CN106521496A - Method for conducting chemical nickel plating to prepare high-hydrogen-evolution-activity electrode after electrophoresis of carbon nano tube on surface of carbon steel - Google Patents
Method for conducting chemical nickel plating to prepare high-hydrogen-evolution-activity electrode after electrophoresis of carbon nano tube on surface of carbon steel Download PDFInfo
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- 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
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Abstract
A method for conducting chemical nickel plating to prepare a high-hydrogen-evolution-activity electrode after electrophoresis of a carbon nano tube on the surface of carbon steel is provided. The invention relates to a method for conducting chemical nickel plating to prepare a high-hydrogen- evolution-activity electrode after electrophoresis of a carbon nano tube on the surface of carbon steel and aims at solving the problem that at present, in a sodium hydroxide solution, the hydrogen evolution activity of a carbon steel cathode commonly used in electrolysis hydrogen production is low. The method for conducting chemical nickel plating to prepare the high hydrogen evolution activity electrode after electrophoresis of the carbon nano tube on the surface of carbon steel comprises the first step of carbon nano tube colloidal fluid preparing, the second step of carbon steel pretreatment, the third step of electrophoresis of the carbon nano tube micelle to the surface of the carbon steel and the fourth step of chemical nickel preparing, and a carbon nano tube/Ni-P alloy composite coating with higher hydrogen evolution activity is obtained on the surface of the carbon steel. The carbon steel/carbon nano tube electrophoresis layer/Ni-P alloy composite has good hydrogen evolution activity and stability, and the problem of high energy consumption caused by adopting the carbon steel cathode in electrolysis hydrogen production in the sodium hydroxide solution.
Description
Technical field
The invention belongs to the preparation field of hydrogen-precipitating electrode, is related to one kind chemical nickel plating after the electrophoresis CNT of carbon steel surface
Method to improve the hydrogen evolution activity in sodium hydroxide solution.
Background technology
Water electrolysis hydrogen production is the hydrogen energy source that electric energy and water are converted into cleaning, and energy is stored in the form of chemical energy
Come, in case of need, be the effective way for solving lack of energy.With the century-old development of electrolytic hydrogen production technology, the field phase
Other hydrogen producing technologies are defined with the advantage of oneself uniqueness, such as hydrogen manufacturing purity is high, process is simple is easy to operate, production capacity
It is strong etc..At present, the most commonly used system in electrolytic hydrogen production technology is exactly alkaline aqueous solution electrolysis system, that is, liberation of hydrogen is electric
Pole and analysis oxygen electrode are placed in sodium hydroxide solution, produce oxygen in anode, produce high-purity hydrogen in negative electrode during electrolysis.
But alkaline aqueous solution electrolysis system also faces important technical problem aborning.In order to improve hydrogen evolution activity,
Reduce the cost of electric energy of hydrogen manufacturing, it is necessary to adopt noble metal catalyst, but its electrode cost is too high；If using gold such as carbon steel, nickel
, used as hydrogen-precipitating electrode, its energy conversion efficiency is again too low, and substantial amounts of power consumption is finally released in the form of heat energy in groove pressure for category
Run out.In order to balance the contradiction between power consumption and hardware input, the actual production of electrolytic hydrogen production is often using common
Carbon steel as hydrogen-precipitating electrode, to sacrifice the input that unnecessary electric energy reduces to hardware as cost, but its relatively low hydrogen evolution activity
The development space of enterprise is also limit, profit margin is reduced.
Therefore, for more effective electrolytic hydrogen production, it is necessary to reduce the overpotential of hydrogen evolution of carbon steel, the liberation of hydrogen for improving carbon steel is lived
Property, the hardware input of enterprise is so not only released, and alleviates the burden that high power consumption expense is brought.Improve carbon
The hydrogen evolution activity of steel effectively must could be modified to carbon steel from two angle comprehensive considerations of geometrical factor and capacity factor,
Prepare the high electrode of hydrogen evolution activity.That is, it is necessary to obtain the coating conduct with more bigger serface on carbon steel surface
The carrier of hydrogen evolution activity point, then loads the material of high hydrogen evolution activity again, could farthest play liberation of hydrogen catalyst
Effect, reduces power consumption taking into account while hardware puts into, so as to improve the profit of alkaline aqueous solution electrolysis system.
