CN106507852B - A kind of chemical plating nickel-phosphorus alloy method in silicon carbide ceramics substrate - Google Patents
A kind of chemical plating nickel-phosphorus alloy method in silicon carbide ceramics substrateInfo
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- CN106507852B CN106507852B CN201010050076.7A CN201010050076A CN106507852B CN 106507852 B CN106507852 B CN 106507852B CN 201010050076 A CN201010050076 A CN 201010050076A CN 106507852 B CN106507852 B CN 106507852B
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Abstract
The present invention relates to a kind of method for carrying out nickel-phosphorus alloy plating by electroless plating technology in silicon carbide ceramics substrate, it is characterised in that：(1) oil removing and cleaning are carried out with reference to the ultrasonic cleaning mode of acetone, ethanol to silicon carbide substrate using " deionized water soaks in advance "；(2) before carrying out Metal Palladium activation, high-temperature oxydation is carried out to substrate first, then is corroded with Fluohydric acid., to strengthen the bond strength of chemical deposit and substrate；(3) activated using ionic palladium activating solution, can be prevented effectively from interference of the stannous ion to plating solution, and acid mist to equipment, environment, operator harm；(4) using the acidic bath plating in ultra-smooth or coarse silicon carbide ceramics substrate based on sodium hypophosphite, plated layer compact is smooth, in non crystalline structure；(5) after through chemical plating surface modification, by the heat treatment process under high temperature and different atmosphere, make amorphous nickel-phosphorus coating that crystallization to occur, so as to increase substantially the mechanical performance of coating hardness, wearability etc..
Description
Technical field
The present invention relates to a kind of surface modifying method in non-metal material surface metal lining, particularly relate to
And a kind of method of the plating nickel-phosphorus alloy in silicon carbide ceramics substrate.
Background technology
Carborundum (SiC) is as a kind of ultra hard ceramic material, with a series of excellent physical and chemical performances,
Such as higher elastic modelling quantity, moderate density, less thermal coefficient of expansion, higher thermal conductivity factor and resistance to
Impact property, high specific stiffness, dimensional stability of height etc., are increasingly becoming preparation space optics material
First choice, and applied within the specific limits.High performance spatial optical elements requirement has super
High smooth surface (surface roughness ＜ 1nmRMS), it is tired that this make it that carbofrax material faces following two aspect
It is difficult：(1) because SiC material specific stiffness is big, chemical stability is high, it is difficult to straight by mechanical polishing method
Obtain to obtain high-quality SiC optical surfaces；(2) full solid SiC material is directly prepared extremely difficult, it is residual
The defects such as the stomata stayed can influence processing quality, finally influence surface quality.At present, for above-mentioned
The conventional solution of problem is：1) surface modification is carried out to SiC material, it is high fine and close in its coating surface
Coating, is then polished to coating；2) SiC material optical fabrication new method is developed.Wherein,
SiC ceramic surface be coated with silicon, silica, nickel, nickel-chrome alloy layer method application it is more universal, plating
Method processed is typically such as sputtered using physical method, electron beam evaporation, chemical vapor deposition.However, thing
Though logos, which prepares SiC modified layers, that good adhesion, plated layer compact, defect are few, its equipment is held high
Expensive, complex operation, and be difficult to be coated with compared with thick film layers and large-size workpiece.Therefore, how inquire into low
The electroless plating technology of cost realizes that the surface of silicon carbide ceramics is modified, so as to realize the quick plating compared with thick film layers
System and large-size workpiece are coated with, significant.
" chemical plating " is also known as " electroless-plating ", is that one kind utilizes redox reaction with catalysis
Activity metal or non metallic substrate on generation metal or alloy coating method [Li Ning,《Chemical plating practicality skill
Art》, Chemical Industry Press, 2004/1], at present at metal material (such as stainless steel, alloy material)
Surface anticorrosion antirust treatment [" it is high that one kind is used for 304 stainless steel surfaces to Chinese patent 200710170300.4
The chemical plating bath of phosphorus chemistry plating Ni-P alloys ", 200810120010.3 are " before chemical nickel plating of zinc/aluminum-based alloy
Processing and application " ,] and plastic wear-resisting conductive processing [" one kind use of Chinese patent 200810142571.3
In the selective chemical plating method of plastic basis material "] in terms of in be used widely.But chemical plating ceramics,
Application especially in terms of the modification of silicon carbide ceramics surface, has not yet to see report.
