CN107119267A - Surface of ceramic body chemical solution nickel plating process - Google Patents
Surface of ceramic body chemical solution nickel plating process Download PDFInfo
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- CN107119267A CN107119267A CN201710516606.4A CN201710516606A CN107119267A CN 107119267 A CN107119267 A CN 107119267A CN 201710516606 A CN201710516606 A CN 201710516606A CN 107119267 A CN107119267 A CN 107119267A
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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
-
- 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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- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemically Coating (AREA)
Abstract
Contain following components in surface of ceramic body chemical solution nickel plating process, every liter of chemical nickel-plating solution formula：Nickel sulfate：10~30g；Sodium Thiosulfate：10~25g；Sodium succinate is as buffer, and pH value is between 3.8~5.0；Complexing agent includes citric acid and sodium citrate, totally 5.5~15g；Wherein, citric acid quality is more than sodium citrate；Surplus is water；Temperature control is at 85 DEG C；Because the surface after catalytic treatment is amorphous state, i.e., in substantially planar state, wearability and self lubricity are good, coefficient of friction is small, and Abherent is good, and case hardness can be enhanced about more than once, after heat treatment hardness reaches more than 3 times of life-span raising after Hv1000, work plated film to coating.In wedge angle or edge projection, without significantly thickening, imitate type very well, grinding, the thickness and uniform ingredients of sedimentary are not required to after plating.Alloy catalytic layer fusing point is 850 890 DEG C.Low resistance, solderability is good.
Description
Technical field
The invention belongs to chemical plating nickel technology fields of the C23C in IPC classification to metal material, i.e., with metallic nickel materials pair
The general chemical plating of the coating surface processing of ceramic material, especially surface of ceramic body chemical solution nickel plating process.
Background technology
Chemical plating is a kind of effective surface modifying method, and chemical plating is also known as electroless plating (Electroless
Plating), it is referred to as self-catalysis plating (Autocatalytic plating) [1].Detailed process refers to:In certain bar
Under part, the metal ion in the aqueous solution is reduced agent reduction, and the process being deposited on solid matrix surface.Chemical nickel plating is
A kind of technique that last layer amorphous Ni-P alloy plate is plated in metal or nonmetallic surface by chemical method.By in ceramics
Material surface metal lining nickel tends to improve the surface property of material on the basis of original material property is kept.Due to changing
Learning nickel coating has the performances such as excellent corrosion resistance, wearability and micromagnetism, therefore chemical nickel plating has extensive industry should
With such as being protected on the nonmetallic surface such as steel, casting, aluminium alloy metal surface or glass, plastics, ceramics by chemical nickel
Shield organism material is not wear-resistant or play clear embellishment etc. by burn into.
Traditional chemical nickel-plating solution mainly includes basal liquid and additive, and the nickel ion in basal liquid is during plating
Progressively it is transferred to workpiece to be machined surface.Contain Pb in its additive2+、Sn2+、Sb3+、Hg2+Etc. one kind or several of heavy metal ion
Kind, these heavy metal ion do not participate in reaction during plating, only occur transfer and convert, if liquid waste processing is improper, very
Environmental pollution is easily caused, and its pollution to soil is irreversible, has a strong impact on ecological environment and health.Separately
Outside, the stability of present chemical nickel-plating solution is relatively low, and misoperation is easily hydrolyzed, and causes the waste of material and environment dirty
Dye, and easily there are the bad phenomenons such as pit, pin hole, uneven thickness, surface piebald in chemical Ni-plating layer.
Improved technology scheme of the prior art is less.Pacify micro electronmechanical institute to exist《Material science》Disclose one《Ceramic watch
Face chemical nickel plating》Document, describe using Sodium Thiosulfate as reducing agent respectively using potassium tartrate, sodium hypophosphite, tertiary sodium phosphate as
Complexing agent carries out the optimum formula and process conditions of chemical nickel plating and the characteristics of to each formula and effect compares in ceramic surface
Compared with, as a result show, this technique can ceramic surface obtain function admirable chemical Ni-plating layer.
