CN109351359A - It is a kind of using carbon nanotube as the preparation method of the more metal carbides of Material synthesis - Google Patents

It is a kind of using carbon nanotube as the preparation method of the more metal carbides of Material synthesis Download PDF

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CN109351359A
CN109351359A CN201811214556.5A CN201811214556A CN109351359A CN 109351359 A CN109351359 A CN 109351359A CN 201811214556 A CN201811214556 A CN 201811214556A CN 109351359 A CN109351359 A CN 109351359A
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metal
carbon nanotube
metal carbides
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room temperature
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高爽
常立民
王海瑞
聂平
赵翠梅
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Jilin Normal University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/85—Chromium, molybdenum or tungsten
    • B01J23/88—Molybdenum
    • B01J23/882—Molybdenum and cobalt
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/85—Chromium, molybdenum or tungsten
    • B01J23/88—Molybdenum
    • B01J23/883—Molybdenum and nickel
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/85—Chromium, molybdenum or tungsten
    • B01J23/888—Tungsten

Abstract

The present invention discloses a kind of using carbon nanotube as the preparation method of more metal carbides of Material synthesis, belongs to technical field of material；It is complex for existing preparation method and be only applicable to prepare a kind of more metal carbides of problem, the present invention is using carbon nanotube as carbon source, it is uniformly mixed with metal salt M (M=Fe, Co, Ni) and ammonium molybdate or ammonium tungstate, then by under tube furnace, inert atmosphere calcining, ultimately forms more metal carbides；The preparation method is easy to operate, at low cost, reproducible, has universality, can prepare a series of more metal carbides, mainly includes bimetallic carbide Co3Mo3C、Ni3Mo3C、Fe3Mo3C、Co6W6C、Ni6W6C and Fe6W6Three metal carbides Co of C and three metal carbidesxFe3‑xMo3C、CoxNi3‑xMo3C、NixFe3‑xMo3C、CoxFe6‑xW6C、NixFe6‑ xW6C and CoxNi6‑xW6C, and obtained more metal carbides have excellent electrocatalytic hydrogen evolution performance.

