CN105195737B - A kind of method of SiC particulate surface cladded with nickel - Google Patents
A kind of method of SiC particulate surface cladded with nickel Download PDFInfo
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Abstract
The present invention discloses a kind of method of SiC particulate surface cladded with nickel, belongs to micro particles technical field of surface, it comprises the following steps：1) deoil abatement processes；2) SiC particulate is activated；3) plating, prepare chemical plating fluid, prepare the 40g/L of nickel sulfate hexahydrate 20, the 30g/L of sodium hypophosphite 10, the 50g/L of citric acid 30, the 70g/L of ammonium sulfate 50 deionized water solution, the 10g/L of SiC particulate 5 after activation is taken to be placed in the plating solution prepared, reaction system is placed in 30 40 DEG C of waters bath with thermostatic control in water bath by regulation pH value of solution to 8 12, it is subject to mechanical agitation, obtains the reaction solution after plating；4) post-process.The method of the SiC particulate surface cladded with nickel of the present invention, nickel particle is previously deposited on SiC particulate surface by the method that is activated without palladium, and cladding nickel comprehensively is implemented to SiC particulate by chemical nickel-plating solution, solve the low wetability of SiC particulate, it is difficult to the problem of being combined with molten metal.
Description
Invention field
The invention belongs to micro particles technical field of surface, and in particular to a kind of side of SiC particulate surface cladded with nickel
Method.
Background technology
Silicon-carbide particle has that density is low, hardness is high, elastic modelling quantity is high, thermal coefficient of expansion is small, wear-resisting and corrosion-resistant etc. excellent
Different in nature energy, is a kind of preferable reinforcing material.If it is moulding with height, the metal of excellent toughness is combined, and will be had
There are low cost and the good composite of combination property, therefore strengthen with carborundum the method for metallicity and cause both at home and abroad
The extensive concern of material practitioner.But silicon carbide ceramics particle has higher interface energy, is easily sent out when it is combined with metal body
Raw early fallout, so as to influence it as the application of hard phase, i.e., to synthesize SiC ceramic matrix composite material then needs to solve between different phases
Dispersiveness and boundary moisture sex chromosome mosaicism, this turns into the key point for making composite.Research is found, certain metallics is applied
Overlay on SiC particulate surface and compound particle is made, the interface wet ability and chemical compatibility of SiC and matrix can be improved, after being combined
Material has that specific strength is high, wear-resistant, thermal coefficient of expansion is small, low excellent properties of cost and this advanced composite is current
It is widely used in the numerous areas such as Aeronautics and Astronautics, automobile, chemical industry, electronics.
Metal ion is set to be reduced into metal in the presence of reducing agent using metal salt solution, in the plating with catalytic surface
The method that metal deposition layer is obtained on part is referred to as chemical plating.Chemical nickel plating has extraordinary covering power, and adhesion is high, technique
Simply, it is with low cost, it can carry out metalized to non-conductive matrix, and also chemical Ni-plating layer has that hardness is high, wear-resisting, corrosion resistant
The performances such as erosion.Metallic cover type ceramic particle refers to coat the composite ceramics that one layer of out-phase metal is constituted in ceramic grain surface
Grain, has the premium properties of clad metal and core ceramics concurrently, can be by the features such as the obdurability of metal material, workability and pottery
The high temperature resistant of ceramic material, wear-resistant and corrosion-resistant etc. performance combine.
The content of the invention
Goal of the invention：It is an object of the invention to provide a kind of method of SiC particulate surface cladded with nickel, SiC is not only solved
The low wetability of particle, it is difficult to the problem of being combined with molten metal, and comprehensive cladding is implemented to SiC particulate by chemical nickel-plating solution
Nickel.