Kunming University of Science and Technology discloses ZTA ceramics in a kind of ionic liquid in Chinese patent application 201610499240.X
The method of chemical nickel plating on surface, its step is：Surface preparation is carried out to ZTA ceramic particles first, then prepares and contains ion
The chemical nickel-plating solution of liquid, and chemical nickel-plating solution is added into heating in rotation coating bath, after temperature is constant, it is put into surface clear
Clean ZTA ceramic particles, slow rotation carries out chemical nickel plating.Ionic liquid is introduced chemical nickel-plating solution by the present invention, slow down
Plating rate, overcomes the shortcoming that plating solution is unstable, ceramic grain surface plating is uneven；In addition, the rotation that the present invention is used
Stirring means efficiently solve the problem of big particle diameter ZTA ceramic particle plating is uneven, and ZTA ceramic grain surface nickel plating is improved
Its wettability with molten metal, and enhance its bond strength with metallic matrix.
University of Science ＆ Technology, Beijing comes to the surface in Chinese patent application 201010520736.3 there is provided a kind of aluminium nitride ceramics
The method for learning nickel plating, belongs to ceramic membrane metallizing art.It is comprised the following steps that：1st, mechanical grinding aln surface；2nd, use
Mixed acid or alkali roughening aluminium nitride chip, and thoroughly clean the soda acid of residual；3rd, by the substrate being roughened in stannous chloride solution
Middle sensitization, is activated in palladium chloride solution；Or no-palladium activating；4th, by nickel sulfate, sodium hypophosphite, sodium citrate, sodium acetate,
Lactic acid, thiocarbamide, lauryl sodium sulfate, weigh certain mass and are configured to chemical plating solution in order；4th, will be molten with acid or alkali
Liquid pH value is adjusted to 4.0~6.0, and solution is heated into 70~95 DEG C, is put into ready substrate and is carried out chemical nickel plating.The present invention
The characteristics of be that can add a certain amount of surfactant so that coating is more in Difficult to plate substrates performing electroless nickel plating on surface of aluminum nitride ceramic
Plus it is fine and close smooth, coating strengthens with basal body binding force, and coating soldering is more preferable.
Kunming University of Science and Technology discloses Al in a kind of ionic liquid in Chinese patent application 201610496597.22O3Pottery
The method of porcelain chemical nickel plating on surface, its process is：(1) by Al2O3Ceramic particle is cleaned and clear with deionized water after filtering with acetone
Wash；(2) first nickel sulfate solution is slowly added into sodium citrate solution, then sequentially adds ortho phosphorous acid sodium solution, boric acid
Solution obtains base soln, and ionic liquid, regulation solution ph to 9-10, you can obtain chemistry are then added into base soln
Nickel plating solution；(3) chemical nickel-plating solution is heated to 40-70 DEG C, Al is put into after temperature is constant2O3Ceramic particle carries out chemistry
Nickel plating, drying is sealed up for safekeeping after plating is cleaned after terminating with deionized water, you can.
Shanghai Shenhe Thermo-magenetic Electronic Co., Ltd. is related to a kind of pottery in the Chinese patent application 201010564506.7 of proposition
The golden processing method of porcelain metallized substrate metal surface electronickelling, makes circuit on metallized ceramic base plate first；Then use
Ceramic deposited metal technology is to metallized ceramic base plate deposited metal layer, so as to realize the connection of circuit；Use anti-plate nickel gold
Deposited metal layer in the spacing of ink special covering circuit is so as to form the golden ink special coating of anti-plate nickel；Dispel circuit
Surface on the golden ink special of the anti-plate nickel that remains and the metal level of deposition, and be ground it is smooth, with certain roughness
Metal covering carry out electronickelling gold；Dispel the golden ink special coating of anti-plate nickel；Dispel deposited metal layer.Additionally provide thus
Manufacture metallized ceramic base plate.
In the prior art, although, chemical nickel plating has many advantages, and such as wetability to metal is good, coating is combined by force
Spend higher, wear-resisting, corrosion resistance preferable, easy to operate etc..But still suffer from following deficiency in surface of ceramic body chemical nickel plating：
1), led due to containing 8% or so phosphorus, usually easily occurring nickel corrosion and phosphorus rich layer etc. in chemical nickel and gold nickel dam
The risk for causing welding spot reliability to decline.Some high-end metallized ceramic base plates, such as DBC substrates, can to its solderability and solder joint
Require very high by property, usual chemical nickel and gold can not meet its needs.
