CN107475697A - A kind of carbon nano tube surface Electroless Plating Ni P plating solutions and method - Google Patents
A kind of carbon nano tube surface Electroless Plating Ni P plating solutions and method Download PDFInfo
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- CN107475697A CN107475697A CN201710691204.8A CN201710691204A CN107475697A CN 107475697 A CN107475697 A CN 107475697A CN 201710691204 A CN201710691204 A CN 201710691204A CN 107475697 A CN107475697 A CN 107475697A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
- C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1851—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
- C23C18/1872—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment
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- Chemically Coating (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
A kind of Ni P chemical plating fluids and chemical plating method for carbon nano tube surface, it is characterized in that the chemical plating solution includes nickel sulfate(NiSO4·6H2O)18 34g/L, citric acid(C6H8O7·H2O)10 20g/L, lactic acid(C3H6O3)15 25mL/L, anhydrous sodium acetate(CH3COONa)8 16g/L, sodium hypophosphite(NaH2PO2·H2O)20 30 g/L and absolute alcohol(C2H5OH)80‑120mL/L.The chemical plating method of the present invention includes:After CNT is dissolved in into absolute alcohol, alkali cleaning and pickling are carried out, is then placed in chemical plating solution, control pH value and temperature to carry out plating, Ni P is deposited to CNT matrix surface and form coating.The present invention has simple to operate, easy realization, economical.The CNT of the present invention is expected to that strong and weak moderate interface cohesion can be obtained in aluminum matrix composite, effectively suppresses Al4C3Excessive generation.
Description
Technical field
It is specifically a kind of to be used for CNT the present invention relates to the preparation technology of carbon nano tube surface chemical Ni-P plating
The Ni-P electroplate liquid formulations and plating method on surface, belong to carbon nano tube surface technology field.
Background technology
CNT has the electric property of excellent mechanical property, very high chemical stability and uniqueness.But low-dimensional is received
There are many defects in rice material, dispersiveness is also poor in itself.Particularly the surface texture of CNT often influences electricity, power
Many performances such as, optics, in order to improve carbon nano tube surface structure, the general method for using coating, so as to improve or change
Dispersiveness, stability and the compatibility with other materials of nanotube, can make it obtain new physics, chemistry and mechanicalness
Energy.
In order to give full play to the unique function of CNT, sight has been thrown into modified and surface modification about scholar,
The research topic in new focus and forward position is formd, with different material enveloped carbon nanometer tube, the wiener that available can be special
Nano composite material.Ni-P is plated in carbon nano tube surface, it is physical will further to improve electric conductivity, corrosion stability, hardness, lubricity etc.
Can, the coating is alternatively arranged as anti-corrosion, wear-resistant coating, thermal boundary and seal coating, microwave absorbing material etc..In addition, in CNT
Outer surface coats coating, will make to form strong and weak moderate interface cohesion between CNT and Metal Substrate.This is to utilize carbon nanometer
Control is for the indispensable key link of superpower composite.
Ni-P is plated on common material, technology is more ripe, but for nano material, the technology of chemical Ni-P plating compared with
For complexity, operation is difficult.In the prior art, the application of existing CNT cladding different metal, but its common feature is work
Skill route is grown, and complex operation, uses precious metal palladium as catalyst, therefore with high costs, is restricted industrialization, it is difficult to full
Demand of the sufficient development of modern industry to it.Thus, the limitation of original technology how is broken through, more preferable preparation method is found and comes in carbon
Ni-P is plated on nanotube, is the important development direction of carbon nano tube surface technology field, and this area forward position scholar causes always
The subject matter of power research.
The content of the invention
The purpose of the present invention is for being led at present because lacking and plating Ni-P plating solutions and technique in carbon nano tube surface accordingly
Cause carbon nano tube surface can not form Ni-P coating the problem of, invention one kind can not have to palladium chtalyst, the uniform Ni-P of coating
Chemical plating formula, while a kind of corresponding chemical plating method is provided.
