CN103451634A - Method for chemical nickel plating on surface of micron silicon carbide powder - Google Patents
Method for chemical nickel plating on surface of micron silicon carbide powder Download PDFInfo
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Abstract
The invention discloses a method for chemical nickel plating on the surface of micron silicon carbide powder, and relates to a method for nickel plating on the surface of an object. According to the method for nickel plating, the quantity of a reducing agent added at the beginning is the minimum quantity of the reducing agent for a reaction, and then the reducing agent is continuously added at a small flow by using a burette to ensure that the reducibility of the reducing agent in a plating solution is kept constant, so that the aim of controlling the reaction speed is achieved. By adopting the method, relatively stable nickel plating micron silicon carbide powder is obtained through a reasonable process, and the problems that the nickel plating micron silicon carbide powder is unstable and the surface of the nickel plating micron silicon carbide powder is exposed in the prior art are effectively solved.
Description
[technical field]
The present invention relates to a kind of body surface nickel plating process, specifically the present invention relates to the chemical nickel plating method of a kind of micron carborundum powder surface.
[background technology]
Known, metallic nickel is the silvery white metal, density 8.9 grams per cubic centimters.1455 ℃ of fusing points, 2730 ℃ of boiling points.Matter is hard, has magnetic and good plasticity-.The erosion resistance had, not oxidized in air, anti-highly basic again; Due to the afore-mentioned characteristics of metallic nickel, so nickel is mainly used to manufacture stainless steel and other corrosion-resisting alloies, as nickel steel, steel nickel chrome and various non-ferrous metal alloy, the cupronickel that nickeliferous composition is higher, just not perishable.Also make hydrogenation catalyst and green and prepared etc. by nickel compound for ceramic, extraordinary chemical ware, electronic circuit, glass; Wherein metallic substance is most important engineering materials; and, in metallic substance, 90% is iron and steel, it is the maximum engineering metal material of application; ferrous materials has low price, aboundresources, superior performance and the characteristics such as easily accomplish scale production, and has obtained and has been widely used.
Metal-base composites is to take metal or alloy as matrix, the matrix material that the high performance second-phase of take is reinforcement, and the development of its development and modern science and technology and hi-tech industry is closely related.Developing rapidly of particularly space flight, aviation, electronics, automobile and sophisticated and futuristic weapons system proposed to material the performance requriements day by day increased, except requiring material to have some special performances, also will have good over-all properties, this has effectively promoted developing rapidly of advanced composite material.
SiC is the reinforcement material of current more use, with traditional metallic substance, compares and has many advantages, and wherein strength and stiffness are than high, lightweight and close to zero thermal expansivity and good solidity to corrosion etc.The price that SiC is relatively low, and realized suitability for industrialized production.The Young's modulus of reinforcement particle, tensile strength and hardness, all than steel-based height, add and rule according to the performance of matrix material, and its intensity, hardness and Young's modulus all should be higher than body material.Theoretical investigation and actual experiment result all show, volume fraction just can make the Young's modulus of matrix material improve 50% in 10%～30% enhanced granule, and intensity also has in various degree and improves.In fields such as national aerospace technology, telecommunications and communications and transportation, have broad application prospects, but the metal current based composites exists the interface wetting property that a general problem is reinforcement and metal poor, bonding strength is relatively low, and this has affected the mechanical property of final material to a great extent.
When SiC pottery is connected with metal, because wettability between metal and pottery is poor, easily on metal and ceramic interface, the defect of macroscopic view or microcosmic occurs, thereby reduced widely its over-all properties.If form the coating of metal or alloy at SiC powder surface and intermetallic, thereby improve interface wet ability and the chemical compatibility between pottery and matrix, can greatly improve the interfacial bonding property of matrix and SiC powder.Electroless plating method is to utilize metal salt solution to make metal ion be reduced into metal under the effect of reductive agent, obtain the settled layer of metal on the surface of plating piece, the method has that technique is simple, with low cost, coating evenly, with the advantages such as matrix is combined, there is very consequence in the process for treating surface of powder.