The content of the invention
The present invention is to solve in sodium hydroxide solution, the conventional carbon steel cathodes hydrogen evolution activity of electrolytic hydrogen production is relatively low at present
Problem, and provide it is a kind of by the chemical nickel plating after the electrophoresis CNT of carbon steel surface improving the side of carbon steel hydrogen evolution activity
Method.
A kind of method that chemical nickel plating prepares high hydrogen evolution activity electrode after the electrophoresis CNT of carbon steel surface of the present invention
Carry out according to the following steps：
(1) preparation of CNT colloidal solution：A. the hexadecyltrimethylammonium chloride of 1.0 ~ 2.5 g is weighed, is added to
In 1000 mL ethanol+isopropyl alcohol mixture, after 20 min are stirred at room temperature, the CNT of 1.0 ~ 3.0 g is added；
B. 1.5 h are processed using ultrasonic cell disruptor after 0.5 h is stirred at 45 DEG C；C. repeat step b 10 ~ 30 times, complete
Into the preparation of CNT colloidal solution；
(2) carbon steel pre-treatment：D. carbon steel is immersed ultrasonically treated 2 ~ 5 minutes in Wax removal water, then through the cleaning of one running water,
Three road deionized water cleanings, remove surface and oil contaminant；E. by through oil removing carbon steel immersion temperature be 45 ~ 50 DEG C, volume basis it is dense
Etch 1 ~ 3 minute in the hydrochloric acid solution for 10 ~ 15% is spent, then after one running water cleaning, three road deionized water cleanings, it is complete
Into the pre-treatment of carbon steel；
(3) carbon steel surface electrophoresis CNT micelle：F. carbon steel immersion step (1) after step (2) process is matched somebody with somebody
As negative electrode in the CNT colloidal solution of system, titanium net carries out electricity as anode, the voltage for applying 60 ~ 75 V at electrolytic cell two ends
4 ~ 10 min of swimming, rinse 10 ~ 60 s using isopropanol after taking-up, and 10 ~ 60 s in the nmp solution of PVDF are immersed after drying naturally,
60 ~ 180 s are rinsed using isopropanol after taking-up, and carbon steel surface electricity is completed after then 1 ~ 12 h being dried under conditions of 60 ~ 70 DEG C
Swimming CNT；
(4) chemical nickel plating：G. the carbon steel for being prepared by step (3)/carbon nano-tube electrophoretic layer composite immersion volume basis are dense
Etch 1 ~ 3 minute in the hydrochloric acid solution for 10 ~ 15% is spent, then is immersed after one running water cleaning, three road deionized water cleanings
Temperature is 10 ~ 30 min of plating in 85 ~ 95 DEG C of low-phosphorous chemical nickel-plating liquid, afterwards through one running water cleaning, three roads go from
Sub- water cleaning, then cold wind is dried up and completes the chemical nickel plating after the electrophoresis CNT of carbon steel surface.
In ethanol+isopropyl alcohol mixture described in a of step (1), ethanol and the volume ratio of isopropanol are 0.2 ~ 5.0；
In the nmp solution of the PVDF described in step (3), the mass percent of PVDF is 0.1 ~ 1.0%；It is low-phosphorous described in step (4)
It is 1 ~ 20 mg/ for the concentration of 3 ~ 18 g/L, KI that chemical nickel-plating liquid presses the concentration that the concentration of lactic acid is 5 ~ 25 mL/L, sodium glutamate
The ratio that L, the concentration of sodium hypophosphite are 10 ~ 20 g/L, the concentration of six hydration nickel sulfate is 25 ~ 35 g/L, by lactic acid, glutamic acid
Sodium, KI, sodium hypophosphite and six hydration nickel sulfate are well mixed in sequentially adding water, and adjustment pH is formulated for 5.8 ~ 6.4.
