 2～3h of air stirring to starting to carry out impactive nickel plating to hollow work-piece；During air stirring, air mass flow be 4～
6m3/h；Starting heater switch to be opened during stirring, composite plating solution being heated, heating-up temperature is 60 DEG C.
6. the method for preparing hollow work-piece inner surface Ni-SiC composite deposites as claimed in claim 1, it is characterised in that described de-
During fat, hollow work-piece is placed in the alkali liquor of preparation and is reacted：The temperature of alkali liquor is 75～85 DEG C；Response time be 3～
5min；With 75～85 DEG C of hot water injection 2min；Deionized water rinses 2min；
Described alkali liquor is by 20～40g/LNaOH, 20～30g/LNa2CO3, 5～15g/LNa3PO4With 5～7mL/LOP emulsifyings
Agent is configured to form.
7. the method for preparing hollow work-piece inner surface Ni-SiC composite deposites as claimed in claim 1, it is characterised in that erosion
Technological parameter is：30%HCl solution is prepared under room temperature, erosion time is 4～6min；After the completion of erosion, deionized water is not carried out
Rinse, directly carry out next step activation processing.
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| CN110129863A (en) * | 2019-03-28 | 2019-08-16 | 中冶赛迪工程技术股份有限公司 | A kind of metal-based nano composite coating and preparation method thereof with wear resistant friction reducing performance |
| CN110938850A (en) * | 2019-12-16 | 2020-03-31 | 南京信息职业技术学院 | Composite nickel electroplating solution, nickel-based nano composite coating and preparation method |
| CN111593381A (en) * | 2020-05-09 | 2020-08-28 | 西北工业大学 | Anode device for preparing Ni-SiC composite coating on inner wall of hollow part |
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| CN109580058B (en) * | 2019-01-23 | 2021-03-09 | 福建省安元光学科技有限公司 | Method for judging stress of die product by utilizing surface roughness of coating |
| CN110129863A (en) * | 2019-03-28 | 2019-08-16 | 中冶赛迪工程技术股份有限公司 | A kind of metal-based nano composite coating and preparation method thereof with wear resistant friction reducing performance |
| CN110938850A (en) * | 2019-12-16 | 2020-03-31 | 南京信息职业技术学院 | Composite nickel electroplating solution, nickel-based nano composite coating and preparation method |
| CN111593381A (en) * | 2020-05-09 | 2020-08-28 | 西北工业大学 | Anode device for preparing Ni-SiC composite coating on inner wall of hollow part |
| CN111593381B (en) * | 2020-05-09 | 2022-04-19 | 西北工业大学 | Anode device for preparing Ni-SiC composite coating on inner wall of hollow part |
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