Chemical plating is a kind of utilization redox reaction on the metal or non metallic substrate with catalytic activity
The method for generating metal or alloy coating.Carried out when on the non-metallic material such as plastics, ceramics, glass surface
During chemical plating, it is necessary to activated to substrate, its surface is set to deposit one layer of catalyst with catalytic activity
Layer (such as palladium), otherwise can not just carry out chemical plating.SiC ceramic surface be modified another difficult point be, its
Unusual light after the polishing of surface, the coating of plating high bond strength is also stranded very much in this ultra-smooth substrate
It is difficult.It yet there are no the patent or document for the chemical plating nickel-phosphorus alloy for being related to ultra-smooth SiC ceramic substrate
Report.
The content of the invention
The present invention is intended to provide one kind chemical nickeling phosphorus alloy film method in SiC ceramic substrate, can be with
Realization is coated with surface reforming layer in the silicon carbide ceramics substrate of various surface state.Particularly, it is of the invention
The method provided includes a kind of unique SiC ceramic surface coarsening technique, one kind and utilizes novel ion palladium
The SiC ceramic surface activation of solution and sensitizing technology.
The chemical plating surface modification technology for the SiC ceramic substrate that present aspect is provided includes following content：(1)
Oil removing and cleaning；(2) surface high-temp is aoxidized；(3) surface coarsening；(4) ionic palladium sensitization, activation；
(5) chemical plating nickel-phosphorus alloy；(6) plating posttreatment.
The surface of chemical plating nickel-phosphorus alloy of the present invention, which is modified, includes six steps：
Step one：Oil removing and cleaning.Oil removing purpose is removed in SiC ceramic preparation, processing, transportation
Grease, dust, organic matter remnants that may be remained on surface etc., so that nickel-phosphorus alloy coating and substrate knot
Close firm.In practical application, " Solvent degreasing " and " alkaline solution oil removing " is two kinds and common removed
Oily method.Due to the porosity characteristic on silicon carbide ceramics surface, the present invention, which is used, stronger penetration to micropore
" Solvent degreasing " method.In addition, to prevent that electrochemical deoiling liquid from largely penetrating into ceramic micro-cracks
Interior influence quality of coating and ceramic performance, can soak a period of time before oil removing with deionized water, allow ceramics
Hole suction moisture.Cleaning generally uses organic solvent or alkalescent degreasing fluid, is aided with ultrasound with more
The degreasing fluid being immersed in ceramic capillary is thoroughly removed, in order to avoid the follow-up chemical nickel plating of influence.
Therefore, SiC ceramic oil removing of the invention, cleaning are followed successively by：1.SiC ceramic bases are in deionization
Soaked 1-30 minutes in water, do not apply ultrasound or be cleaned by ultrasonic.2.SiC ceramic bases immersion acetone is molten
In agent, it is cleaned by ultrasonic 1-30 minutes；In 3.SiC ceramic bases immersion alcohol solvent, it is cleaned by ultrasonic 1-30 points
Clock；4. with deionized water clean substrate surface, dry at ambient temperature or baking oven in dry for standby.
Step 2：Surface high-temp is aoxidized.
The SiC ceramic substrate surface for roughness very little polished through oversintering, and SiC is difficult to and otherization in normal temperature
Thing reaction is learned, is also difficult to obtain suitable roughness on surface using coarsening solution.Due to SiC and nickel-phosphorus alloy
The thermal coefficient of expansion of material differs larger (Ni-P alloys：12~14.5 × 10-6/K；SiC：4.7×10-6/ K),
When taking out workpiece from high temperature plating solution, coating peeling, even phenomenon of rupture are often produced.In SiC potteries
Ceramic liner basal surface introduces silicon oxide intermediate, then can alleviate this by coating caused by thermal expansion coefficient difference
Peeling and phenomenon of rupture.
