CN106929835A - Chemical plating fluid and use its method to SiC particulate Surface coating Ni P - Google Patents
Chemical plating fluid and use its method to SiC particulate Surface coating Ni P Download PDFInfo
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- CN106929835A CN106929835A CN201710120413.7A CN201710120413A CN106929835A CN 106929835 A CN106929835 A CN 106929835A CN 201710120413 A CN201710120413 A CN 201710120413A CN 106929835 A CN106929835 A CN 106929835A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
- C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1635—Composition of the substrate
- C23C18/1639—Substrates other than metallic, e.g. inorganic or organic or non-conductive
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1851—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
- C23C18/1872—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment
- C23C18/1886—Multistep pretreatment
- C23C18/1893—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
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- Chemical Kinetics & Catalysis (AREA)
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemically Coating (AREA)
- Electroplating Methods And Accessories (AREA)
Abstract
The present invention relates to a kind of chemical plating fluid, it is used for SiC particulate Surface coating Ni P, the invention further relates to using the chemical plating fluid, to the method for SiC particulate Surface coating Ni P, it comprises the following steps：1) surface of SiC cleaning treatment；2) SiC particulate roughening；3) SiC particulate activation sensitization；4) chemical plating fluid and plating are prepared；5) chemical plating posttreatment.As [Ni in chemical plating fluid2+] concentration be 0.25mol/L, [NH4 +] concentration be 0.6mol/L, [Ni2+]/[H2PO2 ‑] the ratio between concentration is 0.4, citric acid concentration is 0.1mol/L, and trace lactic acid and thiocarbamide when surface of SiC parcel effect it is best.The present invention implements cladding nickel comprehensively to SiC particulate by chemical nickel-plating solution, solves the low wetability of SiC particulate, the difficult problem being combined with molten metal, and the chemical plating fluid maintenance cost is low, long service life.
Description
Technical field
The invention belongs to micro particles technical field of surface, and in particular to a kind of chemical plating fluid, it is used for SiC
Grain Surface coating Ni-P, the invention further relates to using the chemical plating fluid is to the method for SiC particulate Surface coating Ni-P and thus obtains
The SiC particulate for obtaining.
Background technology
The requirement of conventional high-temperature alloy has big crystallite dimension even monocrystalline, because the crystal grain of alloy material is smaller, it is brilliant
Interfacial area is bigger, and atoms permeating is easier, so the verting and deforming and mould by crystal grain in the presence of high temperature and stress
Property deformation so that alloy material creep speed accelerate, shorten its high-temperature and durable.And it is distributed in dystectic pottery of crystal boundary
Porcelain particle has obvious Grain boundary pinning to act on, and substantially reduces metallic atom grain boundary diffusion speed, while crystal boundary is to dislocation
Effective inhibition is played in movement, improves the high temperature yield stress of alloy material, therefore compared to traditional coarse-grain high temperature alloy
Material has more preferable elevated temperature strength, stability and enduring quality.Therefore, it is proposed to large scale crystal grain is excellent with ceramic particle
Point is attached in high temperature alloy.
However, the wetability between ceramic particle and metal material is bad, to solve this problem, it is usually taken to ceramics
The method of particle surface deposited nickel layer.At present, there are plating and two kinds of main methods of chemical plating in ceramic grain surface deposited metal,
Wherein plating needs applying direct current source device, relatively costly, and chemical nickel plating does not need applying direct current source device then, is a kind of
Excellent process for treating surface, a range of application is obtained in many industrial departments.
Specifically, electroless plating method refers to make reducing metal ions Cheng Jin in the presence of reducing agent using metal salt solution
Category, the method that metal deposition layer is obtained on the plating piece with catalytic surface.Chemical nickel plating has extraordinary covering power, knot
High with joint efforts, process is simple is with low cost, can carry out metalized to non-conductive matrix, and chemical Ni-plating layer has hardness
The performance such as high, wear-resisting, corrosion-resistant.Metallic cover type ceramic particle refers to coat one layer of out-phase metal in ceramic grain surface to constitute
Composite ceramic particle, have concurrently clad metal and core ceramics premium properties, can be by the obdurability of metal material, easy processing
The performance such as the high temperature resistant of the features such as property and ceramic material, wear-resistant and corrosion-resistant combines.