Technical scheme：For achieving the above object, the present invention is adopted the following technical scheme that：
A kind of method of SiC particulate surface cladded with nickel, comprises the following steps：
1) deoil abatement processes
Original SiC particle cleaning is deoiled decontamination, SiC particulate is then cleaned with deionized water to neutrality, after filtering drying
Obtain pretreated SiC particulate；
2) SiC particulate is activated
Pretreated SiC particulate is activated using the alcoholic solution of organic nickel；First prepare activating solution, the water of nickel acetate four
10-20g/L, sodium borohydride 2-6g/L configures its ethanol solution；The SiC particulate 10-40g/L of cleaning is taken, preparation is added to
In good activating solution, and reaction system is placed in 30-40 DEG C of water bath, after mechanic whirl-nett reaction, SiC activated
Grain；It is specifically that 2-6g sodium borohydride granules are placed in beaker, use anhydrous second by the particle water of 10-20g nickel acetates four to prepare activating solution
Alcoholic solution does solvent configuration activating solution, and is settled to 1L；Then SiC particulate 10-40g clean after pretreatment is taken, is added to just
In the activating solution configured；
3) plating
Chemical plating fluid is prepared, nickel sulfate hexahydrate 20-40g/L, sodium hypophosphite 10-30g/L, citric acid 30-50g/ is prepared
L, ammonium sulfate 50-70g/L deionized water solution takes the SiC particulate 5-10g/L after activation to be placed in the plating solution prepared, will
Reaction system is placed in 30-40 DEG C of water bath with thermostatic control in water bath, is subject to mechanical agitation, and regulation pH value of solution is obtained after plating to 8-12
Reaction solution；Chemical plating fluid is prepared to specifically refer to weigh nickel sulfate hexahydrate 20-40g, sodium hypophosphite 10-30g, citric acid 30-
50g, ammonium sulfate 50-70g is placed in beaker, and solvent configuration chemical plating fluid is made of deionized water solution, 1L is settled to, then takes work
SiC particulate 5-10g after change is placed in the chemical plating fluid just configured；
4) post-process
Reaction solution after plating is staticly settled, filtered, 80-90 DEG C of more than 10h drying in air dry oven is placed in, obtains
Surface is by the SiC particulate of nickel coated.
Step 1) in, described abatement processes of deoiling are first to carry out absolute ethyl alcohol ultrasonic cleaning successively to original SiC particle
5-10min, 5%wt NaOH solution are cleaned by ultrasonic 5-10min, 10%vol hydrochloric acid solution and are cleaned by ultrasonic 5-10min, after filtering
SiC particulate is cleaned to neutrality with deionized water again, is placed in air dry oven and dries, and oven temperature is 80-90 DEG C, time 10h
More than, until it is dry and hard, obtain pretreated SiC particulate.
Step 1) in, described abatement processes of deoiling are directly to be cleaned by ultrasonic 5-10min with acetone to original SiC particle,
SiC particulate is cleaned to neutrality with deionized water again after filtering, is placed in air dry oven and dries, and oven temperature is 80-90 DEG C, when
Between more than 10h, until dry and hard, obtain pretreated SiC particulate.
Step 2) in, described churned mechanically mixing time 30-60min, rotating speed 300-400r/min, in course of reaction
Middle dropwise addition 5%wt NaOH solution used as stabilizers；Reaction terminate after, reaction solution is stood, precipitated, filter after be placed in 10h in baking oven
Dry above, oven temperature is 80-90 DEG C, the SiC particulate activated.
Step 3) in, described churned mechanically mixing time is 40min-80min, rotating speed 300-400r/min.
Beneficial effect：Compared with prior art, the method that SiC particulate surface of the invention deposits nickel, by being activated without palladium
Method be previously deposited nickel particle on SiC particulate surface, and cladding nickel comprehensively is implemented to SiC particulate by chemical nickel-plating solution,
Solve the low wetability of SiC particulate, it is difficult to the problem of being combined with molten metal.By in chemical plating fluid, removing stabilizer, make it
Fast reaction, more thick nickel particle cladding is realized on the surface of SiC particulate, from scanning result we can see that.With
This simultaneously, EDS scanning results are displayed without the presence of P element, the often Ni-P coating that traditional nickel plating technology is realized, obtain
Be more pure nickel coated.
Brief description of the drawings
Fig. 1 is the SiC particulate SEM photograph after activating in embodiment 1；
Fig. 2 is the SiC particulate SEM photograph after plating in embodiment 1；
Fig. 3 randomly selects the EDS testing results of the SiC particulate after activation；
Fig. 4 is to randomly select the EDS testing results of SiC particulate after plating in embodiment 1；
Fig. 5 is the SiC particulate SEM photograph after activating in embodiment 2；
Fig. 6 is the SiC particulate SEM photograph after plating in embodiment 2；
Fig. 7 is to randomly select the EDS testing results of SiC particulate after plating in embodiment 2；
Fig. 8 is the SiC particulate SEM photograph after plating in embodiment 3；
Fig. 9 is the EDS testing results that SiC particulate after plating is randomly selected in embodiment 3；
Figure 10 is the SiC particulate SEM photograph after plating in embodiment 4；
Figure 11 is the EDS testing results that SiC particulate after plating is randomly selected in embodiment 4.