The existing similarity of the electroless plating of powder electroless and block big scale material, a lot of differences is arranged again, similarity is mainly the pretreatment technology to the preplating material, plating solution composition and plating technic thereof are basic identical, difference is mainly that powder body material is with respect to blocks of large, there is large specific surface area, therefore, generally more violent in electroless plating reaction, reaction process is wayward, and in reaction process, various parameters are such as temperature, the pH value, main salt and various additives concentration etc. is not easy to control, also easily cause reunion and the sedimentation thereof of powder granule.
In the research method of chemical nickel plating is carried out on SiC ceramic powder surface in the past, be substantially all to adopt once adding or adding fully for twice of reductive agent, its result is all undesirable.In order to ascertain the reason, the inventor has carried out the replica test analysis according to report in the past, find that reaction is violent, reaction times is short, and in plating solution, there is the spongiform nickel of part to generate, SiC ceramic powder overlay coating and inhomogeneous, and exposed phenomenon is arranged, thereby affected the application of SiC composite ceramic material, analyzing its reason is mainly in the initial stage, in plating solution, the amount of reductive agent is larger, its reductibility is stronger, thereby make a large amount of depositions rapidly of main salt metal ion in plating solution and cause the appearance of the inhomogeneous and surface exposure phenomenon of micron carborundum powder surface.
[summary of the invention]
In order to overcome the deficiency in background technology, the invention discloses the chemical nickel plating method of a kind of micron carborundum powder surface, the present invention obtains comparatively stable nickel plating micron carborundum powder by rational technique, has effectively overcome the unstable and nickel plating micron carborundum powder surface exposure problem of nickel plating micron carborundum powder that prior art causes.
Realize that technical scheme of the present invention is as follows:
The chemical nickel plating method of a kind of micron carborundum powder surface, described nickel plating process is the minimum reduction dosage that only can react in the amount of the reductive agent that starts to add, then carry out the reductive agent that adds low discharge, continual by dropper, make the reductibility of reductive agent in plating solution keep constant, thereby reach the purpose of controlling speed of response, reaction below main generation the in plating solution:
Ni
2++N
2H
4?→?Ni+N
2+H
2+2H
+。
The chemical nickel plating method of described micron carborundum powder surface, concrete nickel plating step:
A, utilize the sodium hydroxide solution that concentration is 60-70g/L, carry out the grease removal oil removing of a micron carborundum powder " SiC " surface at the temperature of 50 ℃, then utilize after washed with de-ionized water alligatoring 10h in hydrochloric acid " massfraction the is 37% " solution that is 50% at mass ratio again, the hydrochloric acid soln temperature is 40 ℃, stand-by to neutrality with deionized water rinsing micron carborundum powder " SiC " after finishing;
B, the tin protochloride by previous step micron carborundum powder " SiC " with 15g/L, the hydrochloric acid of 60ml/L is mixed with sensitizing solution, and micron carborundum powder " SiC " time of body in sensitizing solution is 5-10min; The activation solution formula is Palladous chloride 0.5g/L, utilizes hydrochloric acid to become the activation solution that the pH value is 3-4 to be activated solution preparation, and soak time is 5 minutes;
The plating solution of C, preparation 500ML, in the chemical reagent of described 500ML plating solution, comprise: the six water nickelous chlorides of 30-35g/L, the citrate three sodium of 25-45g/L, the sodium laurylsulfonate of 0.1g/L, the o-benzoic sulfimide of 0.01g/L, add the distilled water dissolving and be mixed with the 200ml plating solution; Six water nickelous chlorides, citrate three sodium are diluted with the 100ML deionized water respectively, sodium laurylsulfonate, o-benzoic sulfimide are respectively with the dilution of 50ML deionized water, sodium dodecyl sulfate solution after dilution is joined to the citrate three sodium solution after dilution, then six water nickel chloride solutions are added in above-mentioned mixing solutions, then o-benzoic sulfimide solution is joined to the plating solution that above-mentioned mixing solutions obtains 500ML;
D, in the plating solution of 450ML, utilize the sodium hydroxide solution of deionized water and 3Mol/L, plating solution is deployed into to 470ML, the pH value of plating solution is reconciled to 10-11, add micron carborundum powder " SiC " body after alligatoring, wherein in add-on and plating solution, the amount ratio of nickel metal is 3:1;
E, while utilizing the heating unit temperature to be heated to 80-90 ℃ the plating solution of previous step, speed stirring plating solution with stirrer with 10-15 revolutions per second, and then add reductive agent hydrazine hydrate 30ML with the speed of 14-16 ml/h.L by drop-burette, after reductase 12 h, reaction process finishes, and by powder, precipitate, washs, separates and dry micron silicon carbide powder that obtains plating nickel on surface.