One of technical scheme is:
A kind of Ni-P chemical plating solutions for carbon nano tube surface processing, consisting of:
Nickel sulfate(NiSO4·6H2O) 18-34g/L
Citric acid(C6H8O7·H2O) 10-20g/L
Liquid lactic acid(C3H6O3) 15-25mL/L
Anhydrous sodium acetate(CH3COONa) 8-16g/L
Sodium hypophosphite(NaH2PO2·H2O) 20-30 g/L
Absolute alcohol(C2H5OH) 80-120mL/L
Surplus is deionized water.
The two of technical scheme are:
The process of a kind of chemical Ni-P plating for carbon nano tube surface processing, it is characterized in that it mainly includes following step
Suddenly:
(1)Carbon nano tube surface pre-processes:First CNT is dissolved in absolute alcohol, is subsequently placed in NaOH solution and carries out clearly
Wash, then sample is placed in sulfuric acid solution and carries out pickling, pH value close to 7, centrifugal filtration, is dried, is treated after cleaning repeatedly
Plating.
(2)Chemical plating process:Pretreated CNT is placed in Ni-P chemical plating solutions, solution temperature 80-
95 DEG C, pH value 4.2-4.6, solution is stirred using glass bar, plating 2-2.5h, finally take out centrifugal filtration, washing,
Absolute alcohol is washed, centrifugal filtration, drying.
Described configuration Ni-P chemical plating solutions are:A certain amount of distilled water is put into beaker, successively weigh nickel sulfate,
The reagents such as citric acid, sodium hypophosphite, lactic acid, anhydrous sodium acetate and absolute alcohol are put into beaker, pay attention to adding reagent every time
When, to wait a reagent to be completely dissolved;After standing 5min, examination pH value is measured with PH, is adjusted with ammoniacal liquor to 4.2-4.6 or so.
The beneficial effects of the invention are as follows:
(1)The present invention innovatively proposes a kind of Ni-P electroplate liquid formulations and plating method for carbon nano tube surface chemical plating,
By carbon nano tube surface pretreatment and chemical plating process, coating is uniform and is well combined, and is provided for carbon nano tube surface processing
It is a kind of can industrialized production preparation method.
(2)The invention provides the preparation method that a kind of CNT of no palladium chtalyst plates Ni-P, simple to operate, Yi Shi
Existing, economical.
(3)CNT provided by the invention with Ni-P coating is expected to that strong and weak fit can be obtained in aluminum matrix composite
In interface cohesion, effectively suppress Al4C3Excessive generation.
Brief description of the drawings
Fig. 1 is SEM patterns and the EDS energy spectrum analysis of the CNT of surface chemical plating Ni-P in comparative example of the present invention.
Fig. 2 is SEM patterns and the EDS energy spectrum analysis of the CNT of surface chemical plating Ni-P in the embodiment of the present invention.
Embodiment
The embodiment of the present invention is described in detail with reference to the accompanying drawings and examples, but the present invention not only limits
In embodiment.
Embodiment 1.
As shown in Figure 1, 2.
A kind of method of carbon nano tube surface chemical Ni-P plating, step are as follows:
First, take 1 gram of carbon nanotube powder to be dissolved in 25 milliliters of absolute alcohols, be subsequently placed in NaOH solution and cleaned, connect
Sample being placed in sulfuric acid solution and carry out pickling, cause that centrifugal filtration is dry, to be plated close to 7 for pH value after cleaning repeatedly;
Then CNT is put into plating in following solution:
Nickel sulfate(NiSO4·6H2O) 25g/L
Citric acid(C6H8O7·H2O) 13g/L
Liquid lactic acid(C3H6O3) 20mL/L
Anhydrous sodium acetate(CH3COONa) 12g/L
Sodium hypophosphite(NaH2PO2·H2O) 22 g/L
Absolute alcohol(C2H5OH) 100mL/L
Deionized water surplus.
