CN105618789A - Preparation method of nitrogen-doped carbon nano tube packaging cobalt nanoparticles - Google Patents
Preparation method of nitrogen-doped carbon nano tube packaging cobalt nanoparticles Download PDFInfo
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Abstract
The invention discloses a preparation method of nitrogen-doped carbon nano tube packaging cobalt nanoparticles. The preparation method comprises the steps that cobalt salt and imidazole are dissolved in water, and heating is conducted for removing a solvent, so that purple red solid powder is obtained; the solid powder is placed in a tube furnace; inert gas is introduced into the tube furnace, the temperature is increased to 600-1100 DEG C and kept for 0.5-4 hours, and cooling is conducted till the indoor temperature is reached; and an obtained solid is treated for 6-24 hours in an acid solution at the temperature below 100 DEG C, and the material is obtained after filtering, washing and drying. According to the material, the granularity of the cobalt nanoparticles is 2-20 nm, the content, by weight, of cobalt is 2%-20%, and the content, by weight, of doped nitrogen is 1%-20%. The material can serve as a catalyst for the hydrogen evolution reaction in an electrolyte with the pH value being 0-15 and can also serve as a catalyst for the oxygen evolution reaction under the alkaline condition that the pH value is 13-15. The price of a precursor adopted in the method is low, the preparation process is easy and convenient to implement, and large-scale preparation can be achieved.
Description
Technical field
The present invention relates to a kind of with the mixture of cobalt salt and imidazoles for presoma, by high temperature pyrolysis and follow-up pickling processes, the method preparing nitrogen-doped carbon nanometer pipe encapsulation cobalt nano-particle.
Background technology
Hydrogen, as the high-grade energy of a kind of pollution-free reusable edible, is increasingly subject to people's attention. It can with greenhouse gases CO2By chemical conversion, generate the raw material of industry (methanol etc.), it is also possible to directly as the fuel of fuel cell. But the development and utilization of Hydrogen Energy, first have to solve cheap hydrogen source problem. The technology of preparing of hydrogen mainly includes gas renormalizing and hydrogen production from coal gasification, biomass hydrogen preparation, water electrolysis hydrogen producing and photolysis hydrogen manufacturing etc. The water electrolysis hydrogen producing history of existing more than 200 year so far, is prepare ultra-high purity hydrogen (> 99.995%) simplest method, but owing to water electrolysis process consumes electric energy relatively greatly, the 4% of hydrogen Jin Zhan world hydrogen output prepared by water electrolysis. Along with developing rapidly and to CO of regenerative resource2The restriction of gas discharging, water electrolysis hydrogen producing will play an increasingly important role. If combined with photovoltaic generation, hydroelectric generation and wind-power electricity generation by water electrolysis hydrogen producing, water electrolysis hydrogen producing will have a good application prospect.
Can at 1��3Acm as the electrolyzer of dielectric film using PEM-2High current density under work, volume is little, and efficiency is high, and the hydrogen purity of generation may be up to 99.995%, it is believed that is the most promising water electrolysis technology. The positive and negative end of electrolysis water there occurs oxygen evolution reaction and evolving hydrogen reaction respectively. But widely used platinum based noble metal liberation of hydrogen catalyst and iridio noble metal oxygen-separating catalyst, owing to reserves are limited, expensive, largely constrain the development of the water electrolysis technology based on PEM. In the last few years, cheap catalyst is sought to substitute noble metal and to improve its electrocatalysis characteristic and receive and increasingly pay close attention to widely. From the volcano type curve of evolving hydrogen reaction it can be seen that the evolving hydrogen reaction activity of cobalt is higher. But cobalt is easily subject to corrode under strong acid or basic conditions, and long-term recycling, the easy agglomeration of catalyst, unstable properties. A kind of effective solution is to be coated with by cobalt simple substance carbon-coating, improves its resistance to corrosion and suppresses growing up of catalyst. It addition, oxygen evolution reaction causes higher overpotential due to dynamic process slowly, cause relatively low energy conversion efficiency, be therefore the factor more restricted in the reaction of electrolysis water. Owing to a lot of electrochemical reactions are had higher electrocatalysis characteristic by transition metal, therefore cobalt simple substance carbon-coating cladding is put forward high oxygen separated performance.