Embodiment
With reference to specific embodiment, the present invention is described further.
Element is C, O, Ni, Si, Pt, Ni from left to right in Fig. 3.Element is C, Ni, Si, Pt, Ni from left to right in Fig. 4.
Element is C, O, Ni, Si, Pt, Ni, Pt from left to right in Fig. 7.Element is C, O, Ni, Si, Pt, Ni, Pt from left to right in Fig. 9.
Element is C, O, Ni, Si, Pt, Ni from left to right in Figure 11.
Embodiment 1
1) quantitative former SiC particulate is taken, acetone is cleaned by ultrasonic SiC particulate 5min, cleaned afterwards with deionized water to neutrality, mistake
Filter, is placed in air dry oven 80 DEG C, 10h dry for standby；
2) SiC particulate after 40g cleanings is taken, 1L anhydrous second of the formula for nickel acetate four water 20g, sodium borohydride 6g is placed in
In alcoholic solution, reaction system is placed in 30 DEG C of waters bath with thermostatic control, and adds mechanical agitation 300r/min, soak time 30min, course of reaction
The middle a small amount of NaOH solution of addition makees stabilizer, after question response terminates, stands, and precipitation filtering is placed in air dry oven 80 DEG C,
10h drying is stand-by；Fig. 1 is the SiC particulate SEM photograph after activating in embodiment 1, and SiC is can be seen that from the picture after activation
The particle surface success a little Ni of plating, but being uniformly distributed on its surface is not realized；
3) take 10g activate after SiC particulate, grind 1min, configure chemical plating fluid 1L, be formulated as nickel sulfate hexahydrate 30g, it is secondary
Sodium phosphite 25g, citric acid 50g, ammonium sulfate 70g, plus deionized water is to 1L specifications；Plating solution is placed in 30 DEG C of constant water bath box
In, with NaOH and H2SO4Solution adjust pH to 8.0, the SiC after grinding is added in plating solution, while plus mechanical agitation, rotating speed
300r/min, reaction time 40min, after question response terminates, plating solution is staticly settled, filtering, is placed in air dry oven 80 DEG C,
10h is dried, and obtains the SiC particulate of nickel coated；Fig. 2 is the SiC particulate SEM photograph after plating in embodiment 1, the SiC particulate after plating
Surface is evenly distributed with point-like nickel particle, can not realize its complete cladding to SiC particulate, as can be seen from Figure 2 particle
Surface has most of exposed.
The SiC particulate of the nickel coated obtained to embodiment 1 randomly selects carry out spectroscopy detection, and Fig. 3 is SiC after activation
The EDS testing results of grain, wherein, except C, outside Si, with the presence of the Ni that mass fraction is 6%, wherein Pt is sample making course metal spraying
The doping of processing.Fig. 4 is the EDS testing results (power spectrum result) that SiC particulate is randomly selected after plating, and display is containing mass fraction
24.81% nickel is attached to particle surface.
Embodiment 2
1) quantitative SiC particulate is taken, is placed in absolute ethyl alcohol and is cleaned by ultrasonic 5min, the NaOH that 5%wt is placed in after filtering is molten
Be cleaned by ultrasonic 5min in liquid, filter, be placed in 10%vol hydrochloric acid solutions and be cleaned by ultrasonic 5min, filter, cleaned with deionized water to
Neutrality, is placed in air dry oven, 80 DEG C of dry for standby；
2) SiC particulate after 20g cleanings is taken, 1L anhydrous second of the formula for nickel acetate four water 20g, sodium borohydride 6g is placed in
In alcoholic solution, reaction system is placed in 30 DEG C of waters bath with thermostatic control, and adds mechanical agitation 400r/min, soak time 45min, course of reaction
The middle a small amount of NaOH solution of addition makees stabilizer, after question response terminates, stands, and precipitation filtering is placed in air dry oven 80 DEG C,
10h drying is stand-by；Fig. 5 is the SiC particulate SEM photograph after activation, and the SiC particulate surface attachment after activation has point-like nickel
Grain, and be distributed more uniform；
3) take 5g activate after SiC particulate, grind 1min, configure chemical plating fluid 1L, be formulated as nickel sulfate hexahydrate 26g, it is secondary
Sodium phosphite 20g, citric acid 44g, ammonium sulfate 66g, plus deionized water is to 1L specifications.Plating solution is placed in 40 DEG C of constant water bath box
In, with NaOH and H2SO4 solution adjust pH to 9.0, the SiC after grinding is added in plating solution, while plus mechanical agitation, rotating speed
400r/min, reaction time 60min, after question response terminates, plating solution is staticly settled, filtering, is placed in air dry oven 80 DEG C,
10h is dried, and obtains the SiC particulate of nickel coated.Fig. 6 is the SiC particulate SEM photograph after plating in embodiment 2, the sample SEM after plating
As a result show, a large amount of nickel particles are successfully attached to the surface of SiC particulate, and realize complete cladding substantially.