The surface high-temp oxidation technology of SiC ceramic substrate is：800-1500 DEG C of oxidizing temperature, especially
1000-1200℃；Oxidization time 1-48 hours, especially 4-12 hours.
Step 3：Surface coarsening；Ceramics are with the interaction of nickel-phosphorus alloy coating, prolonging brilliant, diffusion and key
The effect of conjunction is very faint, and the combination of coating and matrix surface is mainly by mechanical bond, therefore matrix
Pattern influences notable to the adhesion of coating and matrix.
For the SiC ceramic substrate by high-temperature oxydation, its roughening process is：Hydrofluoric acid coarsening solution is selected,
Its composition is --- the hydrofluoric acid (HF) of 40% mass concentration: concentrated ammonia liquor (28% mass concentration): water=
1-100ml: 1-40ml: 100-1000ml, especially hydrofluoric acid (HF): concentrated ammonia liquor: water=20-60ml:
5-20ml∶100-500ml.Coarsening Temperature is room temperature~60 DEG C, especially 1~60min of coarsening time, 2-10
Minute.After roughening, potsherd is taken out, rinsed repeatedly with deionized water, dry for standby.
Step 4：Ionic palladium activation, sensitization；The purpose of ionic palladium activation is that deposition obtains colloid in substrate
Pd nano particle；The purpose of sensitization is " dispergation ", and metal Pd nano particle body is exposed, with
The follow-up plating process of catalysis.Mainly there are three kinds currently for the chemical plating activation method of non metallic substrate：
(a) sensitization activation two-step method；(b) colloid palladium solution activation method；(c) ionic palladium activation method.Due to
First two method uses stannous ion and concentrated acid, therefore activating solution is unstable, and acid mist is to equipment, ring
Border, operating personnel's harm are very big.Therefore, the present invention is entered using advanced ionic palladium activating solution to SiC ceramic
Row activation.
The composition of ionic palladium activating solution is：Palladium bichloride: ammonium chloride: α-aminopyridine: water=0.1-1.0
Gram: 0.1-1.0 grams: 0.1-10 gram: 100-5000 grams.Activating process is：By above-mentioned steps
(3) the SiC ceramic substrate of surface coarsening is placed in above-mentioned ionic palladium activating solution, and temperature control is in room temperature~60
DEG C, soak time is 1-60 minutes, especially 5-20 minute.
Palladium bichloride is sensitized reducing process：Sensitizing solution by 10-200 grams/L sodium hypophosphite solution composition, it is quick
Change temperature is room temperature~60 DEG C, and soak time is 1-60 minutes, especially 5-20 minute.
Step 5：Chemical plating nickel-phosphorus alloy；The species of chemical nickel-plating solution is a lot, is gone back with sodium hypophosphite
The chemical nickel-plating solution of former agent is most widely used, can be divided into acid and alkali plating solution by pH value.Alkali plating solution is obtained
The coating phosphorus content obtained is lower than acidic bath, and coating voidage is larger, and acidic bath sedimentation rate is fast,
The coating of acquisition is finer and close.The need for being modified according to silicon carbide ceramics chemical plating, the present invention is using acid plating
Liquid carries out plating to SiC ceramic.
The composition of described acidic bath is：Nickel sulfate: sodium hypophosphite: lactic acid: citric acid
Sodium: sodium iodide=10-30g/L: 10-30g/L: 10-50ml/L: 10-30g/L: 1-10mg/L.
The pH value control of plating solution is carried out in 4.5-5.5. chemical platings in constant temperature water bath, and useful load is 0.1-5
dm2/ L, the temperature of plating is maintained at 85~95 DEG C, and the time of plating is 1h-6h.The plated layer compact light of gained
It is sliding, in non crystalline structure, and have stronger optical manufacturing characteristic and characteristic resistant to chemical etching.