Preparing the research of the transition-metal catalyst of carbon encapsulation, researcher has done substantial amounts of work, and achieves substantial progress.
The preparation method that Chinese patent CN201110435881.6 discloses a kind of pod-like carbon nanotube encapsulation non-noble metal nanoparticles: by alkali metal or derivatives thereof and metallocene compound in inert gas shielding lower seal to autoclave; Keep 1��20 hour in 150��500 DEG C; The sample of gained processes 3��8 hours in acid solution; Then wash respectively and sucking filtration with water and ethanol, until solution is in neutrality; Gained sample drying, namely obtains the non-noble metal nanoparticles of pod-like carbon nanotube encapsulation.
The preparation method that Chinese patent CN201310065472.0 discloses a kind of carbon coated magnetic metal nanoparticle: using explosive, metal simple substance cobalt or the nickel such as RDX, tetryl or HMX and carbonaceous organic material dicyandiamide or tripolycyanamide mixing as reactant; Reactant is pressed into block, loads and reactor seals evacuation, reactor heating is blasted to 200��250 DEG C, obtains the magnetic metal nano-particle of carbon parcel.
Chinese patent CN201210136642.5 discloses a kind of method preparing the carbon nano oxidized tin composite material of parcel: mix as reactant with water-soluble biological macromole by the mass ratio of 1:0.3��1:10 using stannic water soluble salt, back flow reaction soluble in water generates precipitate, reactant liquor is cooled to room temperature and is separated by precipitate, dry. Dried precipitate is placed in the tube furnace of inert gas shielding, at the heating temperatures 2��10 hours of 400��800 DEG C, obtains the nano oxidized tin composite material of carbon parcel.
The preparation method that Chinese patent CN201110076660.4 discloses a kind of carbon parcel composite titania material: put in calorstat after under magnetic stirring 150��500mg titanium dioxide and sucrose solution that mass concentration is 1%��10% being sufficiently mixed according to mass ratio 1:2��10, at 100 DEG C��150 DEG C temperature, reaction 2��6h, makes sucrose carbonization; The material of gained is pulverized last calcining at constant temperature 2��6 hours in the air atmosphere of 400��700 DEG C, prepare the composite of carbon parcel titanium dioxide.
Summary of the invention
The preparation method that the invention discloses a kind of nitrogen-doped carbon nanometer pipe encapsulation cobalt nano-particle.
A kind of cobalt nano-particle of nitrogen-doped carbon nanometer pipe encapsulation, its preparation method is as follows:
Step 1: respectively cobalt salt and imidazoles are dissolved in water, Homogeneous phase mixing post-heating removes solvent according to a certain percentage, obtains pressed powder;
Step 2: be placed in quartz boat by pressed powder, is then placed in equipped with in the tube furnace of quartz ampoule;
Step 3: pass into noble gas, then raises temperature to 600��1100 DEG C by certain heating rate, and keeps 0.5��4 hour, be cooled to room temperature;
Step 4: processed 6��24 hours under acid solution and the temperature lower than 100 DEG C by the solid obtained, after filtering washing drying, obtains the cobalt nano-particle of nitrogen-doped carbon nanometer pipe encapsulation.
Cobalt salt can be cobaltous acetate, cobalt nitrate or cobaltous chloride.
In mixed solution, the mass ratio of cobalt salt and imidazoles is between 1:10��10:1;
The central authorities of tube furnace it are placed in equipped with the quartz boat of pressed powder.
Described noble gas includes one or two or more kinds in nitrogen, argon or helium, and flow velocity is at 20��100mLmin-1Between.
Heat treated heating rate is 5��20 DEG C of min-1��
Acid solution can be perchloric acid, sulphuric acid, hydrochloric acid or nitric acid, and concentration is at 0.1��2molL-1Between.