By above-mentioned disclosure, the invention has the beneficial effects as follows:
The chemical nickel plating method of micron of the present invention carborundum powder surface, the present invention carries out the reductive agent that adds low discharge, continual by dropper, makes the reductibility of reductive agent in plating solution keep constant, thereby reaches the purpose of controlling speed of response; The present invention is compared with the prior art has the stable and nickel plating micron carborundum powder surface of nickel plating micron carborundum powder without exposed phenomenon; Can keep the reductibility of reductive agent in plating solution to keep constant, the coating surface obtained is even, and coating and substrate combinating strength high, difficult drop-off.
[embodiment]
Below in conjunction with embodiment, the present invention is further detailed; The following examples are not for restriction of the present invention, and only, as supporting to realize mode of the present invention, any equivalent structure in technological frame disclosed in this invention is replaced, and is protection scope of the present invention;
It should be noted that the present invention adds reductive agent or two steps to add the working method step of reductive agent to have the part similarity fully with adopting a traditional step, but there is essential distinction in the preplating powder handling in main process, plating solution preparation and plating.
The chemical nickel plating method of micron of the present invention carborundum powder surface, described nickel plating process is the minimum reduction dosage that only can react in the amount of the reductive agent that starts to add, then carry out the reductive agent that adds low discharge, continual by dropper, make the reductibility of reductive agent in plating solution keep constant, thereby reach the purpose of controlling speed of response, reaction below main generation the in plating solution:
Ni
2++N
2H
4?→?Ni+N
2+H
2+2H
+。
The chemical nickel plating method of described micron carborundum powder surface, concrete nickel plating step:
Use analytical balance accurately to take required six water nickelous chlorides, sodium hydroxide, hydrochloric acid, tin protochloride, citrate three sodium, o-benzoic sulfimide, sodium laurylsulfonate chemical reagent.
A, utilize the sodium hydroxide solution that concentration is 60-70g/L, carry out the grease removal oil removing of a micron carborundum powder " SiC " surface at the temperature of 50 ℃, then utilize after washed with de-ionized water alligatoring 10h in hydrochloric acid " massfraction the is 37% " solution that is 50% at mass ratio again, the hydrochloric acid soln temperature is 40 ℃, stand-by to neutrality with deionized water rinsing micron carborundum powder " SiC " after finishing;
B, the tin protochloride by previous step micron carborundum powder " SiC " with 15g/L, the hydrochloric acid of 60ml/L is mixed with sensitizing solution, and micron carborundum powder " SiC " time of body in sensitizing solution is 5-10min; The activation solution formula is Palladous chloride 0.5g/L, utilizes hydrochloric acid to become the activation solution that the pH value is 3-4 to be activated solution preparation, and soak time is 5 minutes;
The plating solution of C, preparation 500ML, in the chemical reagent of described 500ML plating solution, comprise: the six water nickelous chlorides of 30-35g/L, the citrate three sodium of 25-45g/L, the sodium laurylsulfonate of 0.1g/L, the o-benzoic sulfimide of 0.01g/L, add the distilled water dissolving and be mixed with the 200ml plating solution; Six water nickelous chlorides, citrate three sodium are diluted with the 100ML deionized water respectively, sodium laurylsulfonate, o-benzoic sulfimide are respectively with the dilution of 50ML deionized water, sodium dodecyl sulfate solution after dilution is joined to the citrate three sodium solution after dilution, then six water nickel chloride solutions are added in above-mentioned mixing solutions, again o-benzoic sulfimide solution is joined to above-mentioned mixing solutions, all reagent all takes by the 500ML plating solution, first the plating solution volume is deployed into to 450ML;
Be specially sodium dodecyl sulfate solution is poured in the citric acid three sodium solution prepared while stirring;
Then nickel chloride solution is poured in the mixing solutions prepared while stirring;