Have in terms of the sedimentation mechanism of chemical plating Mi-P alloy four kinds of hypothesis, i.e. atomic hydrogen theory, hydride transmission theory,
Electrochemical theory and the nickel ion coordination theory of light base one.What wherein degree of recognition was higher is atomic hydrogen theoretical, according to the theory,
During chemical plating Mi-P alloy, there is following process：
The first step：Dehydrogenation generates orthophosphite ions to hypophosphorous acid root in solution in the solution, while releasing nascent state
Atomic hydrogen, nascent state atomic hydrogen is adsorbed in catalytic surface so as to be allowed to activate, and the cation nickel in plating solution is reduced, and in catalysis
Metallic nickel is deposited on surface, its reaction equation is as follows：
H2PO2 -+H2O→HPO3 2-+2H++[H]-
Ni2++2[H]-→Ni+H2↑ (evolving hydrogen reaction).
Second step：Part hypophosphorous acid root be hydrogenated thing be reduced into it is elemental phosphorous, while into coating, its reaction equation is as follows：
2H2PO2 -+6[H]-+4H2O→2P+8OH-+5H2↑。
But, there are the following problems compared with electroplating solution for chemical nickel-plating solution：Condition requirement precision is higher, Ge Xianghua
The balance that studies point, the operable scope of technological parameter are narrow；Tolerance for pollutant is poor, or even ppm
The heavy metal ion of level may cause coating performance deterioration or plating leakage, stop plating；In view of the life-span of chemical plating fluid, compare plating
For liquid, the stability of the mixed solution of chemical nickel plating is very poor, in addition it is also necessary to the work safeguarded to solution and adjusted, relatively number
It is tired.This problem why is had, chemical nickel plating is primarily due to and is overcome any surface defect without external force startup and help, reacted
That abutment surface condition starts, i.e. out-phase surface self-catalyzed reaction, unlike this, it is anti-to drive that plating then provides electric power by the external world
The carrying out answered.
The content of the invention
In consideration of it, the present inventor is desirable to provide a kind of new chemical plating fluid, during its use without complicated
Service procedure and long service life, in addition, the present inventor be also directed to it is a kind of to SiC particulate surface carry out activation and
Be sensitized pretreatment activation sensitizing solution, to solve the low wetability of SiC particulate, it is difficult to molten metal be combined problem, and realize it is right
SiC particulate coats nickel-phosphor comprehensively.
For achieving the above object, the present invention is adopted the following technical scheme that：
An a kind of specific embodiment of the invention, there is provided chemical plating fluid, it is used to carry out SiC particulate
The Surface coating of Ni-P, it includes following component：Six hydration nickel sulfate, sodium hypophosphite, ammonium sulfate, trisodium citrate and
Lactic acid and thiocarbamide.
Chemical plating fluid according to an embodiment of the invention, wherein, the six hydration nickel sulfate concentration is 0.05-
0.25mol/L, the concentration of the sodium hypophosphite is 0.08-1.25mol/L, and the ammonium sulfate concentrations are 0.5-0.9mol/L,
The content of the trisodium citrate is 0.1-0.5mol/L, and the lactic acid and thiocarbamide are trace.
Chemical plating fluid according to an embodiment of the invention, wherein, the pH for adjusting the chemical plating fluid is 8-10, temperature
It is 30-50 degrees Celsius.
Chemical plating fluid according to an embodiment of the invention, wherein, the six hydration nickel sulfate concentration is 0.25mol/
L, the concentration of the sodium hypophosphite is 0.625mol/L, and the ammonium sulfate concentrations are 0.6mol/L, the trisodium citrate
Content is 0.1mol/L.
According to one embodiment of present invention without activation sensitization pretreatment, wherein, described activation activation process is not implemented,
Example as a comparison, it was demonstrated that the good result of activation sensitizing solution.
A specific embodiment of the invention, there is provided one kind is using any chemical plating fluid pair as described above
The method of SiC particulate Surface coating Ni-P, it comprises the following steps.
Step one：SiC particulate cleaning treatment
Absolute ethyl alcohol, NaOH solution and hydrochloric acid solution are carried out successively to SiC particulate cleaning to be cleaned by ultrasonic, and then use deionization
Water cleaning SiC particulate obtains pretreated SiC particulate to neutrality, after filtering drying.
Step 2：SiC particulate roughening treatment
The SiC particulate that gained is processed through the step one is put into coarsening solution, and applies magnetic agitation, be roughened
SiC particulate afterwards.