A kind of method that chemical nickel plating prepares high hydrogen evolution activity electrode after the electrophoresis CNT of carbon steel surface of the present invention
By carbon nanotube layer being prepared in carbon steel surface electrophoresis, not only can provide huge specific surface area for follow-up chemical Ni-plating layer
And increased electric conductivity.The carbon steel prepared after its chemical nickel plating on surface/carbon nano-tube electrophoretic layer/Ni-P alloy composite woods
Expect due to high catalytic surface product, good electric conductivity and excellent catalysis activity, therefore can show compared with for carbon steel
Write and improve hydrogen evolution activity, solve the high energy consumption issues that electrolytic hydrogen production is brought using carbon steel cathodes in sodium hydroxide solution.
Description of the drawings
Fig. 1 is one SEM image after the electrophoresis CNT of carbon steel surface of test；
Fig. 2 is one SEM image after carbon steel surface electrophoresis CNT carries out chemical nickel plating again of test；
Fig. 3 be test one prepare carbon steel/carbon nano-tube electrophoretic layer/Ni-P alloy composite materials in 1.0 M NaOH solutions,
Cathode-current density is 150 mA/cm2Under conditions of the potential-time curve that measures.
Specific embodiment
Specific embodiment one：One kind of present embodiment chemical nickel plating after the electrophoresis CNT of carbon steel surface prepares high
The method of hydrogen evolution activity electrode is carried out according to the following steps：
(1) preparation of CNT colloidal solution：A. the hexadecyltrimethylammonium chloride of 1.0 ~ 2.5 g is weighed, is added to
In 1000 mL ethanol+isopropyl alcohol mixture, after 20 min are stirred at room temperature, the CNT of 1.0 ~ 3.0 g is added；
B. 1.5 h are processed using ultrasonic cell disruptor after 0.5 h is stirred at 45 DEG C；C. repeat step b 10 ~ 30 times, complete
Into the preparation of CNT colloidal solution；
(2) carbon steel pre-treatment：D. carbon steel is immersed ultrasonically treated 2 ~ 5 minutes in Wax removal water, then through the cleaning of one running water,
Three road deionized water cleanings, remove surface and oil contaminant；E. by through oil removing carbon steel immersion temperature be 45 ~ 50 DEG C, volume basis it is dense
Etch 1 ~ 3 minute in the hydrochloric acid solution for 10 ~ 15% is spent, then after one running water cleaning, three road deionized water cleanings, it is complete
Into the pre-treatment of carbon steel；
(3) carbon steel surface electrophoresis CNT micelle：F. carbon steel immersion step (1) after step (2) process is matched somebody with somebody
As negative electrode in the CNT colloidal solution of system, titanium net carries out electricity as anode, the voltage for applying 60 ~ 75 V at electrolytic cell two ends
4 ~ 10 min of swimming, rinse 10 ~ 60 s using isopropanol after taking-up, and 10 ~ 60 s in the nmp solution of PVDF are immersed after drying naturally,
60 ~ 180 s are rinsed using isopropanol after taking-up, and carbon steel surface electricity is completed after then 1 ~ 12 h being dried under conditions of 60 ~ 70 DEG C
Swimming CNT；
(4) chemical nickel plating：G. the carbon steel for being prepared by step (3)/carbon nano-tube electrophoretic layer composite immersion volume basis are dense
Etch 1 ~ 3 minute in the hydrochloric acid solution for 10 ~ 15% is spent, then is immersed after one running water cleaning, three road deionized water cleanings
Temperature is 10 ~ 30 min of plating in 85 ~ 95 DEG C of low-phosphorous chemical nickel-plating liquid, afterwards through one running water cleaning, three roads go from
Sub- water cleaning, then cold wind is dried up and completes the chemical nickel plating after the electrophoresis CNT of carbon steel surface.
A kind of chemical nickel plating after the electrophoresis CNT of carbon steel surface of present embodiment prepares high hydrogen evolution activity electrode
Method not only can provide huge ratio table for follow-up chemical Ni-plating layer by preparing carbon nanotube layer in carbon steel surface electrophoresis
Area and increased electric conductivity.The carbon steel prepared after its chemical nickel plating on surface/carbon nano-tube electrophoretic layer/Ni-P alloys are multiple
Condensation material, therefore can compared with for carbon steel due to high catalytic surface product, good electric conductivity and excellent catalysis activity
To significantly improve hydrogen evolution activity, the high energy consumption issues that electrolytic hydrogen production is brought using carbon steel cathodes in sodium hydroxide solution are solved.
