CN103280336A - Method for preparing foam nickel load carbon-coated nickel particle composite material - Google Patents

Method for preparing foam nickel load carbon-coated nickel particle composite material Download PDF

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CN103280336A
CN103280336A CN2013101853454A CN201310185345A CN103280336A CN 103280336 A CN103280336 A CN 103280336A CN 2013101853454 A CN2013101853454 A CN 2013101853454A CN 201310185345 A CN201310185345 A CN 201310185345A CN 103280336 A CN103280336 A CN 103280336A
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nickel
foam
composite material
aqueous solution
concentration
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CN103280336B (en
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赵乃勤
张淼
师春生
何春年
刘恩佐
李家俊
张翔
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Tianjin University
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Tianjin University
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13—Energy storage using capacitors

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Abstract

The invention discloses a method for preparing a foam nickel load carbon-coated nickel particle composite material. The method comprises the following steps of: performing hydrothermal carburization on foam nickel in mixed solution of triethylene glycol and NaOH to obtain carburized foam nickel; preparing electro-deposition plating solution by taking NiSO4.6H2O, NiCl2.6H2O and H3BO3 as solvents and taking Cl2H25SO4Na and C6H4SO2NNaCO.2H2O as additives; performing electro-deposition on nickel particles by taking the carburized foam nickel as an anode and taking a platinum electrode as a cathode; arranging the carburized foam nickel, on which nickel nanoparticles are deposited, in a square boat, and placing into a quartz tubular furnace together; and under the protection of argon gas of a certain flow, heating to 400-700 DEG C at a certain speed; and preserving heat for a while to obtain the foam nickel load carbon-coated nickel particle composite material. The method has the advantages of easiness, practicability, low energy consumption, short preparing period and easiness in industrial batch production, and the prepared composite material has contribution to improvement on the performance of a super capacitor.

