CN107475697B - A kind of carbon nano tube surface chemical Ni-P plating plating solution and method - Google Patents
A kind of carbon nano tube surface chemical Ni-P plating plating solution and method Download PDFInfo
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- CN107475697B CN107475697B CN201710691204.8A CN201710691204A CN107475697B CN 107475697 B CN107475697 B CN 107475697B CN 201710691204 A CN201710691204 A CN 201710691204A CN 107475697 B CN107475697 B CN 107475697B
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- plating
- absolute alcohol
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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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- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
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- Organic Chemistry (AREA)
- Chemically Coating (AREA)
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Abstract
A kind of Ni-P chemical plating fluid 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.Chemical plating method of the invention includes: to carry out alkali cleaning and pickling after carbon nanotube is dissolved in absolute alcohol, then place it in chemical plating solution, controls pH value and temperature carries out plating, so that Ni-P is deposited to carbon nanotube matrix surface and forms coating.The present invention has easy to operate, Yi Shixian, economical.Carbon nanotube of the invention is expected to that strong and weak moderate interface cohesion, effectively inhibition Al can be obtained in aluminum matrix composite4C3Excessive generation.
Description
Technical field
The present invention relates to the preparation processes of carbon nano tube surface chemical Ni-P plating, specifically a kind of to be used for carbon nanotube
The Ni-P electroplate liquid formulation and plating method on surface, belong to carbon nano tube surface technology field.
Background technique
Carbon nanotube has excellent mechanical property, very high chemical stability and unique electric property.But low-dimensional is received
For rice material itself there are many defects, dispersibility is also poor.Especially the surface texture of carbon nanotube 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
Dispersibility, stability and the compatibility with other substances of nanotube, can make it obtain new physics, chemistry and mechanicalness
Energy.
In order to give full play to the unique function of carbon nanotube, sight has been thrown into modified and surface modification in relation to scholar,
The research topic for foring new hot spot and forward position, 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, which is alternatively arranged as anti-corrosion, wear-resistant coating, thermal boundary and seal coating, microwave absorbing material etc..In addition, in carbon nanotube
Outer surface coats coating, will make to form strong and weak moderate interface cohesion between carbon nanotube and Metal Substrate.This is to utilize carbon nanometer
Control is for the indispensable key link of superpower composite material.
Ni-P is plated on common material, technology is more mature, but for nano material, the technology of chemical Ni-P plating compared with
For complexity, operation is difficult.In the prior art, has the application of carbon nanotube cladding different metal, but its common feature is work
Skill route is long, complicated for operation, and being all made of precious metal palladium is catalyst, therefore with high costs, is restricted industrialization, is difficult full
Demand of the sufficient development of modern industry to it.Thus, the limitation of original technology how is broken through, better preparation method is found and comes in carbon
Ni-P is plated on nanotube, is that the important development direction of carbon nano tube surface technology field and this field forward position scholar cause always
The main problem of power research.
Summary of the invention
The purpose of the present invention is be directed to lead due to carbon nano tube surface plates Ni-P plating solution and technique accordingly because lacking at present
It causes the problem of carbon nano tube surface can not form Ni-P coating, palladium chtalyst, the uniform Ni-P of coating can not had to by inventing one kind
Chemical plating formula, while a kind of corresponding chemical plating method being provided.
Technical solution of the present invention first is that:
A kind of Ni-P chemical plating solution 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.
Technical solution of the present invention second is that:
A kind of process of the chemical Ni-P plating for carbon nano tube surface processing, it is characterized in that it mainly includes following
Step:
(1) carbon nano tube surface pre-process: first carbon nanotube is dissolved in absolute alcohol, be subsequently placed in NaOH solution into
Sample, is then placed in sulfuric acid solution and carries out pickling by row cleaning, makes pH value close to 7 after cleaning repeatedly, centrifugal filtration is done
It is dry, it is to be plated.
(2) chemical plating process: pretreated carbon nanotube is placed in Ni-P chemical plating solution, 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 washes, centrifugal filtration, drying.
The configuration Ni-P chemical plating solution are as follows: 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 that reagent is added every time
When, to wait a reagent to be completely dissolved；After standing 5min, examination pH value is measured with PH, is adjusted to 4.2-4.6 or so with ammonium hydroxide.
The beneficial effects of the present invention are:
(1) present invention innovatively proposes a kind of for the Ni-P electroplate liquid formulation of carbon nano tube surface chemical plating and plating side
Method, by carbon nano tube surface pretreatment and chemical plating process, coating is uniform and is well combined, and mentions for carbon nano tube surface processing
Supplied it is a kind of can industrialized production preparation method.