Specific embodiment two：Present embodiment and the second unlike specific embodiment one described in a of step (1)
In alcohol+isopropyl alcohol mixture, ethanol and the volume ratio of isopropanol are 0.2 ~ 5.0.Other are identical with specific embodiment one.
Specific embodiment three：Present embodiment from described in step unlike specific embodiment one or two (3)
In the nmp solution of PVDF, the mass percent of PVDF is 0.1 ~ 1.0%.Other are identical with specific embodiment one or two.
Specific embodiment four：Institute in step (4) unlike one of present embodiment and specific embodiment one to three
The low-phosphorous chemical nickel-plating liquid stated by the concentration of lactic acid be 5 ~ 25 mL/L, sodium glutamate concentration for the concentration of 3 ~ 18 g/L, KI be
The ratio that 1 ~ 20 mg/L, the concentration of sodium hypophosphite are 10 ~ 20 g/L, the concentration of six hydration nickel sulfate is 25 ~ 35 g/L, by breast
Acid, sodium glutamate, KI, sodium hypophosphite and six hydration nickel sulfate are well mixed in sequentially adding water, and adjustment pH is prepared for 5.8 ~ 6.4
Form.Other are identical with one of specific embodiment one to three.
With following verification experimental verification beneficial effects of the present invention：
Test one：A kind of chemical nickel plating after the electrophoresis CNT of carbon steel surface of this test prepares the side of high hydrogen evolution activity electrode
Method is carried out according to the following steps：
(1) preparation of CNT colloidal solution：A. the hexadecyltrimethylammonium chloride of 1.0 g is weighed, 1000 mL are added to
In ethanol+isopropyl alcohol mixture, after 20 min are stirred at room temperature, the CNT of 1.5 g is added；B. at 45 DEG C
1.5 h are processed using ultrasonic cell disruptor after stirring 0.5 h；C. repeat step b 15 times, complete CNT colloid
The preparation of liquid；
(2) carbon steel pre-treatment：D. carbon steel is immersed ultrasonically treated 5 minutes in Wax removal water, then through the cleaning of one running water, three
Road deionized water cleaning, removes surface and oil contaminant；E. the carbon steel through oil removing is immersed temperature for 45 DEG C, concentration expressed in percentage by volume is
Etch 1 minute in 15% hydrochloric acid solution, then after one running water cleaning, three road deionized water cleanings, before completing carbon steel
Process；
(3) carbon steel surface electrophoresis CNT micelle：F. carbon steel immersion step (1) after step (2) process is matched somebody with somebody
As negative electrode in the CNT colloidal solution of system, titanium net carries out electrophoresis 5 as anode, the voltage for applying 60 V at electrolytic cell two ends
Min, rinses 60 s using isopropanol after taking-up, and 20 s in the nmp solution of PVDF are immersed after drying naturally, and isopropyl is adopted after taking-up
Alcohol rinses 150 s, and carbon steel surface electrophoresis CNT is completed after then drying 10 h under conditions of 60 DEG C；
(4) chemical nickel plating：G. the carbon steel for being prepared by step (3)/carbon nano-tube electrophoretic layer composite immersion volume basis are dense
Etch 3 minutes in the hydrochloric acid solution for 15% are spent, then temperature are immersed after one running water cleaning, three road deionized water cleanings
For 10 min of plating in 85 DEG C of low-phosphorous chemical nickel-plating liquid, clean through one running water cleaning, three road deionized waters afterwards,
Then cold wind is dried up and completes the chemical nickel plating after the electrophoresis CNT of carbon steel surface.
In ethanol+isopropyl alcohol mixture described in a of step (1), ethanol and the volume ratio of isopropanol are 0.8；Step
(3) in the nmp solution of the PVDF described in, the mass percent of PVDF is 0.8%；Low-phosphorous chemical nickel plating described in step (4)
Liquid by the concentration of lactic acid be 25 mL/L, sodium glutamate concentration be 4 g/L, KI concentration be 10 mg/L, sodium hypophosphite it is dense
The ratio that the concentration for 18 g/L, six hydration nickel sulfate is 27 g/L is spent, by lactic acid, sodium glutamate, KI, sodium hypophosphite and six water
Close during nickel sulfate sequentially adds water and be well mixed, adjustment pH is formulated for 6.2.