Step 3：SiC particulate activates sensitized treatment
To be placed in activation sensitizing solution by the SiC particulate after the roughening obtained by the step 2, and reaction system is put
In 30-40 DEG C of water bath, apply ul-trasonic irradiation, standing, precipitation, deionized water washing and filtering drying, are lived afterwards
Change the SiC particulate of sensitization.
Step 4：Chemical plating is carried out to SiC particulate
Any one of the 250mL according to Claims 1 to 4 will be added to through the SiC particulate 5g of step 3 activation sensitization
In described chemical plating fluid, reaction system is placed in 30-50 DEG C of water bath with thermostatic control in water bath, and apply magnetic agitation.
5) subsequent treatment
The reaction solution of step 4 treatment is staticly settled, is filtered, more than 10h is dried at being placed in 80-90 DEG C, obtain table
Face is by the SiC particulate of nickel coated.
Method to SiC particulate Surface coating Ni-P according to an embodiment of the invention, wherein, in the step one
In, the ultrasonic cleaning time of the absolute ethyl alcohol is 5-10min；The NaOH solution is the NaOH solution of 5 mass %, and ultrasound is clear
Wash 5-10min；The hydrochloric acid is the pure hydrochloric acid solution of 37 mass %, is cleaned by ultrasonic 5-10min, after alkali cleaning and pickling processes
The SiC particulate precipitate and cleaned with deionized water again after filtering to SiC particulate in neutrality, SiC particulate is precipitated to obtain afterwards, will
The SiC particulate dries more than 10h at being placed in 80-90 DEG C.
Method to SiC particulate Surface coating Ni-P according to an embodiment of the invention, wherein, in the step 2
In, the coarsening solution is pure hydrochloric acid and deionized water by 37 mass % with volume ratio 1:1 is formulated, during the magnetic agitation
Between be 20min, stirring terminate after, by reaction solution stand, precipitate and be filtrated to get SiC particulate, clean with deionized water filter institute
Obtain SiC particulate 3 times, the SiC particulate being roughened.
Method to SiC particulate Surface coating Ni-P according to an embodiment of the invention, wherein, in the step 2
In, the SiC particulate corresponding to coarsening solution 300mL additions is 10-40g.
Method to SiC particulate Surface coating Ni-P according to an embodiment of the invention, wherein, in the step 3
In, the action time of the ultrasonic wave is 20min, after reaction terminates, reaction solution is stood, precipitates and filter, and uses deionized water
SiC particulate obtained by filtering is cleaned 3 times, more than 10h is dried at the SiC particulate after cleaning is placed in into 80-90 DEG C, lived
The SiC particulate of change.
Method to SiC particulate Surface coating Ni-P according to an embodiment of the invention, wherein, the activation sensitization
Liquid is consisted of：
Palladium chloride 0.5g/L, two hydrated stannous chloride 30g/L, sodium chloride 160g/L, 37 mass %HCl 60mL/L.
By above technical scheme, the present invention mainly achieves following technique effect：
(1) compared with plating, it is not necessary to which applying direct current source device, gained plated layer compact, hole is few；May be implemented in gold
Plating on the various different substrate materials such as category, nonmetallic, semiconductor；The metal being evenly distributed can be introduced by the ceramics of fragility
To improve its fracture toughness；Covering power is strong, can make the powder after cladding metal phase be mutually unified into it is netted.
(2) compared with other electroless plating methods, this technique has advantages below：1) surface of SiC treatment is sensitized using activation
One-step method, step simplifies compared with activation sensitization two-step method widely used at present.After traditional sensitization activation two-step method treatment,
Remain in the stannous ion in powder to be difficult to remove, usually the performance to powder brings detrimental effect, and its technique is cumbersome, operation
Complexity, it is difficult in maintenance.Unlike this, activation sensitization one-step method low cost of the invention, raw material prepares easy, meanwhile, in activation
Comprising villaumite (as a example by NaCl) as liquid stabilizer in sensitizing solution；2) traditional handicraft have ignored the solution composition of selection in hydrolysis
During the hydrogen ion that produces and the influence that is caused to the pH of plating solution of hydroxide ion, and stated for the composition of chemical plating fluid
Differ, this technique be fully directed to when under conditions of alkaline low-temperature to surface of SiC chemical Ni-P plating chemical plating fluid each into
The selection for dividing, it is with strong points.