Description

The preparation method of foamed nickel supported carbon coated nickel-particle composite material
Technical field
The present invention relates to a kind of preparation method of foamed nickel supported carbon coated nickel-particle composite material, belong to carbon-clad metal particulate composite technology.
Background technology
Because petroleum resources are shortage day by day, and the internal combustion engine tail gas discharge of burning petroleum is more and more serious to the pollution of environment, people are more and more for the research of novel energy device.Carry out the research and development of products such as hybrid power, fuel cell, chemical cell, capacitive means, and obtained certain effect.Wherein ultracapacitor so characteristic are maximized favourable factors and minimized unfavourable ones, and have more widely than battery and use, so countries in the world are all studying it of doing one's utmost.
Ultracapacitor has electric double layer capacitance and two kinds of mechanism of fake capacitance.At present because the energy density of fake capacitance and than electric capacity than the electric double layer excellence, the people's that its application is subjected to extensive concern.Metal and oxide thereof are the fake capacitance materials of using always.But the volume contraction that redox reaction produces in the application process expands and causes its less stable.From 1993 find the structure of carbon-coated nano lanthanum carbide first in arc evaporation graphite cigarette ash since, the carbon-clad metal nano particle has become one of research focus of world wide clinical practice worker with its particular shape structure and character, as a kind of new type functional composite material, it can increase stability of material to a certain extent.Therefore prepare the carbon-clad metal nano particle as electrode material for super capacitor, can improve the ultracapacitor performance.
Existing carbon-clad metal nano particle is as the correlative study of electrode material for super capacitor in the present existing report, but in the preparation process, the dispersiveness of carbon encapsulated material can not reach optimum state, in addition, in technology for preparing electrode, generally need to add binding agent, to improve the associativity of electroactive material and collector, but can increase the equivalent series resistance of electrode like this, be unfavorable for the ultracapacitor optimization in Properties.The carbon-clad metal nano particle that foamed nickel supported carbon coated nickel-particle composite material can obtain disperseing on the one hand on the other hand, need not to introduce the adhesive preparation electrode in application process, has improved the conductivity of electrode.At present, about the preparation method of foamed nickel supported carbon coated nickel-particle composite material, do not see relevant report as yet.
Summary of the invention
The present invention aims to provide a kind of preparation method of foamed nickel supported carbon coated nickel-particle composite material, and this procedure is simple, has good conduction property and electrochemical stability with the prepared composite material of the method.
The present invention is realized that by following technical proposals a kind of preparation method of foamed nickel supported carbon coated nickel-particle composite material is characterized in that comprising following process:
1) nickel foam is distinguished successively at acetone, deionized water, 1molL -1Ultrasonic cleaning in the hydrochloric acid, air dry is standby;
2) adding volume ratio in reactor is triethylene glycol and the concentration 1molL of 20:1 -1The NaOH aqueous solution, glass bar stirs, and obtains reaction solution, the nickel foam that step 1) is handled well is put into reaction solution then, carburizing 12 ~ 24h under 150 ℃ ~ 250 ℃ conditions of temperature, be cooled to room temperature after, take out nickel foam, with deionized water rinsing to the no Cl in nickel foam surface -, drying, obtain carbon impregnated foam nickel;
3) preparation plating bath: respectively with NiSO 46H 2O, NiCl 26H 2O and H 3BO 3For the solute compound concentration is 300gL -1NiSO 4The aqueous solution, concentration are 40gL -1NiCl 2The aqueous solution and concentration are 35gL -1H 3BO 3The aqueous solution, under 30 ℃ of stirring in water bath conditions, three kinds of aqueous solution mix according to volume ratio 1:1:1, mixed solution is warming up to 40 ~ 60 ℃ stirs, and adding mass concentration in the mixed solution is 4.25gL -1C 12H 25SO 4Na and C 6H 4SO 2NNaCO2H 2O, wherein C 12H 25SO 4Na and C 6H 4SO 2NNaCO2H 2The mass ratio of O is 1:50, and adding concentration then is 3molL -1H 2SO 4Regulate pH to 2.0, obtain plating bath;
4) in the plating bath of step 3) preparation, with step 2) carbon impregnated foam nickel is anode, is negative electrode with the platinum electrode, under the 0.1A current condition, carries out 10 ~ 30s electro-deposition, obtains depositing the carbon impregnated foam nickel of nano nickel particles, air dry is standby;
5) the carbon impregnated foam nickel that step 4) is deposited nano nickel particles places Noah's ark, it is lain against in the quartz tube furnace, and be 50 ~ 300 mLmin at flow -1Argon shield under, with 4 ~ 20 ℃ of min -1Speed be warming up to 400 ~ 700 ℃ after, the insulation 1 ~ 7h, cool to room temperature with the furnace, obtain foamed nickel supported carbon coated nickel-particle composite material.
Compared with prior art, the invention has the beneficial effects as follows: simple to operate, cost is low.Equipment is common drying box, constant pressure source, and quartz tube furnace need not other large-scale or complex device.Foamed nickel supported carbon coated nickel-particle composite material can be by carburizing temperature, the time in the hydro-thermal carburizing process, and electrodeposition process electric current, time parameter and annealing process temperature, time, heating rate are controlled.The composite material of the method preparation can effectively improve the chemical property of ultracapacitor as electrode of super capacitor.
Description of drawings
Fig. 1 is the SEM figure of the embodiment of the invention two obtained foamed nickel supported carbon coated nickel-particle composite materials
Fig. 2 is the TEM figure of the embodiment of the invention two obtained foamed nickel supported carbon coated nickel-particle composite materials.
Embodiment
Be further described below in conjunction with the present invention of embodiment, these embodiment just are used for explanation the present invention, do not limit the present invention.
Embodiment one