The cobalt nano-particle of the nitrogen-doped carbon nanometer pipe encapsulation of preparation, cobalt nanometer particle size is between 2��20nm, and cobalt carrying capacity is between 2��20wt%, and the content of doping nitrogen is between 1��20wt%.
This material can as the catalyst of evolving hydrogen reaction in the electrolyte that pH value is 0-15, and under the alkali condition that pH value is 13-15, it is also possible to as the catalyst of oxygen evolution reaction.
The presoma that this method uses is cheap, and preparation process is easy, it may be achieved prepared by scale.
Accompanying drawing explanation
Fig. 1 is X-ray diffraction (XRD) figure of obtained nitrogen-doped carbon nanometer pipe encapsulation cobalt nano-particle (CoN-C) in embodiment 1. Can be seen that 44.2 ��, the diffraction maximum of 51.5 �� and 75.8 �� belongs to the diffraction maximum of metal Co.
Fig. 2 is transmission electron microscope (TEM) figure of obtained nitrogen-doped carbon nanometer pipe encapsulation cobalt nano-particle (CoN-C) in embodiment 1. Can be seen that Co nano-particle is packaged in CNT.
Fig. 3 is Raman (Raman) spectrogram of obtained nitrogen-doped carbon nanometer pipe encapsulation cobalt nano-particle (CoN-C) in embodiment 2. Can be seen that D, G peak is respectively at 1355cm-1And 1585cm-1Place. ID/IGValue can, as the index weighing degree of graphitization, be worth more little, and degree of graphitization is more high. Figure can be seen that ID/IG=0.73, illustrate that degree of graphitization is higher.
Fig. 4 is the x-ray photoelectron spectrogram (XPS) of the N1s of obtained nitrogen-doped carbon nanometer pipe encapsulation cobalt nano-particle (CoN-C) in embodiment 3. N1s can fit to the nitrogen of three kinds of forms, respectively pyridine nitrogen (398.5eV), pyrroles's nitrogen (400.3eV) and graphitization nitrogen (401.4eV). Electro catalytic activity depends primarily on pyridine nitrogen and the content of graphitization nitrogen. As can be seen from the figure pyridine nitrogen and graphitization nitrogen account for the 70% of total nitrogen content.
The nitrogen-doped carbon nanometer pipe that Fig. 5 is obtained in embodiment 1 encapsulates the cobalt nano-particle (CoN-C) Hydrogen Evolution Performance test under strong acid electrolyte. Test condition: 25 DEG C, 2500rpm, 1MHClO4Aqueous solution. Test process: 8mg catalyst mixes with 1mL ethanol, after ultrasonic 3min, instills 50uL5%nafion solution, continues ultrasonic 30min, obtain catalyst slurry. Take 25uL slurry drops on the glass-carbon electrode that diameter is 5mm, naturally dry. Carrying out test linear scanning in 1MHClO4 solution, sweep limits is 0.1��-0.7V (vs.RHE), sweeps speed 2mVS-1. Conclusion: electric current reaches 10mVs-1Time, the overpotential of CoN-C and MWCNT respectively 0.20V and 0.61V.
The nitrogen-doped carbon nanometer pipe that Fig. 6 is obtained in embodiment 2 encapsulates the cobalt nano-particle (CoN-C) Hydrogen Evolution Performance test under highly basic electrolyte. Test condition: 25 DEG C, 2500rpm, 1MKOH. Test process: 8mg catalyst mixes with 1mL ethanol, after ultrasonic 3min, instills 50uL5%nafion solution, continues ultrasonic 30min, obtain catalyst slurry. Take 25uL slurry drops on the glass-carbon electrode that diameter is 5mm, naturally dry. Carrying out test linear scanning in 1MKOH solution, sweep limits is 0.1��-0.7V (vs.RHE), sweeps speed 2mVS-1. Conclusion: electric current reaches 10mVs-1Time, CoN-C overpotential respectively 0.21V.