Brief description of the drawings
Fig. 1 (a) and Fig. 1 (b) are respectively the SEM photograph and EDS analysis results of the SiC particulate after roughening；
Fig. 2 (a) and Fig. 2 (b) are respectively SEM photograph and the EDS analyses of the SiC particulate after activation sensitization；
Fig. 3 is the percentage weight increase change of each group experiment；
Fig. 4 is the SEM photograph of gained SiC particulate in embodiment 1；
Fig. 5 is the testing result of the EDS of the particle of the SiC for randomly selecting gained in embodiment 1；
Fig. 6 is the SEM photograph of the SiC particulate of gained in embodiment 2；
Fig. 7 is the EDS testing results of the SiC particulate for randomly selecting gained in embodiment 2；
Fig. 8 is the SiC particulate SEM photograph of gained in embodiment 3；
Fig. 9 is the EDS testing results of the SiC particulate for randomly selecting gained in embodiment 3；
Figure 10 is the SiC particulate SEM photograph of gained in comparative example 3；
Figure 11 is the EDS testing results of the SiC particulate for randomly selecting gained in comparative example 3.
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, below in conjunction with the accompanying drawings and embodiment, it is right
The present invention is further elaborated.It should be appreciated that specific embodiment described herein is only used to explain the present invention, not
For limiting the present invention.
Specific implementation step in the present invention to SiC particulate Surface coating Ni-P includes cleaning treatment, the SiC of SiC particulate
The roughening treatment of particle, the activation sensitized treatment of SiC particulate and chemical plating and chemical plating post processing.
1) cleaning treatment of SiC particulate
Original SiC particle cleaning is deoiled decontamination using pickling+alkali cleaning, then clean SiC particulate with deionized water into
Property, pretreated SiC particulate is obtained after filtering drying, detailed process is as follows：
Quantitative SiC particulate is taken, is placed in and is cleaned by ultrasonic 5min in absolute ethyl alcohol, the NaOH that 5 mass % are placed in after filtering is molten
It is cleaned by ultrasonic 5min in liquid, filters, be placed in the pure hydrochloric acid solution of 37 mass % and be cleaned by ultrasonic 5min, filter, uses deionized water
Cleaning is placed in air dry oven, dry for standby at 80 DEG C to neutrality；
2) roughening treatment of SiC particulate
Coarsening solution is made into using hydrochloric acid and deionized water, then the SiC powder 10-40g of cleaned treatment is put into 300mL
Magnetic agitation in coarsening solution, the SiC particulate after being roughened, its detailed process is as follows：
The SiC particulate after 20g cleaning treatments is taken, the pure hydrochloric acid and deionized water of 37 mass % by volume 1 is placed in:1
In the 300mL coarsening solutions being prepared from；20nin being reacted under magnetic stirring, after question response terminates, being stood, precipitation filtering is placed in
80 DEG C in air dry oven, 10h drying is stand-by；Fig. 1 (a) and Fig. 1 (b) are respectively the SiC particulate SEM photograph and EDS after roughening
Analysis, table 1 is then the EDS analysis results of the SiC particulate after roughening, and the picture from after roughening can be seen that SiC particulate surface
Smoother.
Table 1：The EDS analysis results of the SiC particulate after roughening
| Element | Wt% | Atomic percent |
| C | 62.16 | 79.34 |
| Si | 37.84 | 20.66 |
| Total amount | 100.00 | 100.00 |
3) the activation sensitized treatment of SiC particulate
Activation sensitization is carried out to the SiC particulate after roughening using activation sensitization one-step method.
Preparing activation sensitization detailed process is：By 0.25g PdCl2It is added in the HCl solution of 37 mass % of 30mL,
50mL or so is settled to deionized water obtain solution A；80g NaCl are dissolved in 250mL deionized waters again, obtain solution B；
Solution A is mixed with B again, 5min is stirred with glass bar, obtain solution C；Again by 15g SnCl2·2H2O be dissolved in 150mL go from
In sub- water, solution D is obtained；Solution D is stirred again while be added in solution C, obtain bottle-green solution E；Finally plus
Enter deionized water, with volumetric flask constant volume to 500mL, that is, obtain bottle-green activating solution.The SiC particulate after cleaning and roughening is taken to put
In the activation sensitizing solution, addition is 20-40g/L, and reaction system is placed in 30-40 DEG C of water bath, is subject to ultrasonic wave
Effect 20min, after reaction terminates, reaction solution is stood, precipitates, cleaned with deionized water 3 times, after filtering, is placed in baking oven
80-90 DEG C of drying more than 10h, obtains the SiC particulate of activation sensitization.