The SiC particulate of the nickel coated obtained to embodiment 2 randomly selects carry out spectroscopy detection, Fig. 7 for SiC particulate after plating with
The EDS testing results (power spectrum result) that machine is chosen, to show and be attached to particle surface containing mass fraction for 65.17% nickel, plate
Cover effect fine.
Embodiment 3
1) quantitative SiC particulate is taken, is placed in absolute ethyl alcohol and is cleaned by ultrasonic 5min, the NaOH that 5%wt is placed in after filtering is molten
Be cleaned by ultrasonic 5min in liquid, filter, be placed in 10%vol hydrochloric acid solutions and be cleaned by ultrasonic 5min, filter, cleaned with deionized water to
Neutrality, is placed in air dry oven, 90 DEG C of dry for standby；
2) SiC particulate after 20g cleanings is taken, 1L anhydrous second of the formula for nickel acetate four water 10g, sodium borohydride 2g is placed in
In alcoholic solution, reaction system is placed in 30 DEG C of waters bath with thermostatic control, and adds mechanical agitation 400r/min, soak time 60min, course of reaction
The middle a small amount of NaOH solution of addition makees stabilizer, after question response terminates, stands, and precipitation filtering is placed in air dry oven 90 DEG C,
10h drying is stand-by；
3) take 10g activate after SiC particulate, grind 1min, configure chemical plating fluid 1L, be formulated as nickel sulfate hexahydrate 25g, it is secondary
Sodium phosphite 20g, citric acid 40g, ammonium sulfate 65g, plus deionized water is to 1L specifications.Plating solution is placed in 40 DEG C of constant water bath box
In, with NaOH and H2SO4 solution adjust pH to 10.0, the SiC after grinding is added in plating solution, while plus mechanical agitation, turn
Fast 300r/min, reaction time 80min, after question response terminates, plating solution is staticly settled, filtering, is placed in 80 in air dry oven
DEG C, 10h drying obtains the SiC particulate of nickel coated.
Fig. 8 is the SiC particulate SEM photograph after plating in embodiment 3；Fig. 9 is that SiC particulate after plating is randomly selected in embodiment 3
EDS testing results；From the point of view of SEM and EDS results, when pH is 10, plating effect is poor, and nickel particle fails uniform in surface of SiC
It is distributed and is distributed in nickel bulk, it is exposed than more serious.
Embodiment 4
1) quantitative SiC particulate is taken, is placed in absolute ethyl alcohol and is cleaned by ultrasonic 10min, the NaOH that 5%wt is placed in after filtering is molten
It is cleaned by ultrasonic 10min in liquid, filters, be placed in 10%vol hydrochloric acid solutions and be cleaned by ultrasonic 10min, filters, cleaned with deionized water
To neutral, it is placed in air dry oven, 80 DEG C of dry for standby；
2) SiC particulate after 20g cleanings is taken, 1L anhydrous second of the formula for nickel acetate four water 10g, sodium borohydride 2g is placed in
In alcoholic solution, reaction system is placed in 30 DEG C of waters bath with thermostatic control, and adds mechanical agitation 300r/min, soak time 45min, course of reaction
The middle a small amount of NaOH solution of addition makees stabilizer, after question response terminates, stands, and precipitation filtering is placed in air dry oven 80 DEG C,
10h drying is stand-by；
3) take 10g activate after SiC particulate, grind 1min, configure chemical plating fluid 1L, be formulated as nickel sulfate hexahydrate 25g, it is secondary
Sodium phosphite 20g, citric acid 45g, ammonium sulfate 65g, plus deionized water is to 1L specifications.Plating solution is placed in 40 DEG C of constant water bath box
In, with NaOH and H2SO4Solution adjust pH to 12.0, the SiC after grinding is added in plating solution, while plus mechanical agitation, rotating speed
300r/min, reaction time 80min, after question response terminates, plating solution is staticly settled, filtering, is placed in air dry oven 80 DEG C,
10h is dried, and obtains the SiC particulate of nickel coated.