2), for metallized ceramic base plate, when metallic circuit is when being smaller than 0.20mm, chemical nickel is done in circuit surface
It would be possible on ceramics to be deposited nickel gold and cause line short during gold processing, in circuit spacing.Its reason is chemistry
Because trace clearance is too small during nickel gold, it is difficult to accomplish that cleaning thoroughly causes metal ion residual in gap to be deposited upper nickel gold,
Cause line short.
3), require that layer gold thickness reaches 0.2um~3um for some special ceramics metallized substrates, and chemical nickel and gold without
Method meets this requirement.
4), due to chemical nickel plating during except solid state N i and P precipitation, also gaseous state H2Precipitation, if H2Can not
Discharge coating and plating solution, will remain in coating, cause uneven coating even, brazing property is bad in time.
The content of the invention
It is an object of the invention to provide surface of ceramic body chemical solution nickel plating process, by improving the technique of chemical plating, make
Absorption H in coating2Exclude to greatest extent, to obtain finer and close coating, improve chemical nickel plating quality, effectively solve chemistry
Coating surface is uneven in plating, plating rate is too fast causes the problem of plating solution is unstable.
The purpose of the present invention will be realized by following technical measures：Contain in every liter of chemical nickel-plating solution formula with the following group
Point：
Nickel sulfate：10~30g；
Sodium Thiosulfate：10~25g；
Sodium succinate：As buffer, the pH value of the chemical nickel-plating solution is maintained between 3.8~5.0；
Complexing agent includes citric acid and sodium citrate, totally 5.5~15g；Wherein, citric acid quality is more than sodium citrate；
Surplus is water；
Chemical nickel plating reactions steps include successively：Chemical nickel plating in sour environment, chemical nickel plating is immersed in by workpiece to be plated
In solution, temperature control is at 85 DEG C；Carry out, reducing agent dehydrogenation, aoxidize successively in plating process, hydrogen hydrogen is combined, and is reoxidized, nickel
Salt metal is separated out, and liberation of hydrogen and phosphorus are separated out.
Especially, the chemical nickel-plating solution is using water as solvent, and ph is controlled in 3.8~5.0, every liter of chemical nickel-plating solution
Contain following components：
Nickel sulfate 10g, citric acid 3.5g, sodium hypophosphite 13g, sodium succinate 5g, ammonium chloride 7g, sodium citrate 2g are remaining
Measure as water.
Especially, the chemical nickel-plating solution is using water as solvent, and ph is controlled in 3.8~5.0, every liter of chemical nickel-plating solution
Contain following components：
Nickel sulfate 25g, citric acid 7g, sodium hypophosphite 25g, sodium succinate 10g, ammonium chloride 15g, sodium citrate 5g are remaining
Measure as water.
Advantages of the present invention and effect：Hg is free of in chemical nickel-plating solution2+、Cd2+、Cr2+、Pb2+Etc. heavy metal ion, greatly
It is big to reduce the program and workload of chemical nickle-plating wastewater processing；Because the surface after catalytic treatment is amorphous state, i.e., in base
This flat state, wearability and self lubricity are good, therefore, and coefficient of friction is small, and Abherent is good, and alternative hard chrome is used.Through this
After technical finesse, case hardness can be enhanced about more than once, in steel and copper surface up to Hv570.Coating after heat treatment hardness
Up to Hv1000, General Life improves more than 3 times after plated film.Coating after processing increases with substrate bond strength, typically 350~
Non-scale under the conditions of 400Mpa, do not fall off, bubble-free, the bond strength with aluminium is up to 102~241Mpa.It is prominent in wedge angle or edge
Go out part, without too significantly thickening, imitate type very well, grinding, the thickness and uniform ingredients of sedimentary are not required to after plating.
Alloy catalytic layer fusing point is 850-890 DEG C.Low resistance, solderability is good.Blind hole, deep hole, pipe fitting, turning, gap inner surface
Strong adaptability, can obtain homogeneous coating, no matter how complicated product structure has, absolutely not in place of plating leakage.