Fig. 2 (a) and Fig. 2 (b) are respectively the SiC particulate SEM photograph and EDS analyses after activation sensitization, and table 2 is activation sensitization
The EDS analysis results of SiC particulate afterwards, as it is clear from fig. 2 that SiC particulate surface is relatively rough, contain palladium ion simultaneously, and its is specific
Each element content is referring to table 2.
Table 2：The EDS analysis results of the SiC particulate after activation sensitization
| Element | Wt% | Atomic percent |
| C | 43.48 | 64.54 |
| Si | 55.63 | 35.31 |
| Pd | 0.89 | 0.15 |
| Total amount | 100.00 | 100.00 |
4) chemical plating
Configuration chemical plating fluid：Configuration six hydration nickel sulfate concentration is 0.05-0.25mol/L, and ortho phosphorous acid na concn is
0.08-1.25mol/L, ammonium sulfate concentrations are 0.5-0.9mol/L, and the content of trisodium citrate is 0.1-0.5mol/L, Yi Jihen
The lactic acid and thiocarbamide of amount, 250mL solution is settled to deionized water, then adjusts to 8-10 pH value of solution, by activated sensitization
The SiC particulate 5g for the treatment of is placed in chemical plating fluid 250mL, and reaction system is placed in into 30-50 DEG C of water bath with thermostatic control in water bath, is subject to
Magnetic agitation 60min, obtains the reaction solution after plating.
In order to specifically discuss each content for constituting with orthogonal test, from 6 factors of selection：[Ni2+] concentration, [Ni2 +]/[H2PO2 -] concentration, [NH4 +] concentration, citric acid concentration, pH, temperature, test level select 5 levels, design orthogonal test
Design table, it is as shown in table 3 below.
Table 3：The orthogonal test designs table of chemical plating
Design orthogonal test 25, with percentage weight increase m%=(m-m before and after chemical platingo)/mo(m represents SiC powder after plating
The weight of body, moRepresent the weight that original SiC is added, 5.0000g) degree of SiC particulate plated surface Ni-P degree is carried out
Evaluate, the percentage weight increase change of its result each group experiment as shown in Figure 3.
Embodiment 1 (orthogonal experiment 20)
Configuration chemical plating fluid 250mL, the specific composition of the chemical plating fluid is that six hydration nickel sulfate concentration is 0.20mol/L, secondary
The concentration of sodium phosphite is 0.333mol/L, and ammonium sulfate concentrations are 0.7mol/L, and the content of trisodium citrate is 0.1mol/L, with
And the lactic acid and thiocarbamide of trace, it is settled to 250mL solution with deionized water.
Take the SiC particulate 5g after activation sensitization and be placed in the plating solution (thus, the content of SiC particulate is 20g/L in plating solution),
Be placed in for reaction system and react 60min, question response in water bath under 40 DEG C of waters bath with thermostatic control, magnetic agitation by regulation pH value of solution to 9.5
After end, plating solution is staticly settled, filtered, be placed in 80 DEG C in air dry oven, 10h drying obtains the SiC particulate of nickel coated；
Fig. 4 is the SiC particulate SEM photograph after plating in embodiment 1, and the SiC particulate surface after plating is evenly distributed with point-like nickel particle, also not
Its cladding completely to SiC particulate can be realized, as can be seen from Figure 2 particle surface has most of exposed.
The SiC particulate of the nickel coated obtained to embodiment 1 ESEM 500 × times under randomly select and carry out power spectrum inspection
Survey, Fig. 5 and Biao 4 is the EDS testing results of the SiC particulate after the plating of embodiment 1, wherein, in addition to C, Si, there is the mass fraction to be
1.36% P is present, and mass fraction is that 34.00% nickel is attached to particle surface.
Table 4：The EDS testing results of the SiC particulate after the plating of embodiment 1
| Element | Wt% | Atomic percent |
| C | 7.62 | 18.92 |
| O | 2.46 | 4.59 |
| Si | 53.83 | 57.20 |
| P | 2.08 | 2.01 |
| Ni | 34.00 | 17.28 |
| Total amount | 100.00 | 100.00 |
Embodiment 2 (orthogonal experiment 16)
Configuration chemical plating fluid 250mL, the chemical plating fluid composition is that six hydration nickel sulfate concentration is 0.20mol/L, secondary phosphorous
The concentration of sour sodium is 1.0mol/L, and ammonium sulfate concentrations are 0.8mol/L, and the content of trisodium citrate is 0.2mol/L, and trace
Lactic acid and thiocarbamide, be settled to 250mL solution with deionized water.