Step 6：It is heat-treated after plating., can be in height after the cleaned drying of the SiC ceramic that chemical plating is modified
Temperature is lower to be heat-treated.Treatment conditions are：200-600 DEG C of temperature；Time 1-24 hour, heat-treating atmosphere
Can be air, oxygen, nitrogen or argon gas etc..
The features of the present invention：
1. it is a feature of the present invention that in oil removing, cleaning process in SiC ceramic substrate, first to base
Bottom carries out deionized water immersion, so that ceramic surface hole is fully absorbed, so as to avoid electrochemical deoiling liquid
It is a large amount of to penetrate into influence quality of coating in ceramic micro-cracks.In addition, present invention use acetone, ethanol is super
Sound cleaning carries out SiC ceramic substrate oil removing, and effect and efficiency are superior to conventional alkali liquor oil removing.
2. it is a feature of the present invention that before SiC ceramic substrate carries out Metal Palladium activation, first substrate is entered
Row high-temperature oxydation, makes silicon carbide surface layer be reacted with the oxygen in environment, generation and substrate carborundum adhesion
Abnormal firm silicon oxide layer, is then corroded by hydrofluoric acid to the silicon oxide layer again, is produced porous
Structure, so as to strengthen the bond strength of chemical deposit and SiC substrates.It is exactly based on above-mentioned high-temperature oxydation-corruption
Erosion is handled, and just can be coated with the nickel-phosphorus alloy coating of high bond strength on the silicon carbide ceramics surface of ultra-smooth.
3. it is a feature of the present invention that SiC ceramic substrate is lived using new ionic palladium activating solution
Change, it is to avoid interference of the stannous ion to plating solution, and acid mist to equipment, environment, operating personnel danger
Evil, activating solution is also more stablized, and can preserve the several years never degenerates.
4. it is a feature of the present invention that using the acidic bath based on sodium hypophosphite in ultra-smooth or coarse
Silicon carbide ceramics substrate on plating, not only sedimentation rate is very fast, and plated layer compact is smooth, in amorphous
Structure, with stronger optical manufacturing characteristic and characteristic resistant to chemical etching.
5. it is a feature of the present invention that modified through chemical plating surface in SiC ceramic substrate, by height
Heat treatment process under temperature and different atmosphere, crystallizes amorphous nickel-phosphorus coating, so as to significantly carry
The mechanical performance of high coating, such as hardness, wearability.Make SiC ceramic substrate that nickel-phosphorus alloy is presented peculiar
Metallic luster.The adhesive force cut of coating is determined (the results detailed in reality using WS-2005 testers
Apply shown in example 2 and 4 and Fig. 3)
Brief description of the drawings
The X-ray of Electroless Ni-P Coating is spread out in the silicon carbide ceramics substrate that Fig. 1 is prepared according to embodiment 1
Penetrate collection of illustrative plates；Fig. 1 (a) is the diffracting spectrum of silicon carbide ceramics substrate, and Fig. 1 (b) is implementation chemical nickel plating
The diffracting spectrum of sample after phosphorus.
The polishing silicon carbide ceramics substrate chemical nickel phosphorus plating for 80 millimeters of the diameter that Fig. 2 is prepared according to embodiment 1
Alloy sample photo and electron scanning micrograph；Fig. 2 (a) is SiC silicon carbide ceramics before chemical plating
Substrate photo；Fig. 2 (b) is the modified SiC silicon carbide ceramics substrate photo of chemical plating；Fig. 2 (c) is
The modified SiC silicon carbide ceramics substrate scanning electron microscope test photo of chemical plating.
Fig. 3 is modified sample according to polishing silicon carbide ceramics chemical plating surface prepared by embodiment 2 and embodiment 4
The cut test result of product；The nickel-phosphorus alloy that wherein Fig. 3 (a) is prepared for not thermally treated embodiment 2
Coating；The nickel-phosphorus alloy coating that Fig. 3 (b) is prepared for thermally treated embodiment 2；Fig. 3 (c) is real
Apply the coating of the nickel-phosphorus alloy of the preparation of example 4.