Then hydrazine hydrate solution is poured in the mixing solutions prepared while stirring;
Then regulate the pH value to prescribed value with sodium hydroxide and ammonia soln;
Then be diluted to volume calculated with deionized water:
D, in the plating solution of 450ML, utilize the sodium hydroxide solution of deionized water and 3Mol/L, plating solution is deployed into to 470ML, the pH value of plating solution is reconciled to 10-11, add micron carborundum powder " SiC " body after alligatoring, wherein in add-on and plating solution, the amount ratio of nickel metal is 3:1;
E, while utilizing the heating unit temperature to be heated to 80-90 ℃ the plating solution of previous step, speed stirring plating solution with stirrer with 10-15 revolutions per second, and then add reductive agent hydrazine hydrate solution 30ML with the speed of 14-16 ml/h.L by drop-burette, after reductase 12 h, reaction process finishes, and by powder, precipitate, washs, separates and dry micron silicon carbide powder that obtains plating nickel on surface.
Part not in the detailed description of the invention is prior art.
Claims (1)
1. the chemical nickel plating method of a micron carborundum powder surface, it is characterized in that: described nickel plating process is the minimum reduction dosage that only can react in the amount of the reductive agent that starts to add, then carry out the reductive agent that adds low discharge, continual by dropper, make the reductibility of reductive agent in plating solution keep constant, thereby reach the purpose of controlling speed of response, reaction below main generation the in plating solution:
Ni
2++N
2H
4?→?Ni+N
2+H
2+2H
+；
The chemical nickel plating method of described micron carborundum powder surface, concrete nickel plating step:
A, utilize the sodium hydroxide solution that concentration is 60-70g/L, carry out the grease removal oil removing of a micron carborundum powder " SiC " surface at the temperature of 50 ℃, then utilize after washed with de-ionized water alligatoring 10h in hydrochloric acid " massfraction the is 37% " solution that is 50% at mass ratio again, the hydrochloric acid soln temperature is 40 ℃, stand-by to neutrality with deionized water rinsing micron carborundum powder " SiC " after finishing;
B, the tin protochloride by previous step micron carborundum powder " SiC " with 15g/L, the hydrochloric acid of 60ml/L is mixed with sensitizing solution, and micron carborundum powder " SiC " time of body in sensitizing solution is 5-10min; The activation solution formula is Palladous chloride 0.5g/L, utilizes hydrochloric acid to become the activation solution that the pH value is 3-4 to be activated solution preparation, and soak time is 5 minutes;
The plating solution of C, preparation 500ML, in the chemical reagent of described 500ML plating solution, comprise: the six water nickelous chlorides of 30-35g/L, the citrate three sodium of 25-45g/L, the sodium laurylsulfonate of 0.1g/L, the o-benzoic sulfimide of 0.01g/L, add the distilled water dissolving and be mixed with the 200ml plating solution; Six water nickelous chlorides, citrate three sodium are diluted with the 100ML deionized water respectively, sodium laurylsulfonate, o-benzoic sulfimide are respectively with the dilution of 50ML deionized water, sodium dodecyl sulfate solution after dilution is joined to the citrate three sodium solution after dilution, then six water nickel chloride solutions are added in above-mentioned mixing solutions, then o-benzoic sulfimide solution is joined to the plating solution that above-mentioned mixing solutions obtains 500ML;
D, in the plating solution of 450ML, utilize the sodium hydroxide solution of deionized water and 3Mol/L, plating solution is deployed into to 470ML, the pH value of plating solution is reconciled to 10-11, add micron carborundum powder " SiC " body after alligatoring, wherein in add-on and plating solution, the amount ratio of nickel metal is 3:1;
E, while utilizing the heating unit temperature to be heated to 80-90 ℃ the plating solution of previous step, speed stirring plating solution with stirrer with 10-15 revolutions per second, and then add reductive agent hydrazine hydrate 30ML with the speed of 14-16 ml/h.L by drop-burette, after reductase 12 h, reaction process finishes, and by powder, precipitate, washs, separates and dry micron silicon carbide powder that obtains plating nickel on surface.