Description

It is a kind of using carbon nanotube as the preparation method of the more metal carbides of Material synthesis
Technical field
The invention belongs to material preparation technology and application fields, and in particular to a kind of how golden as Material synthesis using carbon nanotube Belong to the preparation method of carbide.
Background technique
Transition metal carbide is due to its unique physicochemical property: such as strong electric conductivity, chemical stability, high-melting-point and by The extensive concern of people.Especially in terms of the energy, such as lithium ion battery, supercapacitor, electro-catalysis water-splitting etc., gold Belong to carbide all to have excellent catalytic properties.Compared to monometallic carbide, bimetallic carbide contains gold due to itself Category-metallic bond, can reinforcing material electric conductivity.Meanwhile the synergistic effect between metal is more advantageous to regulation catalyst itself Electronic structure improves the catalytic activity of material.
Traditional bimetallic carbide synthetic method has arc melting process.Higher temperature is needed using the method, to setting It is standby to require harsh, consumption energy height.Another method is temperature-programmed reduction method, needs to be passed through using this method carbon containing organic Gas is usually contained miscellaneous as carbon source using the bimetallic carbide that the method synthesizes, and experimental repeatability is poor.In recent years Come, Zou et al. is prepared for carbon-coated cobalt tungsten bimetallic by raw material of dicyandiamide in Nanoscale, 2015,7,3130-3136 Carbide, the material can be used as efficient liberation of hydrogen catalyst.Ma et al. is in J.Am.Chem.Soc., 2012,134,1954-1957 It reports using ion exchange resin as precursor preparation bimetallic carbide Co6Mo6C2.These methods are only applicable to single The preparation of bimetallic carbide does not have universality.
Summary of the invention
For the deficiency of above-mentioned synthetic method, the present invention proposes a kind of using carbon nanotube as more metallic carbides of Material synthesis The preparation method of object.The synthetic method has universality, available bimetallic carbide Co3Mo3C、Ni3Mo3C、Fe3Mo3C、 Co6W6C、Ni6W6C and Fe6W6C and three metal carbides CoxFe3-xMo3C (0 < x < 3), CoxNi3-xMo3C (0 < x < 3), NixFe3-xMo3C (0 < x < 3), CoxFe6-xW6C (0 < x < 6), NixFe6-xW6C (0 < x < 6) and CoxNi6-xW6C (0 < x < 6).These more metal carbides are micron grade blocky particle, and size is 0.5-1 μm.And these materials all have electricity Catalytic hydrogen evolution performance, wherein Co3Mo3C is most outstanding, current density 10mA/cm2When overpotential be 169mV.
It is a kind of using carbon nanotube as the preparation method of the more metal carbides of Material synthesis, its step are as follows:
(1), metal salt M, ammonium molybdate or ammonium tungstate, carbon nanotube are placed in mortar and are uniformly mixed；Metal salt M receives with carbon The molar ratio of mitron is 1:(10~20), metal salt M is (5:1)~(1:5) with the molar ratio of ammonium molybdate or ammonium tungstate.
(2), the sample in step (1) is placed in tube furnace, under inert atmosphere protection, with the heating rate of 3 DEG C/min 700~1100 DEG C are risen to by room temperature, and calcines 3h in maximum temperature；
(3), it is down to room temperature after calcining, resulting sample is more metal carbides.
Metal salt M is metal M nitrate, metal ions M Fe3+、Co2+And Ni2+In 1 or 2 kind.
Preferably, the molar ratio of metal salt M and carbon nanotube is 1:18；Mole of metal salt M and ammonium molybdate or ammonium tungstate Than for 1:1.
The invention has the following advantages that
1. this method has low operation temperature, and equipment requirement is simple compared with traditional synthetic method, and has pervasive Property.
2. being pure phase using more metal carbides that the method obtains, impurity is not contained, size is micron grade blocky Particle.
3. these materials in electrocatalytic hydrogen evolution performance test, all have good catalytic activity and good stability.
Detailed description of the invention
The XRD spectra of molybdenum base bimetallic carbide obtained in Fig. 1 embodiment 1, embodiment 2 and embodiment 3；
The XRD spectra of tungsten bimetallic carbide obtained in Fig. 2 embodiment 4, embodiment 5 and embodiment 6；
The three metal carbides Co obtained of Fig. 3 embodiment 7xFe3-xMo3The XRD spectra of C；
The three metal carbides Co obtained of Fig. 4 embodiment 8xFe6-xW6The XRD spectra of C
Specific embodiment
The invention will be further described by way of example and in conjunction with the accompanying drawings, but protection scope of the present invention is not limited to Following embodiments.