Embodiment
Embodiment 1：
(1) oil removing and cleaning.The polishing SiC ceramic for selecting a diameter of 80 millimeters is chemical plating substrate.SiC
Ceramic bases, which are first placed in deionized water, soaks 10 minutes, then ultrasonic in acetone and alcohol solvent respectively
Cleaning 10 minutes, finally cleans substrate surface with deionized water, is placed in dry for standby in 105 DEG C of baking ovens.
(2) surface high-temp is aoxidized.SiC ceramic substrate is placed in Muffle furnace after oil removing, cleaning and drying
Middle carry out high-temperature oxydation, 1000 DEG C of oxidizing temperature, oxidization time 6 hours.
(3) surface coarsening.SiC ceramic substrate is after high-temperature oxydation, and selection hydrofluoric acid coarsening solution enters to it
Row roughening treatment, hydrofluoric acid (HF) of the hydrofluoric acid coarsening solution containing 40% mass concentration, concentrated ammonia liquor, moisture
Wei not be 24 milliliters, 9 milliliters and 200 milliliters, Coarsening Temperature is 30 DEG C, coarsening time 5min.After roughening,
Potsherd is taken out, rinsed repeatedly with deionized water, dry for standby in 105 DEG C of baking ovens is placed in.
(4) ionic palladium activation, sensitization；SiC substrates after roughening are carried out using following ionic palladium activating solution
Activation, ionic palladium activating solution chloride containing palladium, ammonium chloride, α-aminopyridine, water are respectively 0.5 gram, 0.3
Gram, 1 gram and 1000 grams.SiC ceramic substrate through surface coarsening is placed in above-mentioned ionic palladium activating solution, in
5 minutes at 60 DEG C.Then, SiC substrates are transferred in 100 grams/L ortho phosphorous acid sodium solution, 60
It is sensitized 5 minutes at DEG C.
(5) chemical plating nickel-phosphorus alloy；Activated, sensitization SiC substrates then carry out plating process,
Plating solution is constituted：Nickel sulfate: sodium hypophosphite: lactic acid: sodium citrate: sodium iodide=28g/L:
25g/L∶30ml/L∶20g/L∶4mg/L.The pH value of plating solution is controlled 4.8.Chemical plating is in constant temperature
Carried out in water bath, useful load is 2dm2/ L, the temperature of plating is maintained at 88 DEG C, and the time of plating is 1h.
With deionized water cleaning workpiece after the completion of chemical plating, it is placed in 105 DEG C of baking ovens and dries, you can obtain table
The silicon carbide sample of face plating nickel-phosphorus alloy coating.
The X ray diffracting spectrum explanation that accompanying drawing 1 is provided, after plating process, silicon carbide substrate is complete
Covered entirely by nickel phosphor coating, the intrinsic relatively low diffraction maximum of silicon carbide substrate is blanked completely, and higher diffraction
The intensity at peak is also greatly lowered.Meanwhile, after plating on sample diffraction collection of illustrative plates widthization nickel amorphous peak (~450)
It is non crystalline structure to show gained coating.
The sample object photo and electron scanning micrograph that accompanying drawing 2 is provided show, through chemical plating table
Face is modified, and significant change occurs for SiC ceramic surface state, and the distinctive metallic luster of nickel-phosphorus alloy is presented,
SEM photograph shows that film surface is fine and close, uniform, exists without any Micro porosity or defect, shows institute
Obtain the high-quality and high-compactness of coating.
Embodiment 2：
(1) oil removing and cleaning.The polishing SiC ceramic for selecting a diameter of 80 millimeters is chemical plating substrate.SiC
Ceramic bases, which are first placed in deionized water, to be cleaned by ultrasonic 10 minutes, then respectively in acetone and alcohol solvent
It is cleaned by ultrasonic 10 minutes, substrate surface is finally cleaned with deionized water, dry for standby in 105 DEG C of baking ovens is placed in.