(2) the present invention provides the preparation method of the carbon nanotube of no palladium chtalyst plating Ni-P a kind of, easy to operate, Yi Shi
Existing, economical.
(3) carbon nanotube provided by the invention with Ni-P coating is expected to obtain in aluminum matrix composite strong and weak suitable
In interface cohesion, effectively inhibition Al4C3Excessive generation.
Detailed description of the invention
Fig. 1 is SEM pattern and the EDS energy spectrum analysis of the carbon nanotube of surface chemical plating Ni-P in comparative example of the present invention.
Fig. 2 is SEM pattern and the EDS energy spectrum analysis of the carbon nanotube of surface chemical plating Ni-P in the embodiment of the present invention.
Specific embodiment
Specific embodiments of the present invention will be 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, steps are as follows:
Firstly, 1 gram of carbon nanotube powder is taken to be dissolved in 25 milliliters of absolute alcohols, it is subsequently placed in NaOH solution and carries out clearly
It washes, then sample is placed in sulfuric acid solution and carries out pickling, make pH value close to 7 after cleaning repeatedly, centrifugal filtration is dry, to
Plating；
Then carbon nanotube 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 (deionized water) is put into beaker, successively simultaneously by concentration calculation
It weighs the reagents such as nickel sulfate, citric acid, sodium hypophosphite, lactic acid, anhydrous sodium acetate and absolute alcohol to be put into beaker, configure
The Ni-P chemical plating solution of 250ml will wait a reagent to be completely dissolved when reagent being added every time；After standing 5min, counted with PH
PH value is tested, is adjusted to 4.5 with ammonium hydroxide；
Finally, pretreated carbon nanotube is placed in Ni-P chemical plating solution, solution temperature is 85 DEG C, and pH value is
4.5, solution is stirred using glass bar, plating 2h, finally taking-up centrifugal filtration, washing, absolute alcohol are washed, were centrifuged
Filter, drying.
It is worked well using the carbon nanotube for plating Ni-P made from above-mentioned steps, Fig. 2 is the present embodiment surface chemical plating Ni-
The SEM pattern of the carbon nanotube of P and EDS energy spectrum analysis, SEM-EDS analysis shows, carbon nano tube surface has plated layer of Ni-P
Coating.
Comparative example 1
The present embodiment and embodiment 1 are similar, the difference is that there is no absolute alcohol in chemical plating solution, carbon nanotube powders
End is swum in above chemical plating fluid, it is difficult to plating.
Comparative example 2
The present embodiment and embodiment 1 are similar, the difference is that centrifugal filtration is simultaneously dried after Ni-P chemical plating, lack
The step of washing and absolute alcohol are washed.
Using the carbon nano tube surface of plating Ni-P made from above-mentioned steps there are many impurity, Fig. 1 is the present embodiment surface
The SEM pattern of the carbon nanotube of chemical Ni-P plating and EDS energy spectrum analysis, SEM-EDS analysis shows, carbon nano tube surface exists such as
Many impurity elements such as Na, S, O can cause many undesirable influences to product.
Embodiment two.
A kind of method of carbon nano tube surface chemical Ni-P plating, steps are as follows:
Firstly, 1 gram of carbon nanotube powder is taken to be dissolved in 25 milliliters of absolute alcohols, it is subsequently placed in NaOH solution and carries out clearly
It washes, then sample is placed in sulfuric acid solution and carries out pickling, make pH value close to 7 after cleaning repeatedly, centrifugal filtration is dry, to
Plating；
Then carbon nanotube 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 (deionized water) is put into beaker, successively simultaneously by concentration calculation
It weighs the reagents such as nickel sulfate, citric acid, sodium hypophosphite, lactic acid, anhydrous sodium acetate and absolute alcohol to be put into beaker, configure
The Ni-P chemical plating solution of 250ml will wait a reagent to be completely dissolved when reagent being added every time；After standing 5min, counted with PH
PH value is tested, is adjusted to 4.2 with ammonium hydroxide；
Finally, pretreated carbon nanotube is placed in Ni-P chemical plating solution, solution temperature is 95 DEG C, and pH value is
4.2, solution is stirred using glass bar, plating 2.5h, finally taking-up centrifugal filtration, washing, absolute alcohol are washed, were centrifuged
Filter, drying.