1cm * 2.5cm * 2mm nickel foam is distinguished successively at acetone, deionized water, 1molL -1Ultrasonic cleaning in the hydrochloric acid, air dry is standby; Adding volume ratio in reactor is 20mL triethylene glycol and concentration 1mL 1molL -1The NaOH aqueous solution, glass bar stirs, and obtains reaction solution, then the nickel foam of handling well is put into reaction solution, carburizing 12h under 200 ℃ of conditions of temperature, be cooled to room temperature after, take out nickel foam, with deionized water rinsing to the no Cl in nickel foam surface -, air dry under 30 ℃ of conditions obtains carbon impregnated foam nickel; Take by weighing 30gNiSO 46H 2O, 4gNiCl 26H 2O and 3.5gH 3BO 3Join respectively in the 100mL deionized water, obtained aqueous solution under 30 ℃ of stirring in water bath conditions is then with NiSO 4The aqueous solution and NiCl 2The aqueous solution is to H 3BO 3The aqueous solution slowly adds, and mixed solution is warming up to 50 ℃ stirs, and takes by weighing C simultaneously 12H 25SO 4Na0.025g and C 6H 4SO 2NNaCO2H 2O1.25g joins in the mixed solution, adds concentration 3molL then -1H 2SO 4Regulate pH to 2.0, obtain plating bath; Being the electro-deposition plating bath with the plating bath, is anode with the nickel foam after the carburizing, is negative electrode with 1cm * 2.5cm platinum electrode, under the 0.1A current condition, carries out the 10s electro-deposition, has obtained depositing the carbon impregnated foam nickel of nano nickel particles, and air dry is standby; The carbon impregnated foam nickel that has deposited nano nickel particles being placed Noah's ark, it is lain against in the quartz tube furnace, is 100 mLmin at flow -1Argon shield under, with 20 ℃ of min -1Speed be warming up to 700 ℃ after, the insulation 2h, obtain foamed nickel supported carbon coated nickel-particle composite material.
Embodiment two
1cm * 2.5cm * 2mm nickel foam is distinguished successively at acetone, deionized water, 1molL -1Ultrasonic cleaning in the hydrochloric acid, air dry is standby; Adding volume ratio in reactor is 20mL triethylene glycol and concentration 1mL 1molL -1The NaOH aqueous solution, glass bar stirs, and obtains reaction solution, then the nickel foam of handling well is put into reaction solution, carburizing 20h under 200 ℃ of conditions of temperature, be cooled to room temperature after, take out nickel foam, with deionized water rinsing to the no Cl in nickel foam surface -, air dry under 30 ℃ of conditions obtains carbon impregnated foam nickel; Take by weighing 30gNiSO 46H 2O, 4gNiCl 26H 2O and 3.5gH 3BO 3Join respectively in the 100mL deionized water, obtained aqueous solution under 30 ℃ of stirring in water bath conditions is then with NiSO 4The aqueous solution and NiCl 2The aqueous solution is to H 3BO 3The aqueous solution slowly adds, and mixed solution is warming up to 50 ℃ stirs, and takes by weighing C simultaneously 12H 25SO 4Na0.025g and C 6H 4SO 2NNaCO2H 2O1.25g joins in the mixed solution, adds concentration 3molL then -1H 2SO 4Regulate pH to 2.0, obtain plating bath; Being the electro-deposition plating bath with the plating bath, is anode with the nickel foam after the carburizing, is negative electrode with 1cm * 2.5cm platinum electrode, under the 0.1A current condition, carries out the 20s electro-deposition, has obtained depositing the carbon impregnated foam nickel of nano nickel particles, and air dry is standby; The carbon impregnated foam nickel that has deposited nano nickel particles being placed Noah's ark, it is lain against in the quartz tube furnace, is 100 mLmin at flow -1Argon shield under, with 10 ℃ of min -1Speed be warming up to 500 ℃ after, the insulation 5h, obtain foamed nickel supported carbon coated nickel-particle composite material.
Embodiment three
1cm * 2.5cm * 2mm nickel foam is distinguished successively at acetone, deionized water, 1molL -1Ultrasonic cleaning in the hydrochloric acid, air dry is standby; Adding volume ratio in reactor is 20mL triethylene glycol and concentration 1mL 1molL -1The NaOH aqueous solution, glass bar stirs, and obtains reaction solution, then the nickel foam of handling well is put into reaction solution, carburizing 24h under 250 ℃ of conditions of temperature, be cooled to room temperature after, take out nickel foam, with deionized water rinsing to the no Cl in nickel foam surface -, air dry under 30 ℃ of conditions obtains carbon impregnated foam nickel; Take by weighing 30gNiSO 46H 2O, 4gNiCl 26H 2O and 3.5gH 3BO 3Join respectively in the 100mL deionized water, obtained aqueous solution under 30 ℃ of stirring in water bath conditions is then with NiSO 4The aqueous solution and NiCl 2The aqueous solution is to H 3BO 3The aqueous solution slowly adds, and mixed solution is warming up to 50 ℃ stirs, and takes by weighing C simultaneously 12H 25SO 4Na0.025g and C 6H 4SO 2NNaCO2H 2O1.25g joins in the mixed solution, adds concentration 3molL then -1H 2SO 4Regulate pH to 2.0, obtain plating bath; Being the electro-deposition plating bath with the plating bath, is anode with the nickel foam after the carburizing, is negative electrode with 1cm * 2.5cm platinum electrode, under the 0.1A current condition, carries out the 30s electro-deposition, has obtained depositing the carbon impregnated foam nickel of nano nickel particles, and air dry is standby; The carbon impregnated foam nickel that has deposited nano nickel particles being placed Noah's ark, it is lain against in the quartz tube furnace, is 100 mLmin at flow -1Argon shield under, with 10 ℃ of min -1Speed be warming up to 400 ℃ after, the insulation 7h, obtain foamed nickel supported carbon coated nickel-particle composite material.
Embodiment four
1cm * 2.5cm * 2mm nickel foam is distinguished successively at acetone, deionized water, 1molL -1Ultrasonic cleaning in the hydrochloric acid, air dry is standby; Adding volume ratio in reactor is 20mL triethylene glycol and concentration 1mL 1molL -1The NaOH aqueous solution, glass bar stirs, and obtains reaction solution, then the nickel foam of handling well is put into reaction solution, carburizing 15h under 200 ℃ of conditions of temperature, be cooled to room temperature after, take out nickel foam, with deionized water rinsing to the no Cl in nickel foam surface -, air dry under 30 ℃ of conditions obtains carbon impregnated foam nickel; Take by weighing 30gNiSO 46H 2O, 4gNiCl 26H 2O and 3.5gH 3BO 3Join respectively in the 100mL deionized water, obtained aqueous solution under 30 ℃ of stirring in water bath conditions is then with NiSO 4The aqueous solution and NiCl 2The aqueous solution is to H 3BO 3The aqueous solution slowly adds, and mixed solution is warming up to 50 ℃ stirs, and takes by weighing C simultaneously 12H 25SO 4Na0.025g and C 6H 4SO 2NNaCO2H 2O1.25g joins in the mixed solution, adds concentration 3molL then -1H 2SO 4Regulate pH to 2.0, obtain plating bath; Being the electro-deposition plating bath with the plating bath, is anode with the nickel foam after the carburizing, is negative electrode with 1cm * 2.5cm platinum electrode, under the 0.1A current condition, carries out the 15s electro-deposition, has obtained depositing the carbon impregnated foam nickel of nano nickel particles, and air dry is standby; The carbon impregnated foam nickel that has deposited nano nickel particles being placed Noah's ark, it is lain against in the quartz tube furnace, is 100 mLmin at flow -1Argon shield under, with 10 ℃ of min -1Speed be warming up to 500 ℃ after, the insulation 7h, obtain foamed nickel supported carbon coated nickel-particle composite material.