Embodiment
The present invention develops the compound additive of the element without heavy metal, reduces cost of sewage disposal, meanwhile, favorably
In environmental protection.
In the present invention：Contain following components in every liter of chemical nickel-plating solution formula：
Nickel sulfate：10~30g；
Sodium Thiosulfate：10~25g；
Sodium succinate：As buffer, the pH value of the chemical nickel-plating solution is maintained between 3.8~5.0；
Complexing agent includes citric acid and sodium citrate, totally 5.5~15g；Wherein, citric acid quality is more than sodium citrate；
Surplus is water；
Chemical nickel plating reactions steps include successively：Chemical nickel plating in sour environment, chemical nickel plating is immersed in by workpiece to be plated
In solution, temperature control is at 85 DEG C；Carry out, reducing agent dehydrogenation, aoxidize successively in plating process, hydrogen hydrogen is combined, and is reoxidized, nickel
Salt metal is separated out, and liberation of hydrogen and phosphorus are separated out.
With reference to embodiment, the invention will be further described.
Embodiment 1：
The chemical nickel-plating solution using water as solvent, ph control in 3.8~5.0, every liter of chemical nickel-plating solution contain with
Lower component：
Nickel sulfate 10g, citric acid 3.5g, sodium hypophosphite 13g, sodium succinate 5g, ammonium chloride 7g, sodium citrate 2g are remaining
Measure as water.
Embodiment 2：
The chemical nickel-plating solution using water as solvent, ph control in 3.8~5.0, every liter of chemical nickel-plating solution contain with
Lower component：
Nickel sulfate 25g, citric acid 7g, sodium hypophosphite 25g, sodium succinate 10g, ammonium chloride 15g, sodium citrate 5g are remaining
Measure as water.
In the present invention：
Nickel sulfate is mainly used in electroplating industry, is the main nickel salt of electronickelling and chemical nickel, is also coming for metallic nickel ions
Source, can dissociate nickel ion and sulfate ion in electroplating process.
Sodium hypophosphite is chemical plating agent, and catalyst, stabilizer prepare polyamide macromolecule polyamides thing, accelerate chemistry anti-
Should；And can combine to form chelant thing with nickel as the stabilizer chemically reacted, as reducing agent in nickel plating bath and control
Acid-base value, can effectively improve the surface property and finish of nickel plating product.For the big of coating can not be entered using electroplating technology
Type equipment and fine pieces, precision prescribed it is higher and with the complicated profile object of asperities, inner walls of deep holes, require higher table
The object of surface hardness and wearability；Or the surface metalation of the nonmetallic materials such as plastics, ceramics, hyaline-quartz, use this product
Fine and close, uniform nickel, chrome plating can be obtained, and it is more more firm than electroplating.Electronics is widely used in, aviation, machinery, oil etc. is gone
Industry.
Ammonium chloride is clear crystal or white crystalline powder；Odorless, taste is salty, cool；Have and draw moist.It is readily soluble in water,
Slightly soluble in ethanol.The aqueous solution is in faintly acid, acid enhancing during heating.Ferrous metal and other metals are corrosive, it is especially right
Copper corrosion is bigger, to the corrosion-free effect of the pig iron.Industrial ammonium chloride is white powder or grain crystalline body, and odorless, taste be salty and band
Have refrigerant.Easy moisture absorption caking, it is soluble in water, glycerine and liquefied ammonia are dissolved in, ethanol is insoluble in, insoluble in acetone and ether, at 350 DEG C
Shi Shenghua, the aqueous solution is in faintly acid.The purposes of industrial grade ammonium chloride is mainly used in battery, plating, dyeing and weaving, casting, medicine, plant
In terms of suede, fine hair, chemical intermediate.Ammonium chloride in itself can there is provided chlorion progress as the stable reagent of solution containing nickel
Its compound and ammonium chloride, are codissolved in watery hydrochloric acid by coordination when using.
Sodium succinate molecular formula is C4H4Na2O4, is a kind of white solid, odorlessness, in atmosphere not deliquescence；It is soluble in
Water, insoluble in organic solvent.It is mainly used in buffer.It can be additionally used in synthesis medicine and other organic synthesis raw materials.