It is worked well using the carbon nanotube for plating Ni-P made from above-mentioned steps, the carbon of the present embodiment surface chemical plating Ni-P
The SEM pattern and EDS power spectrum of nanotube are similar with Fig. 2, SEM-EDS analysis shows, carbon nano tube surface has plated layer of Ni-
P coating.
Embodiment three.
A kind of method of carbon nano tube surface chemical Ni-P plating, steps are as follows:
Firstly, 1 gram of carbon nanotube powder is taken to be dissolved in 25 milliliters of absolute alcohols, it is subsequently placed in NaOH solution and carries out clearly
It washes, then sample is placed in sulfuric acid solution and carries out pickling, make pH value close to 7 after cleaning repeatedly, centrifugal filtration is dry, to
Plating；
Then carbon nanotube 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 (deionized water) is put into beaker, successively simultaneously by concentration calculation
It weighs the reagents such as nickel sulfate, citric acid, sodium hypophosphite, lactic acid, anhydrous sodium acetate and absolute alcohol to be put into beaker, configure
The Ni-P chemical plating solution of 250ml will wait a reagent to be completely dissolved when reagent being added every time；After standing 5min, counted with PH
PH value is tested, is adjusted to 4.6 with ammonium hydroxide；
Finally, pretreated carbon nanotube is placed in Ni-P chemical plating solution, solution temperature is 80 DEG C, and pH value is
4.6, solution is stirred using glass bar, plating 2.3h, finally taking-up centrifugal filtration, washing, absolute alcohol are washed, were centrifuged
Filter, drying.
It is worked well using the carbon nanotube for plating Ni-P made from above-mentioned steps, the carbon of the present embodiment surface chemical plating Ni-P
The SEM pattern and EDS power spectrum of nanotube are similar with Fig. 2, SEM-EDS analysis shows, carbon nano tube surface has plated layer of Ni-
P coating.
Part that the present invention does not relate to is the same as those in the prior art or can be realized by using the prior art.
Claims (2)
1. a kind of method of carbon nano tube surface chemical Ni-P plating, it is characterized in that it the following steps are included:
(1) carbon nano tube surface pre-processes: first carbon nanotube being dissolved in absolute alcohol, is subsequently placed in NaOH solution and carries out clearly
It washes, then carbon nanotube is placed in sulfuric acid solution and carries out pickling, make pH value close to 7 after cleaning repeatedly, centrifugal filtration is done
It is dry, it is to be plated；
(2) recipe configuration Ni-P chemical plating solution is pressed；Chemical plating solution composition are as follows:
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；
(3) chemical plating process: pretreated carbon nanotube is placed in configured Ni-P chemical plating solution, controls solution temperature
Degree is 80-95 DEG C, pH value 4.2-4.6, is stirred using glass bar to solution, plating 2-2.5h takes out after stirring
Carbon nanotube successively carries out centrifugal filtration, washing, absolute alcohol are washed, centrifugal filtration, drying.
2. the method as described in claim 1, it is characterized in that when the configuration Ni-P chemical plating solution, be put into beaker from
Sub- water successively weighs nickel sulfate, citric acid, sodium hypophosphite, lactic acid, anhydrous sodium acetate and absolute alcohol and is put into beaker, infuses
When reagent is added in meaning every time, a reagent to be waited to be completely dissolved；After standing 5min, examination pH value is measured with pH, with ammonium hydroxide tune
Save pH to 4.2-4.6.
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| CN110067004B (en) * | 2019-06-05 | 2020-08-11 | 苏州大学 | Ni-W-P/CNTs/CC catalytic electrode and preparation method and application thereof |
| CN111020627B (en) * | 2019-12-18 | 2020-10-16 | 青岛大学 | Method for chemically plating NiP on surface of multi-wall carbon nano tube |
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| JP5453601B2 (en) * | 2009-03-17 | 2014-03-26 | 国立大学法人信州大学 | Electroless Ni-P plating solution and electroless Ni-P plating method |
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| CN1775427A (en) * | 2005-11-21 | 2006-05-24 | 谢广文 | Method for preparing nano metal pipe by template chemical plating process |
| CN101058873A (en) * | 2007-05-23 | 2007-10-24 | 湖北工业大学 | Chemical method for coating nickel and zinc on multi-wall nano carbon tube surface |
| CN101818337A (en) * | 2009-11-16 | 2010-09-01 | 兰州理工大学 | Coating method of high-density Ni layer of carbon nano tube |
| CN105195737A (en) * | 2015-10-14 | 2015-12-30 | 东南大学 | Method for covering surfaces of SiC particles with nickel |
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