The process for configuring solution is that a certain amount of distilled water is put into beaker(Deionized water), calculated simultaneously by concentration successively
Weigh the reagents such as nickel sulfate, citric acid, sodium hypophosphite, lactic acid, anhydrous sodium acetate and absolute alcohol to be put into beaker, configure
250ml Ni-P chemical plating solutions, when adding reagent every time, a reagent is waited to be completely dissolved;After standing 5min, counted with PH
PH value is tested, is adjusted with ammoniacal liquor to 4.5;
Finally, pretreated CNT is placed in Ni-P chemical plating solutions, solution temperature is 85 DEG C, pH value 4.5, is made
Solution is stirred with glass bar, plating 2h, finally take out centrifugal filtration, washing, absolute alcohol are washed, centrifugal filtration, drying.
Worked well using the CNT that Ni-P is plated made from above-mentioned steps, Fig. 2 is the present embodiment surface chemical plating Ni-
The SEM patterns of P CNT and EDS energy spectrum analysis, SEM-EDS analysis shows, carbon nano tube surface have plated layer of Ni-P
Coating.
Comparative example 1
The present embodiment and embodiment 1 are similar, and difference is not having absolute alcohol, carbon nanotube powder drift in chemical plating solution
Float over above chemical plating fluid, it is difficult to plating.
Comparative example 2
The present embodiment and embodiment 1 are similar, and difference is after Ni-P chemical platings, and centrifugal filtration is simultaneously dried, and lacks washing
The step of being washed with absolute alcohol.
Many impurity be present using the carbon nano tube surface for plating Ni-P made from above-mentioned steps, Fig. 1 is the present embodiment surface
The SEM patterns of the CNT of chemical Ni-P plating and EDS energy spectrum analysis, SEM-EDS analysis shows, carbon nano tube surface are present such as
Many impurity elements such as Na, S, O, many bad influences can be caused to product.
Embodiment two.
A kind of method of carbon nano tube surface chemical Ni-P plating, step are as follows:
First, take 1 gram of carbon nanotube powder to be dissolved in 25 milliliters of absolute alcohols, be subsequently placed in NaOH solution and cleaned, connect
Sample being placed in sulfuric acid solution and carry out pickling, cause that centrifugal filtration is dry, to be plated close to 7 for pH value after cleaning repeatedly;
Then CNT is put into plating in following solution:
Nickel sulfate(NiSO4·6H2O) 18g/L
Citric acid(C6H8O7·H2O) 10g/L
Liquid lactic acid(C3H6O3) 25mL/L
Anhydrous sodium acetate(CH3COONa) 8g/L
Sodium hypophosphite(NaH2PO2·H2O) 30 g/L
Absolute alcohol(C2H5OH) 120mL/L
Deionized water surplus.
The process for configuring solution is that a certain amount of distilled water is put into beaker(Deionized water), calculated simultaneously by concentration successively
Weigh the reagents such as nickel sulfate, citric acid, sodium hypophosphite, lactic acid, anhydrous sodium acetate and absolute alcohol to be put into beaker, configure
250ml Ni-P chemical plating solutions, when adding reagent every time, a reagent is waited to be completely dissolved;After standing 5min, counted with PH
PH value is tested, is adjusted with ammoniacal liquor to 4.2;
Finally, pretreated CNT is placed in Ni-P chemical plating solutions, solution temperature is 95 DEG C, pH value 4.2, is made
Solution is stirred with glass bar, plating 2.5h, finally take out centrifugal filtration, washing, absolute alcohol are washed, centrifugal filtration, baking
It is dry.
Worked well using the CNT that Ni-P is plated made from above-mentioned steps, the carbon of the present embodiment surface chemical plating Ni-P
The SEM patterns and EDS power spectrums of nanotube are close with Fig. 2, SEM-EDS analysis shows, carbon nano tube surface plated layer of Ni-
P coating.
Embodiment three.