Fig. 7 is the analysis oxygen performance test of nitrogen-doped carbon nanometer pipe encapsulation cobalt nano-particle (CoN-C) obtained in embodiment 2. Test condition: 25 DEG C, 2500rpm, 1MKOH. Test process: 8mg catalyst mixes with 1mL ethanol, after ultrasonic 3min, instills 50uL5%nafion solution, continues ultrasonic 30min, obtain catalyst slurry. Take 25uL slurry drops on the glass-carbon electrode that diameter is 5mm, naturally dry. Carrying out test linear scanning in 1MKOH solution, sweep limits is 0.1��-0.7V (vs.RHE), sweeps speed 2mVS-1. Conclusion: electric current reaches 10mVs-1Time, the voltage needed for CoN-C is 1.63V, lower than the voltage (1.69V) needed for Pt/C. The electrolysis aqueous energy that Fig. 8 is is the positive and negative electrode of alkaline electrolysis water electrolytic cell with obtained nitrogen-doped carbon nanometer pipe encapsulation cobalt nano-particle (CoN-C) in embodiment 3. Test process: Toray carbon paper (TorayTGP-H-060, TorayIndustriesInc.) is as the transition zone of anode and negative electrode; Diffusion layer is made up of carbon black ValcanXC-72R and politef, and specific practice is by 1.2mgcm-2Carbon black and account for the politef of diffusion layer gross mass 40% and be made into serosity and be applied on transition zone, and heat 1h in 350 DEG C in air atmosphere; Catalytic Layer be catalyst and 5wt.%Nafion solution are mixed in aqueous according to the mass ratio of 1:1, ultrasonic disperse being applied on diffusion layer in 70 DEG C. Finally, the negative electrode of 2.1cm �� 2.1cm and anode are respectively placed in the two sides of NafionNRE-212 film and by the pressure hot pressing 3min of 1MPa at 130 DEG C, namely form membrane electrode. Being fixed on monocell by two panels silicagel pad by membrane electrode, monocell uses the flow-field plate of graphite and gold-plated rustless steel hot plate. Utilize high pressure constant flow pump by 1MKOH solution with 2mLmin-1Flow be passed in the anode and cathode of electrolyzer, electrolysis carries out linear scanning test at 80 DEG C. Sweep limits is 0��1.9V, and sweeping speed is 10mVs-1��
Detailed description of the invention
The method that the present invention prepares nitrogen-doped carbon nanometer pipe encapsulation cobalt nano-particle is as follows: respectively cobalt salt and imidazoles is dissolved in water, removes solvent according to different proportion mix homogeneously post-heating, obtain aubergine pressed powder; Pressed powder is placed in quartz boat, is then placed in equipped with in the tube furnace of quartz ampoule; Pass into the noble gas of certain flow rate, then raise temperature to design temperature, and keep certain time, be cooled to room temperature; The solid obtained is processed 12��36 hours under acid solution and the temperature lower than 100 DEG C, after filtering washing drying, obtains the cobalt nano-particle of nitrogen-doped carbon nanometer pipe encapsulation.
Embodiment 1
Weigh 5g imidazoles and 1g cobaltous acetate is dissolved in 150mL water respectively, at 90 DEG C, after mix homogeneously, remove solvent; Solid mixture is placed in quartz boat, is then placed in equipped with in the tube furnace of quartz ampoule, is 100mLmin at flow velocity-1Nitrogen atmosphere under, with 5 DEG C of min-1Speed raise temperature to 700 DEG C, and keep 5 hours, take out after being cooled to room temperature. Obtained solid is joined 0.5molL-1HClO4In solution, process 24 hours at 80 DEG C, after filtering washing and drying, obtain the cobalt nano-particle of nitrogen-doped carbon nanometer pipe encapsulation.
Embodiment 2
Weigh 5g imidazoles and 10g cobalt nitrate is dissolved in 150mL water respectively, at 90 DEG C, after mix homogeneously, remove solvent; Solid mixture is placed in quartz boat, is then placed in equipped with in the tube furnace of quartz ampoule, is 50mLmin at flow velocity-1Argon gas atmosphere under, with 10 DEG C of min-1Speed raise temperature to 600 DEG C, and keep 2 hours, take out after being cooled to room temperature. Obtained solid is joined 1molL-1In HCl solution, process 24 hours at 80 DEG C, after filtering washing and drying, obtain the cobalt nano-particle of nitrogen-doped carbon nanometer pipe encapsulation.