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| WO2017075740A1 (en) * | 2015-11-02 | 2017-05-11 | 苏州金仓合金新材料有限公司 | Nickel-plated silicon carbide particle enhanced copper-based composite material for vehicle bearings and method for preparing same |
| CN106756903A (en) * | 2016-12-14 | 2017-05-31 | 苏州金仓合金新材料有限公司 | A kind of Nickel-plated carbon silicon grain and preparation method thereof |
| 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 |
| 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 |
| CN108866518A (en) * | 2018-07-25 | 2018-11-23 | 东北大学 | The method that nickel ferrite based magnetic loaded ceramic material surfaces prepare chemical Ni-plating layer without activation without sensitization |
| CN109207993A (en) * | 2018-09-17 | 2019-01-15 | 南昌大学 | A kind of wear-resistant coating preparation method of titanium alloy surface |
| CN109852952A (en) * | 2019-02-28 | 2019-06-07 | 浙江英洛华磁业有限公司 | A kind of hydrazine hydrate chemical nickel-plating plating solution and preparation method thereof and nickel plating process |
| CN114807912A (en) * | 2022-05-10 | 2022-07-29 | 常州德创高新材料科技有限公司 | Method for chemically plating nickel on surface of poly glycidyl methacrylate microsphere |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2017075740A1 (en) * | 2015-11-02 | 2017-05-11 | 苏州金仓合金新材料有限公司 | Nickel-plated silicon carbide particle enhanced copper-based composite material for vehicle bearings and method for preparing same |
| CN106756903A (en) * | 2016-12-14 | 2017-05-31 | 苏州金仓合金新材料有限公司 | A kind of Nickel-plated carbon silicon grain and preparation method thereof |
| WO2018107846A1 (en) * | 2016-12-14 | 2018-06-21 | 苏州金仓合金新材料有限公司 | Nickel-plated silicon carbide particles and preparation method therefor |
| 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 |
| 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 |
| US20190264330A1 (en) * | 2018-02-24 | 2019-08-29 | Tangshan Normal University | Method of electroless nickle plating on surface of silicon carbide powder |
| US10995408B2 (en) * | 2018-02-24 | 2021-05-04 | Tangshan Normal University | Method of electroless nickle plating on surface of silicon carbide powder |
| CN108866518A (en) * | 2018-07-25 | 2018-11-23 | 东北大学 | The method that nickel ferrite based magnetic loaded ceramic material surfaces prepare chemical Ni-plating layer without activation without sensitization |
| CN109207993A (en) * | 2018-09-17 | 2019-01-15 | 南昌大学 | A kind of wear-resistant coating preparation method of titanium alloy surface |
| CN109207993B (en) * | 2018-09-17 | 2020-07-28 | 江西景航航空锻铸有限公司 | Preparation method of wear-resistant coating on titanium alloy surface |
| CN109852952A (en) * | 2019-02-28 | 2019-06-07 | 浙江英洛华磁业有限公司 | A kind of hydrazine hydrate chemical nickel-plating plating solution and preparation method thereof and nickel plating process |
| CN114807912A (en) * | 2022-05-10 | 2022-07-29 | 常州德创高新材料科技有限公司 | Method for chemically plating nickel on surface of poly glycidyl methacrylate microsphere |
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