SEM image of this test after the electrophoresis CNT of carbon steel surface is as shown in Figure 1.Carbon steel is through electricity as can be seen from Figure 1
After swimming CNT, CNT may be uniformly distributed in carbon steel surface.
SEM image of this test after carbon steel surface electrophoresis CNT carries out chemical nickel plating again is as shown in Figure 2.From Fig. 2
Understand that the Ni-P alloying pellets for obtaining are tiny, and uniformly can divide after carbon steel surface electrophoresis CNT carries out chemical nickel plating again
Cloth.
Carbon steel/carbon nano-tube electrophoretic layer/Ni-P alloy composite materials prepared by this test are in 1.0 M NaOH solutions, the moon
Electrode current density is 150 mA/cm2Under conditions of the potential-time curve that measures it is as shown in Figure 3.As can be seen from Figure 3, this test
The carbon steel of preparation/carbon nano-tube electrophoretic layer/Ni-P alloy composite materials are in 150 mA/cm2Current density under overpotential of hydrogen evolution
In 150 mV or so（Common carbon steel is in 150 mA/cm2Overpotential of hydrogen evolution under current density>500 mV）, effectively increase
The hydrogen evolution activity of carbon steel.
Carbon steel/carbon nano-tube electrophoretic layer/Ni-P alloy composite materials prepared by this test were in continuous electrolysis hydrogen manufacturing 720 hours
Afterwards, coating does not fall off, and overpotential of hydrogen evolution illustrates to prepare high hydrogen evolution activity electrode using the method steady still within 170 mV
It is fixed reliable.
Claims (4)
1. a kind of method that chemical nickel plating prepares high hydrogen evolution activity electrode after the electrophoresis CNT of carbon steel surface, it is characterised in that
A kind of method that chemical nickel plating after the electrophoresis CNT of carbon steel surface prepares high hydrogen evolution activity electrode is carried out according to the following steps：
(1) preparation of CNT colloidal solution：A. the hexadecyltrimethylammonium chloride of 1.0 ~ 2.5 g is weighed, is added to
In 1000 mL ethanol+isopropyl alcohol mixture, after 20 min are stirred at room temperature, the CNT of 1.0 ~ 3.0 g is added；
B. 1.5 h are processed using ultrasonic cell disruptor after 0.5 h is stirred at 45 DEG C；C. repeat step b 10 ~ 30 times, complete
Into the preparation of CNT colloidal solution；
(2) carbon steel pre-treatment：D. carbon steel is immersed ultrasonically treated 2 ~ 5 minutes in Wax removal water, then through the cleaning of one running water,
Three road deionized water cleanings, remove surface and oil contaminant；E. by through oil removing carbon steel immersion temperature be 45 ~ 50 DEG C, volume basis it is dense
Etch 1 ~ 3 minute in the hydrochloric acid solution for 10 ~ 15% is spent, then after one running water cleaning, three road deionized water cleanings, it is complete
Into the pre-treatment of carbon steel；
(3) carbon steel surface electrophoresis CNT micelle：F. carbon steel immersion step (1) after step (2) process is matched somebody with somebody
As negative electrode in the CNT colloidal solution of system, titanium net carries out electricity as anode, the voltage for applying 60 ~ 75 V at electrolytic cell two ends
4 ~ 10 min of swimming, rinse 10 ~ 60 s using isopropanol after taking-up, and 10 ~ 60 s in the nmp solution of PVDF are immersed after drying naturally,
60 ~ 180 s are rinsed using isopropanol after taking-up, and carbon steel surface electricity is completed after then 1 ~ 12 h being dried under conditions of 60 ~ 70 DEG C
Swimming CNT；
(4) chemical nickel plating：G. the carbon steel for being prepared by step (3)/carbon nano-tube electrophoretic layer composite immersion volume basis are dense
Etch 1 ~ 3 minute in the hydrochloric acid solution for 10 ~ 15% is spent, then is immersed after one running water cleaning, three road deionized water cleanings
Temperature is 10 ~ 30 min of plating in 85 ~ 95 DEG C of low-phosphorous chemical nickel-plating liquid, afterwards through one running water cleaning, three roads go from
Sub- water cleaning, then cold wind is dried up and completes the chemical nickel plating after the electrophoresis CNT of carbon steel surface.