Embodiment 1
38mg ammonium molybdate, 62mg cobalt nitrate and 13mg carbon nanotube are uniformly mixed, gained mixture is put into quartz ampoule, Inert atmosphere N2Under protection, 950 DEG C (heating rate is 3 DEG C/min) are risen to by room temperature, 3h is calcined, is cooled to room temperature.It is acquired Grey powder be cobalt molybdenum bimetallic carbide Co3Mo3C.The material is subjected to electrocatalytic hydrogen evolution performance under the conditions of 1M KOH Test, reaches 10mA cm-2When, need overpotential 169mV.
Embodiment 2
38mg ammonium molybdate, 62mg nickel nitrate and 13mg carbon nanotube are uniformly mixed, gained mixture is put into quartz ampoule, Inert atmosphere N2Under protection, 950 DEG C (heating rate is 3 DEG C/min) are risen to by room temperature, 3h is calcined, is cooled to room temperature.It is acquired Grey powder be nickel molybdenum bimetallic carbide Ni3Mo3C.The material is subjected to electrocatalytic hydrogen evolution performance under the conditions of 1M KOH Test, reaches 10mA cm-2When, need overpotential 217mV.
Embodiment 3
31mg ammonium molybdate, 69mg ferric nitrate and 13mg carbon nanotube are uniformly mixed, gained mixture is put into quartz ampoule, Inert atmosphere N2Under protection, 950 DEG C (heating rate is 3 DEG C/min) are risen to by room temperature, 3h is calcined, is cooled to room temperature.It is acquired Grey powder be iron molybdenum bimetallic carbide Fe3Mo3C.The material is subjected to electrocatalytic hydrogen evolution performance under the conditions of 1M KOH Test, reaches 10mA cm-2When, need overpotential 302mV.
Embodiment 4
47mg ammonium tungstate, 53mg cobalt nitrate and 15mg carbon nanotube are uniformly mixed, gained mixture is put into quartz ampoule, Inert atmosphere N2Under protection, 950 DEG C (heating rate is 3 DEG C/min) are risen to by room temperature, 3h is calcined, is cooled to room temperature.It is acquired Grey powder be cobalt tungsten bimetallic carbide Co6W6C.The material is subjected to electrocatalytic hydrogen evolution performance under the conditions of 1M KOH Test, reaches 10mA cm-2When, need overpotential 227mV.
Embodiment 5
47mg ammonium tungstate, 53mg nickel nitrate and 13mg carbon nanotube are uniformly mixed, gained mixture is put into quartz ampoule, Inert atmosphere N2Under protection, 950 DEG C (heating rate is 3 DEG C/min) are risen to by room temperature, 3h is calcined, is cooled to room temperature.It is acquired Grey powder be nickel tungsten bimetallic carbide Ni6W6C.The material is subjected to electrocatalytic hydrogen evolution performance under the conditions of 1M KOH Test, reaches 10mA cm-2When, need overpotential 259mV.
Embodiment 6
39mg ammonium tungstate, 61mg ferric nitrate and 11mg carbon nanotube are uniformly mixed, gained mixture is put into quartz ampoule, Inert atmosphere N2Under protection, 950 DEG C (heating rate is 3 DEG C/min) are risen to by room temperature, 3h is calcined, is cooled to room temperature.It is acquired Grey powder be ferrotungsten bimetallic carbide Fe6W6C.The material is subjected to electrocatalytic hydrogen evolution performance under the conditions of 1M KOH Test, reaches 10mA cm-2When, need overpotential 347mV.
Embodiment 7
42mg ammonium tungstate, 24mg cobalt nitrate, 34mg ferric nitrate and 13mg carbon nanotube are uniformly mixed, by gained mixture It is put into quartz ampoule, inert atmosphere N2Under protection, 950 DEG C (heating rate is 3 DEG C/min) are risen to by room temperature, 3h is calcined, is cooled to Room temperature.Obtained grey powder is three metal carbides Co of ferro-cobalt tungstenxFe6-xW6C (x=3).By the material in 1M KOH item Electrocatalytic hydrogen evolution performance test is carried out under part, reaches 10mA cm-2When, need overpotential 274mV.
Embodiment 8
42mg ammonium tungstate, 24mg nickel nitrate, 34mg ferric nitrate and 14mg carbon nanotube are uniformly mixed, by gained mixture It is put into quartz ampoule, inert atmosphere N2Under protection, 950 DEG C (heating rate is 3 DEG C/min) are risen to by room temperature, 3h is calcined, is cooled to Room temperature.Obtained grey powder is three metal carbides Ni of ferronickel tungstenxFe6-xW6C (x=3).By the material in 1M KOH item Electrocatalytic hydrogen evolution performance test is carried out under part, reaches 10mA cm-2When, need overpotential 309mV.
Embodiment 9
47mg ammonium tungstate, 27mg nickel nitrate, 27mg cobalt nitrate and 13mg carbon nanotube are uniformly mixed, by gained mixture It is put into quartz ampoule, inert atmosphere N2Under protection, 950 DEG C (heating rate is 3 DEG C/min) are risen to by room temperature, 3h is calcined, is cooled to Room temperature.Obtained grey powder is three metal carbides Co of cobalt nickel tungstenxNi6-xW6C (x=3).By the material in 1M KOH item Electrocatalytic hydrogen evolution performance test is carried out under part, reaches 10mA cm-2When, need overpotential 327mV.