(2) surface high-temp is aoxidized.SiC ceramic substrate is placed in Muffle furnace after oil removing, cleaning and drying
Middle carry out high-temperature oxydation, 1200 DEG C of oxidizing temperature, oxidization time 12 hours.
(3) surface coarsening.SiC ceramic substrate is after high-temperature oxydation, and selection hydrofluoric acid coarsening solution enters to it
Row roughening treatment, hydrofluoric acid (HF) of the hydrofluoric acid coarsening solution containing 40% mass concentration, concentrated ammonia liquor, moisture
Wei not be 24 milliliters, 9 milliliters and 200 milliliters, Coarsening Temperature is 50 DEG C, coarsening time 2min.After roughening,
Potsherd is taken out, rinsed repeatedly with deionized water, dry for standby in 105 DEG C of baking ovens is placed in.
(4) ionic palladium activation, sensitization；SiC substrates after roughening are carried out using following ionic palladium activating solution
Activation, ionic palladium activating solution chloride containing palladium, ammonium chloride, α-aminopyridine, water are respectively 0.8 gram, 0.5
Gram, 1 gram and 1000 grams.SiC ceramic substrate through surface coarsening is placed in above-mentioned ionic palladium activating solution, in
Activated 20 minutes under room temperature condition.Then, SiC substrates are transferred to 100 grams/L ortho phosphorous acid sodium solution
In, it is sensitized 20 minutes at ambient temperature.
(5) chemical plating nickel-phosphorus alloy；Activated, sensitization SiC substrates then carry out plating process,
Plating solution composition is: nickel sulfate: sodium hypophosphite: lactic acid: sodium citrate: sodium iodide=30g/L:
25g/L∶25ml/L∶20g/L∶4mg/L.The pH value of plating solution is controlled 4.8.Chemical plating is in constant temperature
Carried out in water bath, useful load is 2dm2/ L, the temperature of plating is maintained at 88 DEG C, and the time of plating is 1h.
(6) plating posttreatment.After the cleaned drying of the SiC ceramic that chemical plating is modified, Muffle furnace is placed in
In in 500 DEG C of air atmospheres be heat-treated 2 hours.
The more preferable chemical plating of hardness, abrasion resistance is can obtain after sample cooling and is modified carborundum ceramics sample.Such as
Shown in Fig. 3 (a) and (b), wherein the coating of 10 microns of not thermally treated non-layer gold of thick nickel-plated phosphor with
The adhesion of matrix is 42N, and the adhesion after being heat-treated increases to 77N, and increase rate is up to 83%.
Embodiment 3：
It is chemical plating substrate to select without the SiC ceramic of optical polish.Except electroless plating time is extended for 5 hours
Outside, other techniques are carried out by embodiment 1, finally can obtain the chemical plating in coarse silicon carbide ceramics substrate
Nickel-phosphorus alloy sample.
Embodiment 4：
Selection polishing SiC ceramic is chemical plating substrate.In addition to electroless plating time is extended for 5 hours, other techniques
Carried out by embodiment 1, finally can obtain thickness in polishing silicon carbide ceramics substrate up to 50 microns of chemistry
Plating nickel-phosphorus alloy sample.
The chemical plating coating and the adhesion test result of substrate that accompanying drawing 3 (c) is provided show：By 5 hours
After plating process, SiC ceramic surface nickel-phosphorus alloy thickness is 50 microns, and the adhesion of coating and substrate is high
Up to 122N, the adhesion (~20-60N) of remote super general chemistry coated coating and matrix (such as and stainless steel).
This absolutely proves the present invention for nickel-phosphorus alloy coating and the improvement effect of SiC ceramic substrate bond strength.