Figure 10 is the SiC particulate SEM photograph after plating in embodiment 4；Figure 11 is that SiC is randomly selected after plating in embodiment 4
The EDS testing results of grain.In embodiment 4, the sample that pH is prepared when being 12, in experimentation, reaction is violent, there is the wadding of black
Shape Ni is generated, from the point of view of SEM results, Ni form generation change, and skewness, fails complete coated Si/C.Random constituency
EDS results show that Ni mass fraction also only has 32.32%.
1~4 analysis is understood in conjunction with the embodiments, pH be 8,9,10, the test results of 12 4 groups of examples can be seen that and work as pH
During equal to 9, Ni is best to the Surface coating effect of SiC particulate, although Ni realizes the part to SiC particulate surface under other conditions
Cladding, but exposed surface of SiC has the higher surface can, however it remains wetability difference shortcoming, can not be with as hardening constituent
Parent metal realizes good interface cohesion.
Claims (1)
1. a kind of method of SiC particulate surface cladded with nickel, it is characterised in that comprise the following steps：
1) deoil abatement processes
Original SiC particle cleaning is deoiled decontamination, SiC particulate is then cleaned with deionized water to neutrality, obtained after filtering drying
Pretreated SiC particulate；
2) SiC particulate is activated
Pretreated SiC particulate is activated using the alcoholic solution of organic nickel；First prepare activating solution, the water 10- of nickel acetate four
20g/L, sodium borohydride 2-6g/L configures its ethanol solution；The SiC particulate concentration 10-40g/L of cleaning is taken, preparation is added to
In good activating solution, and reaction system is placed in 30-40 DEG C of water bath, after mechanic whirl-nett reaction, SiC activated
Grain；
3) plating
Chemical plating fluid is prepared, nickel sulfate hexahydrate 20-40g/L, sodium hypophosphite 10-30g/L, citric acid 30-50g/L, sulphur is prepared
Sour ammonium 50-70g/L deionized water solution, takes the SiC particulate concentration 5-10g/L after activation to be placed in the plating solution prepared, adjusts
PH value of solution is saved to 8-12, reaction system is placed in 30-40 DEG C of water bath with thermostatic control in water bath, is subject to mechanical agitation, is obtained after plating
Reaction solution；
4) post-process
Reaction solution after plating is staticly settled, filtered, 80-90 DEG C of more than 10h drying in air dry oven is placed in, obtains surface
By the SiC particulate of nickel coated；Step 1) in, described abatement processes of deoiling are first to carry out anhydrous second successively to original SiC particle
The NaOH solution that alcohol is cleaned by ultrasonic 5-10min, 5%wt is cleaned by ultrasonic 5-10min, 10%vol hydrochloric acid solution ultrasonic cleaning 5-
10min, SiC particulate is cleaned to neutrality after filtering with deionized water again, is placed in air dry oven and is dried, oven temperature is 80-
90 DEG C, more than time 10h, until it is dry and hard, obtain pretreated SiC particulate；Step 2) in, described churned mechanically stirring
Time 30-60min, rotating speed 300-400r/min；Reaction terminate after, reaction solution is stood, precipitated, filter after be placed in baking oven
More than 10h is dried, and oven temperature is 80-90 DEG C, the SiC particulate activated；Step 3) in, described churned mechanically stirring
Time is 40min-80min, rotating speed 300-400r/min.
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| CN106929835A (en) * | 2017-03-02 | 2017-07-07 | 苏州金仓合金新材料有限公司 | Chemical plating fluid and use its method to SiC particulate Surface coating Ni P |
| CN107475697B (en) * | 2017-08-14 | 2019-10-11 | 江苏大学 | A kind of carbon nano tube surface chemical Ni-P plating plating solution and method |
| CN108118315A (en) * | 2018-02-24 | 2018-06-05 | 唐山师范学院 | A kind of method of the uniform and stable silicon carbide powder chemical nickel plating on surface of coating |
| CN110273096B (en) * | 2019-06-28 | 2021-01-08 | 鞍钢股份有限公司 | SiC/M2 powder high-speed steel composite material and preparation method thereof |
| CN111185594B (en) * | 2020-02-19 | 2022-06-21 | 中北大学 | Preparation method of nickel-coated ceramic composite powder based on selective laser melting molding |
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