Embodiment 10
34mg ammonium molybdate, 28mg cobalt nitrate, 38mg ferric nitrate and 13mg carbon nanotube are uniformly mixed, by gained mixture It is put into quartz ampoule, inert atmosphere N2Under protection, 950 DEG C (heating rate is 3 DEG C/min) are risen to by room temperature, 3h is calcined, is cooled to Room temperature.Obtained grey powder is three metal carbides Co of ferro-cobalt molybdenumxFe3-xMo3C (x=1.5).By the material in 1M Electrocatalytic hydrogen evolution performance test is carried out under the conditions of KOH, reaches 10mA cm-2When, need overpotential 251mV.
Embodiment 11
34mg ammonium molybdate, 28mg nickel nitrate, 38mg ferric nitrate and 13mg carbon nanotube are uniformly mixed, by gained mixture It is put into quartz ampoule, inert atmosphere N2Under protection, 950 DEG C (heating rate is 3 DEG C/min) are risen to by room temperature, 3h is calcined, is cooled to Room temperature.Obtained grey powder is three metal carbides Ni of ferronickel molybdenumxFe3-xMo3C (x=1.5).By the material in 1M Electrocatalytic hydrogen evolution performance test is carried out under the conditions of KOH, reaches 10mA cm-2When, need overpotential 283mV.
Embodiment 12
38mg ammonium molybdate, 21mg nickel nitrate, 31mg cobalt nitrate and 13mg carbon nanotube are uniformly mixed, by gained mixture It is put into quartz ampoule, inert atmosphere N2Under protection, 950 DEG C (heating rate is 3 DEG C/min) are risen to by room temperature, 3h is calcined, is cooled to Room temperature.Obtained grey powder is three metal carbides Co of cobalt nickel molybdenumxNi3-xMo3C (x=1.5).By the material in 1M Electrocatalytic hydrogen evolution performance test is carried out under the conditions of KOH, reaches 10mA cm-2When, need overpotential 308mV.
Embodiment 13
38mg ammonium molybdate, 62mg cobalt nitrate and 13mg carbon nanotube are uniformly mixed, gained mixture is put into quartz ampoule, Inert atmosphere N2Under protection, 1050 DEG C (heating rate is 3 DEG C/min) are risen to by room temperature, 3h is calcined, is cooled to room temperature.It is acquired Grey powder be cobalt molybdenum bimetallic carbide Co3Mo3C.The material is subjected to electrocatalytic hydrogen evolution performance under the conditions of 1M KOH Test, reaches 10mA cm-2When, need overpotential 213mV.
Embodiment 14
38mg ammonium molybdate, 62mg cobalt nitrate and 13mg carbon nanotube are uniformly mixed, gained mixture is put into quartz ampoule, Inert atmosphere N2Under protection, 850 DEG C (heating rate is 3 DEG C/min) are risen to by room temperature, 3h is calcined, is cooled to room temperature.It is acquired Grey powder be cobalt molybdenum bimetallic carbide Co3Mo3C.The material is subjected to electrocatalytic hydrogen evolution performance under the conditions of 1M KOH Test, reaches 10mA cm-2When, need overpotential 183mV.
Embodiment 15
38mg ammonium molybdate, 62mg cobalt nitrate and 13mg carbon nanotube are uniformly mixed, gained mixture is put into quartz ampoule, Inert atmosphere N2Under protection, 750 DEG C (heating rate is 3 DEG C/min) are risen to by room temperature, 3h is calcined, is cooled to room temperature.It is acquired Grey powder be cobalt molybdenum bimetallic carbide Co3Mo3C.The material is subjected to electrocatalytic hydrogen evolution performance under the conditions of 1M KOH Test, reaches 10mA cm-2When, need overpotential 200mV.
Above-described embodiment has been respectively synthesized bimetallic carbide Co3Mo3C、Ni3Mo3C、Fe3Mo3C、Co6W6C、Ni6W6C and Fe6W6C and three metal carbides CoxFe3-xMo3C、CoxNi3-xMo3C、NixFe3-xMo3C、CoxFe6-xW6C、NixFe6-xW6C and CoxNi6-xW6C。
1 XRD spectra is it is found that correspond respectively to standard using molybdenum base bimetallic carbide prepared by this method with reference to the accompanying drawings Card M3Mo3C-structure, i.e. Co3Mo3C、Ni3Mo3C、Fe3Mo3C, and be free of any miscellaneous phase.The XRD spectra of attached drawing 2 shows to adopt Standard card M is corresponded respectively to tungsten bimetallic carbide prepared by this method6W6C-structure, i.e. Co6W6C、Ni6W6C and Fe6W6C, and be free of any miscellaneous phase.Attached drawing 3 is the XRD spectra of three metal carbides of molybdenum base, as seen from the figure, the XRD of the material Spectrogram is located at Co3Mo3C and Fe3Mo3The centre of C shows that the material both contains Co3Mo3C-structure, and contain Fe3Mo3C-structure, because This, it is concluded that it is CoxFe3-xMo3C (0 < x < 3).Attached drawing 4 is the XRD spectra of three metal carbides of tungsten base, as seen from the figure, The XRD spectra of the material is located at Co6W6C and Fe6W6The centre of C shows that the material both contains Co6W6C-structure, and contain Fe6W6C Structure, therefore, it is concluded that it is CoxFe6-xW6C (0 < x < 6).