Claims (9)
1. a kind of method of chemical plating nickel-phosphorus alloy in silicon carbide ceramics substrate, it is characterised in that：
Step 1：Oil removing and cleaning
A) SiC ceramic substrate is soaked 1-30 minutes in deionized water, is not applied ultrasound or is entered
Row is cleaned by ultrasonic；
B) SiC ceramic substrate is immersed in acetone solvent after taking out, is cleaned by ultrasonic 1-30 minutes；
C) SiC ceramic substrate is immersed in alcohol solvent, be cleaned by ultrasonic 1-30 minutes；
D) with deionized water clean substrate surface, dry at ambient temperature or baking oven in dry；
Step 2：Surface high-temp is aoxidized
Oxidizing temperature is 800-1500 DEG C, oxidization time 1-48 hours；
Step 3：Surface coarsening
A) component for the hydrofluoric acid coarsening solution selected is：Hydrofluoric acid/28% of 40% mass concentration
Concentrated ammonia liquor/water=1-100ml/1-40ml/100-1000ml of mass concentration, Coarsening Temperature is room temperature
~60 DEG C, 1~60min of coarsening time；
B) after being roughened, ceramic bases is taken out, rinsed repeatedly with deionized water, dry；
Step 4：Ionic palladium activation, sensitization
A) composition of ionic palladium activating solution is：Palladium bichloride/ammonium chloride/α-aminopyridine/water
=0.1-1.0 grams/0.1-1.0 grams/0.1-1.0 grams/100-5000 grams；Activating process is：By step 3
The SiC ceramic substrate of surface coarsening is placed in ionic palladium activating solution, and temperature control is in room temperature
~60 DEG C, soak time is 1-60 minutes；
B) palladium bichloride sensitization reducing process is：Sensitizing solution by 10-200g/L sodium hypophosphite
Solution composition, sensitizing temperature is room temperature~60 DEG C, and sensitization time is 1-60 minutes；
Step 5：Chemical plating nickel-phosphorus alloy
A) plating is carried out to SiC ceramic substrate using acidic bath, the composition of acidic bath is：
Nickel sulfate/sodium hypophosphite/lactic acid/sodium citrate/sodium iodide
=10-30g/L/10-30g/L/10-50ml/L/10-30g/L/1-10mg/L, the pH value control of plating solution
In 4.5-5.5；
B) chemical plating is carried out in constant temperature water bath, and the temperature of plating is 85~95 DEG C, plating
Time be 1h-6h；
Step 6：It is heat-treated after plating
After the cleaned drying of SiC ceramic substrate that chemical plating is modified, heat is carried out at high temperature
Handle, heat treatment condition is：200-600 DEG C of temperature；Heat-treating atmosphere be air, oxygen,
Nitrogen or argon gas.
2. the method as described in claim 1, it is characterised in that the oxidation temperature described in step 2
Spend for 1000-1200 DEG C, oxidization time is 4-12 hours.
3. the method as described in claim 1, it is characterised in that the hydrofluoric acid described in step 3
Coarsening solution component is the concentrated ammonia liquor: water of the hydrofluoric acid: 28% mass concentration of 40% mass concentration
=20-60ml: 5-20ml: 100-500ml.
4. the method as described in claim 1, it is characterised in that during roughening described in step 3
Between be 2-10 minutes.
5. the method as described in claim 1, it is characterised in that the ionic palladium described in step 4
Soak time is 5-20 minutes.
6. the method as described in claim 1, it is characterised in that the palladium bichloride described in step 4
Sensitization time is 5-20 minutes.
7. the method as described in claim 1, it is characterised in that the chemical plating described in step 5
When useful load be 0.1-5dm2/L。
8. the method as described in claim 1, it is characterised in that the heat treatment described in step 6
Time is 1-24h.
9. the method as described in claim 1, it is characterised in that step 6 is heat-treated, makes non-
Metallic luster is presented in brilliant nickel-phosphorus coating crystallization, nickel-phosphorus alloy.
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| CN109736079A (en) * | 2019-01-07 | 2019-05-10 | 东华大学 | A kind of nickel phosphorus/carbon nanotube/fabric base functional material and its preparation and application |
| CN115522187A (en) * | 2022-09-30 | 2022-12-27 | 深圳市吉迩科技有限公司 | Ceramic plate coating method based on chemical plating method |
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