2. one kind chemical nickel plating after the electrophoresis CNT of carbon steel surface according to claim 1 prepares high hydrogen evolution activity electricity
The method of pole, it is characterised in that the volume of ethanol and isopropanol in the ethanol+isopropyl alcohol mixture described in a of step (1)
Than for 0.2 ~ 5.0.
3. one kind chemical nickel plating after the electrophoresis CNT of carbon steel surface according to claim 1 prepares high hydrogen evolution activity electricity
The method of pole, it is characterised in that the mass percent of PVDF is 0.1 ~ 1.0% in the nmp solution of the PVDF described in step (3).
4. one kind chemical nickel plating after the electrophoresis CNT of carbon steel surface according to claim 1 prepares high hydrogen evolution activity electricity
The method of pole, it is characterised in that it is 5 ~ 25 mL/L, paddy ammonia that the low-phosphorous chemical nickel-plating liquid described in step (4) presses the concentration of lactic acid
The concentration of sour sodium for 3 ~ 18 g/L, KI concentration be 1 ~ 20 mg/L, sodium hypophosphite concentration be 10 ~ 20 g/L, six hydrated sulfuric acids
The concentration of nickel is the ratio of 25 ~ 35 g/L, and lactic acid, sodium glutamate, KI, sodium hypophosphite and six hydration nickel sulfate are sequentially added water
In be well mixed, adjustment pH be formulated for 5.8 ~ 6.4.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108624907A (en) * | 2018-04-26 | 2018-10-09 | 复旦大学 | Nonmetal basal body efficient catalytic electrode and preparation method thereof |
| CN110067004A (en) * | 2019-06-05 | 2019-07-30 | 苏州大学 | Ni-W-P/CNTs/CC catalysis electrode and preparation method and application |
| CN114908366A (en) * | 2022-06-08 | 2022-08-16 | 湘潭大学 | Preparation method of porous Ni-Cu/CNTs-Ni cathode material |
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| CN101255591A (en) * | 2008-04-03 | 2008-09-03 | 厦门大学 | Method for preparing carbon nano-tube/nano-nickel composite film |
| CN101550523A (en) * | 2009-05-07 | 2009-10-07 | 山东交通学院 | Nickel aluminide intermetal compound-carbon nanotube composite material and preparation thereof |
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| CN102142545A (en) * | 2011-02-28 | 2011-08-03 | 深圳市豪鹏科技有限公司 | Secondary battery anode piece and preparation method thereof |
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| CN101255591A (en) * | 2008-04-03 | 2008-09-03 | 厦门大学 | Method for preparing carbon nano-tube/nano-nickel composite film |
| CN101550523A (en) * | 2009-05-07 | 2009-10-07 | 山东交通学院 | Nickel aluminide intermetal compound-carbon nanotube composite material and preparation thereof |
| CN101781757A (en) * | 2010-03-12 | 2010-07-21 | 哈尔滨工业大学 | Method for chemically plating nano nickel particles on surface of multi-wall carbon nano tube without using palladium |
| CN102142545A (en) * | 2011-02-28 | 2011-08-03 | 深圳市豪鹏科技有限公司 | Secondary battery anode piece and preparation method thereof |
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| CN108624907A (en) * | 2018-04-26 | 2018-10-09 | 复旦大学 | Nonmetal basal body efficient catalytic electrode and preparation method thereof |
| CN110067004A (en) * | 2019-06-05 | 2019-07-30 | 苏州大学 | Ni-W-P/CNTs/CC catalysis electrode and preparation method and application |
| 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 |
| CN114908366A (en) * | 2022-06-08 | 2022-08-16 | 湘潭大学 | Preparation method of porous Ni-Cu/CNTs-Ni cathode material |
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