Take the SiC particulate 5g after activation sensitization and be placed in the plating solution for preparing that (thus, the content of SiC particulate is in plating solution
20g/L), be placed in reaction system in water bath and react 60min under 40 DEG C of waters bath with thermostatic control, magnetic agitation by regulation pH value of solution to 10,
After question response terminates, plating solution is staticly settled, filtered, be placed in air dry oven and dry 10h at 80 DEG C, obtain nickel coated
SiC particulate.Fig. 6 is the SiC particulate SEM photograph after plating in embodiment 2, and the SiC particulate surface after plating is uniformly distributed born of the same parents' shape nickel
Grain, relatively realizes its cladding completely to SiC particulate.
The SiC particulate of the nickel coated obtained to embodiment 2 ESEM 500 × times under randomly select and carry out power spectrum inspection
Survey, Fig. 7 and Biao 5 is the EDS testing results of the SiC particulate after the plating of embodiment 2, wherein, in addition to C, Si, there is the mass fraction to be
2.16% P is present, and mass fraction is that 36.50% nickel is attached to particle surface.
Table 5：The EDS testing results of the SiC particulate after the plating of embodiment 2
| Element | Wt% | Atomic percent |
| C | 28.25 | 54.16 |
| O | 4.48 | 6.46 |
| Si | 28.61 | 23.46 |
| P | 2.16 | 1.60 |
| Ni | 36.50 | 14.32 |
| Total amount | 100.00 | 100.00 |
Embodiment 3 (orthogonal experiment 23)
Configuration chemical plating fluid 250mL, the composition of the chemical plating fluid is that six hydration nickel sulfate concentration is 0.25mol/L, secondary Asia
The concentration of sodium phosphate is 0.625mol/L, and ammonium sulfate concentrations are 0.6mol/L, and the content of trisodium citrate is 0.1mol/L, and
The lactic acid and thiocarbamide of trace, 250mL solution is settled to deionized water.
Take the SiC particulate 5g after activation sensitization and be placed in the plating solution for preparing that (thus, the content of SiC particulate is in plating solution
20g/L), be placed in reaction system in water bath and react 60min under 45 DEG C of waters bath with thermostatic control, magnetic agitation by regulation pH value of solution to 10,
After question response terminates, plating solution is staticly settled, filtered, be placed in air dry oven and dry 10h at 80 DEG C, obtain nickel coated
SiC particulate.In experimentation, reaction is violent, and the cotton-shaped Ni for having black is generated, and Fig. 8 is the SiC particulate after plating in embodiment 3
SEM photograph, the SiC particulate surface after plating is uniformly distributed born of the same parents' shape nickel particle, the cladding completely of SiC particulate.
The SiC particulate of the nickel coated obtained to embodiment 3 ESEM 500 × times under randomly select and carry out power spectrum inspection
Survey, Fig. 9 and Biao 6 is the EDS testing results of the SiC particulate after the plating of embodiment 3, wherein, except C, outside Si, there is the mass fraction to be
2.65% P is present, and mass fraction is that 53.26% nickel is attached to particle surface.
Table 6：The EDS testing results of the SiC particulate after the plating of embodiment 3
| Element | Wt% | Atomic percent |
| C | 17.87 | 42.37 |
| O | 3.64 | 6.47 |
| Si | 22.58 | 22.89 |
| P | 2.65 | 2.43 |
| Ni | 53.26 | 25.83 |
| Total amount | 100.00 | 100.00 |
In addition, in order to inquire into activation influence of the activation process to chemical plating effect, with comparative example 3 pairs without activation sensitization
SiC particulate carries out chemical Ni-P plating.