Citric acid is a kind of important organic acid, also known as citric acid, and clear crystal, Chang Hanyi molecular crystalline water, odorless has
Very strong tart flavour, it is soluble in water.Its calcium salt is more soluble than in hot water in cold water, and this property is commonly used to be identified and isolated from lemon
Acid.Suitable temperature is controlled to obtain anhydrous citric acid during crystallization.Citric acid chemical name 2- hydroxy propane -1,2,3- tricarboxylics
Acid.According to the difference of its water content, it is divided into Citric Acid Mono and anhydrous citric acid.The purposes of citric acid widely, for changing
Industry is learned, as buffer, complexing agent, metal cleaner, mordant, gelling agent, toner etc..
Sodium citrate alias sodium citrate, is a kind of organic compound, and outward appearance arrives clear crystal for white.Odorless, there is clear
Cool salty pungent.It is stable in normal temperature and air, it is micro- in humid air to have dissolubility, weathering phenomenon is produced in hot-air.It is heated to
150 DEG C lose the crystallization water.It is soluble in water, dissolve in glycerine, be insoluble in alcohols and other organic solvents, cross thermally decompose, in humidity
Environment in it is micro- have deliquescence, micro- in hot-air to have weathering, its solution ph is about 8.Sodium citrate is excellent in chemistry
Chelating agent/complexing agent, industrially the application to sodium citrate is all to utilize this characteristic.With complexing of metal ion ability.
Sodium citrate is to Ca2+、Mg2+There is good complexing power Deng metal ion, to other metal ions, such as Fe2+ plasmas
There is good complexing power.Sodium citrate has fabulous solubility property, and dissolubility is raised and increased with water temperature.Citric acid
There is sodium good pH to adjust and shock-absorbing capacity.Sodium citrate is a kind of weak acid strong alkali salt, can constitute stronger with compatibility of citric acid
PH buffer, therefore have its important use in some occasions for being not suitable for pH wide variations.In addition, sodium citrate also has
Excellent retarding performance and stability.
The present invention description is made by specific embodiment, but it is clear that still can with various modification can be adapted and convert and
Without departing substantially from the spirit and scope of the present invention.Therefore, specification is regarded in an illustrative, rather than a restrictive.
Claims (3)
1. surface of ceramic body chemical solution nickel plating process, it is characterised in that contain in every liter of chemical nickel-plating solution formula with the following group
Point：
Nickel sulfate：10~30g；
Sodium Thiosulfate：10~25g；
Sodium succinate：As buffer, the pH value of the chemical nickel-plating solution is maintained between 3.8~5.0；
Complexing agent includes citric acid and sodium citrate, totally 5.5~15g；Wherein, citric acid quality is more than sodium citrate；
Surplus is water；
Chemical nickel plating reactions steps include successively：Chemical nickel plating in sour environment, chemical nickel-plating solution is immersed in by workpiece to be plated
In, temperature control is at 85 DEG C；Carry out, reducing agent dehydrogenation, aoxidize successively in plating process, hydrogen hydrogen is combined, and is reoxidized, nickel salt gold
Category is separated out, and liberation of hydrogen and phosphorus are separated out.
2. surface of ceramic body chemical solution nickel plating process as claimed in claim 1, it is characterised in that the chemical nickel-plating solution
Using water as solvent, ph controls contain following components in 3.8~5.0, every liter of chemical nickel-plating solution：
Nickel sulfate 10g, citric acid 3.5g, sodium hypophosphite 13g, sodium succinate 5g, ammonium chloride 7g, sodium citrate 2g, surplus is
Water.
3. surface of ceramic body chemical solution nickel plating process as claimed in claim 1, it is characterised in that the chemical nickel-plating solution
Using water as solvent, ph controls contain following components in 3.8~5.0, every liter of chemical nickel-plating solution：
Nickel sulfate 25g, citric acid 7g, sodium hypophosphite 25g, sodium succinate 10g, ammonium chloride 15g, sodium citrate 5g, surplus is
Water.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113151811A (en) * | 2021-04-13 | 2021-07-23 | 赤壁市聚茂新材料科技有限公司 | Non-palladium activated nickel plating solution and nickel plating method |
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