Claims (4)

1. a kind of using carbon nanotube as the preparation method of the more metal carbides of Material synthesis, its step are as follows:
1), metal M salt, ammonium molybdate or ammonium tungstate, carbon nanotube are placed in mortar and uniformly mixed；Metal salt M and carbon nanotube Molar ratio be 1:(10~20), the molar ratio of metal M salt and ammonium molybdate or ammonium tungstate is (5:1)~(1:5).
2), the sample in step 1) is placed in tube furnace, under inert atmosphere protection, with the heating rate of 3 DEG C/min by room temperature 700~1100 DEG C are risen to, and calcines 3h in maximum temperature；
3) it is down to room temperature after, calcining, resulting sample is more metal carbides；Wherein, the metal ions M in metal M salt is Fe3+、Co2+And Ni2+In 1 or 2 kind；More metal carbides are Co3Mo3C、Ni3Mo3C、Fe3Mo3C、Co6W6C、 Ni6W6C、Fe6W6C、CoxFe3-xMo3C (0 < x < 3), CoxNi3-xMo3C (0 < x < 3), NixFe3-xMo3C (0 < x < 3), CoxFe6-xW6C (0 < x < 6), NixFe6-xW6C (0 < x < 6) or CoxNi6-xW6C (0 < x < 6).
2. according to claim 1 using carbon nanotube as the preparation method of the more metal carbides of Material synthesis, feature exists In the metal M salt is the nitrate of metal ions M.
3. according to claim 1 using carbon nanotube as the preparation method of the more metal carbides of Material synthesis, feature exists In the molar ratio of metal salt M and carbon nanotube is 1:18.
4. according to claim 1 using carbon nanotube as the preparation method of the more metal carbides of Material synthesis, feature exists In metal M salt is 1:1 with the molar ratio of ammonium molybdate or ammonium tungstate.
CN201811214556.5A 2018-10-18 2018-10-18 It is a kind of using carbon nanotube as the preparation method of the more metal carbides of Material synthesis Pending CN109351359A (en)

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