Comparative example 3
Activation sensitization is not carried out except SiC pretreatments are not carried out, treatment same as Example 3 is carried out, its specific steps is such as
Under：
1) quantitative SiC particulate is taken, is placed in and is cleaned by ultrasonic 10min in absolute ethyl alcohol, the NaOH of 5 mass % is placed in after filtering
It is cleaned by ultrasonic 10min in solution, filters, be placed in 37 mass % hydrochloric acid solutions and be cleaned by ultrasonic 10min, filter, uses deionized water
Cleaning is placed in air dry oven, 80 DEG C of dry for standby to neutrality；
2) SiC particulate after 20g cleanings is taken, the hydrochloric acid and deionized water of 37 mass % by volume 1 is placed in:1 prepares
300mL coarsening solutions in；20nin being reacted under magnetic stirring, after question response terminates, being stood, precipitation filtering is placed in air blast
10h is dried in drying box at 80 DEG C stand-by；
3) chemical plating fluid 250mL is configured, the chemical plating fluid composition is that six hydration nickel sulfate concentration is 0.25mol/L, secondary Asia
The concentration of sodium phosphate is 0.625mol/L, and ammonium sulfate concentrations are 0.6mol/L, and the content of trisodium citrate is 0.1mol/L, and
The lactic acid and thiocarbamide of trace, 250mL solution is settled to deionized water.The SiC particulate 5g for taking not activated sensitization is placed in preparation
In good plating solution (that is, SiC particulate content is 20g/L), reaction system is placed in 45 DEG C of perseverances in water bath by regulation pH value of solution to 10
60min is reacted under tepidarium, magnetic agitation, after question response terminates, plating solution is staticly settled, filtered, be placed in air dry oven
80 DEG C, 10h drying.
Figure 10 is the SiC particulate SEM photograph after plating in comparative example 3；Figure 11 and Biao 7 be surface sweeping Electronic Speculum randomly select 500 ×
The EDS testing results of SiC particulate after being plated in comparative example 3 under times.In comparative example 3, the sample prepared when pH is 10, from SEM results
From the point of view of, the form generation change of Ni, and skewness, fail complete coated Si/C.The EDS results in random constituency show, Ni's
Mass fraction also only has 19.60%.As can be seen here, activation sensitization is indispensable important step, and activation of the invention is quick
Change serves important facilitation to chemical nickel plating.
Table 7：The EDS testing results of SiC particulate after being plated in comparative example 3
| Element | Wt% | Atomic percent |
| C | 33.52 | 57.00 |
| O | 4.04 | 5.15 |
| Si | 41.01 | 29.82 |
| P | 1.83 | 1.21 |
| Ni | 19.60 | 6.82 |
| Total amount | 100.00 | 100.00 |
Knowable to binding analysis embodiment 1~3 and comparative example 3, pre-treatment is carried out to original SiC quite important while preparing six
Hydrated sulfuric acid nickel concentration is 0.25mol/L, and the concentration of sodium hypophosphite is 0.625mol/L, and ammonium sulfate concentrations are 0.6mol/L,
The content of trisodium citrate be 0.1mol/L, and trace lactic acid and thiocarbamide, be settled to 250mL solution with deionized water, take
SiC particulate 20g/L after activation sensitization is placed in the plating solution for preparing, and reaction system is placed in water-bath by regulation pH value of solution to 10
45 DEG C of waters bath with thermostatic control, are subject to magnetic agitation in groove, obtain the reaction solution after plating, and surface of SiC parcel effect is best.
That is, as [Ni in chemical plating fluid2+] concentration be 0.25mol/L, [NH4 +] concentration be 0.6mol/L, [Ni2+]/
[H2PO2 -] the ratio between concentration is 0.4, citric acid concentration is 0.1mol/L, and trace lactic acid and thiocarbamide when, surface of SiC parcel
Effect is best.Although Ni is realized to the part on SiC particulate surface cladding under other conditions, exposed surface of SiC have compared with
Surface high can, however it remains wetability difference shortcoming, can not realize good interface cohesion with parent metal as hardening constituent.Together
When, activation sensitization plays an important roll for surface of SiC plating Ni-P.
5) chemical plating posttreatment
Reaction solution after plating is staticly settled, is filtered, be placed in air dry oven drying more than 10h at 80-90 DEG C, obtained
To surface by the SiC particulate of nickel coated.
Presently preferred embodiments of the present invention is the foregoing is only, not for limiting practical range of the invention；If do not taken off
From the spirit and scope of the present invention, the present invention is modified or equivalent, all should covered in the claims in the present invention
In the middle of protection domain.
Claims (10)
1. a kind of chemical plating fluid, its Surface coating for being used to carry out SiC particulate Ni-P, it is characterised in that comprising following component：
Six hydration nickel sulfate, sodium hypophosphite, ammonium sulfate, trisodium citrate and lactic acid and thiocarbamide.