Embodiment 3
Weigh 1g imidazoles and 5g cobaltous chloride is dissolved in 150mL water respectively, at 90 DEG C, after mix homogeneously, remove solvent; Solid mixture is placed in quartz boat, is then placed in equipped with in the tube furnace of quartz ampoule, is 150mLmin at flow velocity-1Nitrogen atmosphere under, with 20 DEG C of min-1Raise temperature to 1100 DEG C, and keep 3 hours, take out after being subsequently cooled to room temperature. Obtained solid is joined 0.5molL-1HNO3In solution, process 24 hours at 80 DEG C, after filtering washing and drying, obtain the cobalt nano-particle of nitrogen-doped carbon nanometer pipe encapsulation.
Claims (8)
1. the preparation method of a nitrogen-doped carbon nanometer pipe encapsulation cobalt nano-particle, it is characterised in that:
Step 1: respectively cobalt salt and imidazoles are dissolved in water, is proportionally uniformly mixed into mixed solution post-heating and removes aqueous solvent, obtain pressed powder; In mixed solution, the mass ratio of cobalt salt and imidazoles is between 1:10��10:1;
Step 2: be placed in quartz boat by pressed powder, is then placed in tube furnace;
Step 3: pass into the gas of inert atmosphere in tube furnace, then tube furnace raises temperature to 600��1100 DEG C, and keeps 0.5��4 hour, is cooled to room temperature;
Step 4: processed 6��24 hours under acid solution and the temperature lower than 100 DEG C by the solid obtained, after filtering washing drying, obtains the cobalt nano-particle of nitrogen-doped carbon nanometer pipe encapsulation.
2. preparation method as claimed in claim 1, it is characterised in that: cobalt salt can be cobaltous acetate, cobalt nitrate or cobaltous chloride.
3. preparation method as claimed in claim 1, it is characterised in that: the gas of described inert atmosphere includes one or two or more kinds in nitrogen, argon or helium, and the flow velocity in gas inlet pipe formula stove is at 20��100mLmin-1Between.
4. preparation method as claimed in claim 1, it is characterised in that: it is 5��10 DEG C of min that tube furnace raises the heating rate of temperature course-1��
5. preparation method as claimed in claim 1, it is characterised in that: the temperature lower than 100 DEG C refers between 60��90 DEG C of temperature.
6. preparation method as claimed in claim 1, it is characterised in that: acid solution can be perchloric acid, sulphuric acid, hydrochloric acid or nitric acid, and concentration is at 0.2��1molL-1Between.
7. preparation method as claimed in claim 1, it is characterised in that: the cobalt nano-particle of the nitrogen-doped carbon nanometer pipe encapsulation of preparation, cobalt nanometer particle size is between 2��20nm, and cobalt content is between 2��20wt%, and the content of doping nitrogen is between 1��20wt%.
8. preparation method as claimed in claim 1, it is characterized in that: this nitrogen-doped carbon nanometer pipe encapsulation cobalt nano-particle under pH value 0-15 electrolyte as the catalyst of evolving hydrogen reaction, and under pH value 13-15 alkali condition, it is also possible to as the catalyst of oxygen evolution reaction.
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| CN107051568A (en) * | 2017-05-08 | 2017-08-18 | 中南大学 | One kind analysis oxygen Fe two cobaltous selenide@N CT composite catalysts of doping and its preparation method and application |
| CN108666584A (en) * | 2018-04-13 | 2018-10-16 | 东莞理工学院 | A kind of Co-N-C/ carbon nano-tube catalysts and its preparation method and application |
| CN108923051A (en) * | 2018-07-06 | 2018-11-30 | 郑州大学 | A kind of nitrogen-doped carbon nanometer pipe composite catalyst of package metals cobalt nano-particle and its application |
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