Claims (1)

1. the preparation method of a foamed nickel supported carbon coated nickel-particle composite material is characterized in that comprising following process:
1) nickel foam is distinguished successively at acetone, deionized water, 1molL -1Ultrasonic cleaning in the hydrochloric acid, air dry is standby;
2) adding volume ratio in reactor is triethylene glycol and the concentration 1molL of 20:1 -1The NaOH aqueous solution, glass bar stirs, and obtains reaction solution, the nickel foam that step 1) is handled well is put into reaction solution then, carburizing 12 ~ 24h under 150 ℃ ~ 250 ℃ conditions of temperature, be cooled to room temperature after, take out nickel foam, with deionized water rinsing to the no Cl in nickel foam surface -, drying, obtain carbon impregnated foam nickel;
3) preparation plating bath: respectively with NiSO 46H 2O, NiCl 26H 2O and H 3BO 3For the solute compound concentration is 300gL -1NiSO 4The aqueous solution, concentration are 40gL -1NiCl 2The aqueous solution and concentration are 35gL -1H 3BO 3The aqueous solution, under 30 ℃ of stirring in water bath conditions, three kinds of aqueous solution mix according to volume ratio 1:1:1, mixed solution is warming up to 40 ~ 60 ℃ stirs, and adding mass concentration in the mixed solution is 4.25gL -1C 12H 25SO 4Na and C 6H 4SO 2NNaCO2H 2O, wherein C 12H 25SO 4Na and C 6H 4SO 2NNaCO2H 2The mass ratio of O is 1:50, and adding concentration then is 3molL -1H 2SO 4Regulate pH to 2.0, obtain plating bath;
4) in the plating bath of step 3) preparation, with step 2) carbon impregnated foam nickel is anode, is negative electrode with the platinum electrode, under the 0.1A current condition, carries out 10 ~ 30s electro-deposition, obtains depositing the carbon impregnated foam nickel of nano nickel particles, air dry is standby;
5) the carbon impregnated foam nickel that step 4) is deposited nano nickel particles places Noah's ark, it is lain against in the quartz tube furnace, and be 50 ~ 300 mLmin at flow -1Argon shield under, with 4 ~ 20 ℃ of min -1Speed be warming up to 400 ~ 700 ℃ after, the insulation 1 ~ 7h, cool to room temperature with the furnace, obtain foamed nickel supported carbon coated nickel-particle composite material.
CN201310185345.4A 2013-05-20 2013-05-20 The preparation method of foamed nickel supported carbon coated nickel-particle composite material Expired - Fee Related CN103280336B (en)

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CN105197878A (en) * 2015-06-23 2015-12-30 华东师范大学 Preparation method for implementing electron field emission device by use of graphene
CN105632781A (en) * 2016-03-03 2016-06-01 哈尔滨工程大学 Preparation method of super capacitor electrode material containing cadmium sulfide
CN111554501A (en) * 2020-04-28 2020-08-18 天津大学 Preparation method of superparamagnetic nickel nanoparticles for magnetically adsorbing bacteria and spores

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Publication number Priority date Publication date Assignee Title
CN105197878A (en) * 2015-06-23 2015-12-30 华东师范大学 Preparation method for implementing electron field emission device by use of graphene
CN105632781A (en) * 2016-03-03 2016-06-01 哈尔滨工程大学 Preparation method of super capacitor electrode material containing cadmium sulfide
CN105632781B (en) * 2016-03-03 2018-07-24 哈尔滨工程大学 A kind of preparation method of the electrode material for super capacitor containing cadmium sulfide
CN111554501A (en) * 2020-04-28 2020-08-18 天津大学 Preparation method of superparamagnetic nickel nanoparticles for magnetically adsorbing bacteria and spores

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