2. chemical plating fluid according to claim 1, it is characterised in that the six hydration nickel sulfate concentration is 0.05-
0.25mol/L, the concentration of the sodium hypophosphite is 0.08-1.25mol/L, and the ammonium sulfate concentrations are 0.5-0.9mol/L,
The content of the trisodium citrate is 0.1-0.5mol/L, and the lactic acid and thiocarbamide are trace.
3. chemical plating fluid according to claim 1 and 2, it is characterised in that the pH of the regulation chemical plating fluid is 8-10, temperature
Spend is 30-50 DEG C.
4. chemical plating fluid according to claim 1 and 2, it is characterised in that the six hydration nickel sulfate concentration is
0.25mol/L, the concentration of the sodium hypophosphite is 0.625mol/L, and the ammonium sulfate concentrations are 0.6mol/L, the lemon
The content of sour trisodium is 0.1mol/L.
5. side of a kind of chemical plating fluid using as described in any one of Claims 1 to 4 to SiC particulate Surface coating Ni-P
Method, it is characterised in that comprise the following steps：
Step one：SiC particulate cleaning treatment
Absolute ethyl alcohol, NaOH solution and hydrochloric acid solution are carried out successively to SiC particulate cleaning to be cleaned by ultrasonic, it is then clear with deionized water
SiC particulate to neutrality is washed, pretreated SiC particulate is obtained after filtering drying；
Step 2：SiC particulate roughening treatment
The SiC particulate that gained is processed through the step one is put into coarsening solution, and applies magnetic agitation, after being roughened
SiC particulate；
Step 3：SiC particulate activates sensitized treatment
To be placed in activation sensitizing solution by the SiC particulate after the roughening obtained by the step 2, and reaction system is placed in 30-
In 40 DEG C of water baths, apply ul-trasonic irradiation, standing, precipitation, deionized water washing and filtering drying, obtain activation and be sensitized afterwards
SiC particulate；
Step 4：Chemical plating is carried out to SiC particulate
250mL will be added to through the SiC particulate 5g of step 3 activation sensitization according to any one of Claims 1 to 4
Chemical plating fluid in, reaction system is placed in 30-50 DEG C of water bath with thermostatic control in water bath, and apply magnetic agitation；
5) subsequent treatment
The reaction solution of step 4 treatment is staticly settled, is filtered, more than 10h is dried at being placed in 80-90 DEG C, obtain surface quilt
The SiC particulate of nickel coated.
6. method according to claim 5, it is characterised in that in the step one, the ultrasound of the absolute ethyl alcohol is clear
The time is washed for 5-10min；The NaOH solution is the NaOH solution of 5 mass %, is cleaned by ultrasonic 5-10min；The hydrochloric acid is 37
The pure hydrochloric acid solution of quality %, be cleaned by ultrasonic 5-10min, by alkali cleaning and pickling processes after the SiC particulate precipitation and mistake
Cleaned to SiC particulate in neutrality with deionized water again after filter, SiC particulate is precipitated to obtain afterwards, the SiC particulate is placed in 80-90
More than 10h is dried at DEG C.
7. method according to claim 5, it is characterised in that in the step 2, the coarsening solution is by 37 matter
The pure hydrochloric acid and deionized water of % are measured with volume ratio 1:1 is formulated, and the magnetic agitation time is 20min, after stirring terminates,
Reaction solution is stood, is precipitated and is filtrated to get SiC particulate, filtering gained SiC particulate is cleaned with deionized water 3 times, be roughened
SiC particulate.
8. method according to claim 5, it is characterised in that in the step 2, corresponding to the coarsening solution 300mL
The SiC particulate of addition is 10-40g.
9. the method for a kind of SiC particulate surface cladded with nickel according to claim 5, it is characterised in that in the step 3
In, the action time of the ultrasonic wave is 20min, after reaction terminates, reaction solution is stood, precipitates and filter, and uses deionized water
SiC particulate obtained by filtering is cleaned 3 times, more than 10h is dried at the SiC particulate after cleaning is placed in into 80-90 DEG C, lived
The SiC particulate of change.
10. method according to claim 5, it is characterised in that the activation sensitizing solution is consisted of：
Palladium chloride 0.5g/L, two hydrated stannous chloride 30g/L, sodium chloride 160g/L, 37 mass %HCl 60mL/L.
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| CN111185594A (en) * | 2020-02-19 | 2020-05-22 | 中北大学 | Preparation method of nickel-coated ceramic composite powder based on selective laser melting molding |
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