A kind of method of carbon nano tube surface chemical Ni-P plating, step are as follows:
First, take 1 gram of carbon nanotube powder to be dissolved in 25 milliliters of absolute alcohols, be subsequently placed in NaOH solution and cleaned, connect
Sample being placed in sulfuric acid solution and carry out pickling, cause that centrifugal filtration is dry, to be plated close to 7 for pH value after cleaning repeatedly;
Then CNT is put into plating in following solution:
Nickel sulfate(NiSO4·6H2O) 34g/L
Citric acid(C6H8O7·H2O) 20g/L
Liquid lactic acid(C3H6O3) 15mL/L
Anhydrous sodium acetate(CH3COONa) 16g/L
Sodium hypophosphite(NaH2PO2·H2O) 20 g/L
Absolute alcohol(C2H5OH) 80mL/L
Deionized water surplus.
The process for configuring solution is that a certain amount of distilled water is put into beaker(Deionized water), calculated simultaneously by concentration successively
Weigh the reagents such as nickel sulfate, citric acid, sodium hypophosphite, lactic acid, anhydrous sodium acetate and absolute alcohol to be put into beaker, configure
250ml Ni-P chemical plating solutions, when adding reagent every time, a reagent is waited to be completely dissolved;After standing 5min, counted with PH
PH value is tested, is adjusted with ammoniacal liquor to 4.6;
Finally, pretreated CNT is placed in Ni-P chemical plating solutions, solution temperature is 80 DEG C, pH value 4.6, is made
Solution is stirred with glass bar, plating 2.3h, finally take out centrifugal filtration, washing, absolute alcohol are washed, centrifugal filtration, baking
It is dry.
Worked well using the CNT that Ni-P is plated made from above-mentioned steps, the carbon of the present embodiment surface chemical plating Ni-P
The SEM patterns and EDS power spectrums of nanotube are close with Fig. 2, SEM-EDS analysis shows, carbon nano tube surface plated layer of Ni-
P coating.
Part that the present invention does not relate to is same as the prior art or can be realized using prior art.
Claims (3)
1. a kind of Ni-P for carbon nano tube surface processing chemical plating solution, it is characterised in that solution composition is:
Nickel sulfate(NiSO4·6H2O) 18-34g/L
Citric acid(C6H8O7·H2O) 10-20g/L
Lactic acid(C3H6O3) 15-25mL/L
Anhydrous sodium acetate(CH3COONa) 8-16g/L
Sodium hypophosphite(NaH2PO2·H2O) 20-30 g/L
Absolute alcohol(C2H5OH) 80-120mL/L
Surplus is deionized water.
A kind of 2. method of the carbon nano tube surface chemical Ni-P plating described in claim 1, it is characterized in that it comprises the following steps:
(1)Carbon nano tube surface pre-processes:First CNT is dissolved in absolute alcohol, is subsequently placed in NaOH solution and carries out clearly
Wash, then CNT is placed in sulfuric acid solution and carries out pickling, cause pH value close to 7, centrifugal filtration, to do after cleaning repeatedly
It is dry, it is to be plated;
(2)By recipe configuration Ni-P chemical plating solutions;
(3)Chemical plating process:Pretreated CNT is placed in the Ni-P chemical plating solutions configured, controls solution temperature
Spend for 80-95 DEG C, pH value 4.2-4.6, solution is stirred using glass bar, plating 2-2.5h, stirring is taken out after terminating
CNT carries out centrifugal filtration successively, washing, absolute alcohol are washed, centrifugal filtration, drying.
3. method as claimed in claim 2, it is characterized in that during the configuration Ni-P chemical plating solutions, be put into beaker from
Sub- water, nickel sulfate, citric acid, sodium hypophosphite, lactic acid, anhydrous sodium acetate and absolute alcohol are weighed successively and is put into beaker, is noted
When meaning adds reagent every time, a reagent is waited to be completely dissolved;After standing 5min, examination pH value is measured with PH, is adjusted with ammoniacal liquor
PH to 4.2-4.6.
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Cited By (2)
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CN110067004A (en) * | 2019-06-05 | 2019-07-30 | 苏州大学 | Ni-W-P/CNTs/CC catalysis electrode and preparation method and application |
CN111020627A (en) * | 2019-12-18 | 2020-04-17 | 青岛大学 | Method for chemically plating NiP on surface of multi-wall carbon nano tube |
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