CN106745525A - Metallic composite, its preparation method and application - Google Patents
Metallic composite, its preparation method and application Download PDFInfo
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- CN106745525A CN106745525A CN201611088920.9A CN201611088920A CN106745525A CN 106745525 A CN106745525 A CN 106745525A CN 201611088920 A CN201611088920 A CN 201611088920A CN 106745525 A CN106745525 A CN 106745525A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
- C02F1/4672—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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Abstract
The invention provides a kind of metallic composite, its preparation method and application, the metallic composite includes：Three-dimensional carrier；With the composite oxide of metal being supported on three-dimensional carrier；The composite oxide of metal is formed by the nickel molybdenum oxide calcined in protective gas high temperature.Compared with prior art, the metallic composite that the present invention is provided has catalysis activity higher as water oxygen and urea oxidation catalyst.
Description
Technical field
The invention belongs to electrode material technical field, more particularly to a kind of metallic composite, its preparation method and application.
Background technology
At present, for developing country, fuel cell is no longer a kind of new technology, and it is that the whole world realizes that low-carbon (LC) is passed through
The significant opportunity of Ji body.Fuel cell be it is a kind of can by add fuel it is lasting chemical energy is switched to the high effect cleaning of electric energy
TRT.China provides electric power very dependent on coal fire power plant, and electric power has 80% from non-renewable energy resources coal, and 19% comes from
Hydroelectric generation, this structure causes China as the big country of world's CO2 emission first.Meanwhile, Chinese population has 1,300,000,000 to occupy generation
, also there are many carbon emission amounts on boundary first in other manufactures and family field, therefore, these factors all make China or even the whole world
Very big challenge is faced in energy supply and secure side.Global every country has been carried out and has been implemented to solve these problems
Regenerative resource strategy, wherein fuel cell are selections that is most potential and being expected to all-round market, while electric power more than needed can
First hydrogen manufacturing, is subsequently used for fuel cell car, is a kind of high-quality scheme of propulsion low carbon development.Therefore, fuel cell just with " by
Point is to face " mode gradually develop realization commercialization in different areas, the project of current fuel cell is generating electricity
Developed rapidly and approved with power network support, communications and transportation, cogeneration of heat and power and stand-by power supply and long-range generating, wherein,
The constructed fuel cell power plant the biggest in the world of South Korea, generated output is up to 11.2MW；The U.S. has deployed and has exceeded
1350 sets of back-up source fuel cells；Automaker (benz, modern times, Toyota, Honda, Ford, Nissan and logical all over the world
With) have begun to promote the commercialization of fuel cell electric vehicle (FCEVs).
Hydrogen fuel cell due to the mass energy density high and almost advantage such as zero carbon emission, as current fuel
The focus and emphasis of battery research.The hydrogen production process of wherein more environmental protection is exactly water electrolysis hydrogen production gas.Water electrolysis hydrogen production is anti-
Oxygen evolution reaction and the hydrogen evolution reaction of negative electrode of anode should be divided into.Due to the presence of anode and catholyte overpotential,
The decomposition voltage of 1.23V generally needs the voltage of 2V or so could to obtain hydrogen, relatively low electric energy hydrogen energy conversion efficiency in theory
Result in hydrogen manufacturing cost higher.It is respectively ruthenium/iridium base and platinum that oxygen evolution best so far and hydrogen separate out catalyst
Noble metal catalyst, but its cost very high limits large-scale application.Therefore, the product hydrogen of Cheap highly effective is developed
Producing VPO catalysts turns into a research with innovative significance, is also the reduction of hydrogen fuel cell cost and promotes its alive
It is able to, extensively using essential condition, ensure that it can obtain great business success in future with this in the range of boundary.
The content of the invention
In view of this, the technical problem to be solved in the present invention be provide a kind of metallic composite, its preparation method and
Using the metallic composite has activity higher as water oxygen and urea oxidation reaction catalyst.
The invention provides a kind of metallic composite, including：
Three-dimensional carrier；
With the composite oxide of metal being supported on three-dimensional carrier；The composite oxide of metal is by high in protective gas
The nickel molybdenum oxide of temperature calcining is formed.
Preferably, the three-dimensional carrier is one or more in nickel foam, carbon cloth and foam copper.
Preferably, the mass fraction of nickel is 25%~40% in the metallic composite；The mass fraction of molybdenum is 45%
~60%；The mass fraction of oxygen is 0~30%.
Preferably, the composite oxide of metal is monodimension nano stick array.
Preferably, a diameter of 40~80nm of the composite oxide of metal；The draw ratio of the metallic composite is
(10~80)：1.
Preferably, the temperature of the high-temperature calcination is 200 DEG C~600 DEG C；The time of high-temperature calcination is 1~3h.
Present invention also offers a kind of preparation method of metallic composite, including：
S1) nickel source compound, molybdenum source compound are mixed with three-dimensional carrier in water, heating response obtains nickel-loaded molybdenum
The three-dimensional carrier of oxide；
S2) three-dimensional carrier of the nickel-loaded molybdenum oxide is calcined in protective gas high temperature, Metals composite is obtained
Material.
Preferably, the step S1) in heating response temperature be 120 DEG C~180 DEG C；The time of heating response be 4~
12h。
Present invention also offers above-mentioned metallic composite as anode material application.
Present invention also offers above-mentioned metallic composite as anode electrocatalyst application.
The invention provides a kind of metallic composite, its preparation method and application, the metallic composite includes：It is three-dimensional
Carrier；With the composite oxide of metal being supported on three-dimensional carrier；The composite oxide of metal is by protective gas high temperature
The nickel molybdenum oxide of calcining is formed.Compared with prior art, the metallic composite that the present invention is provided is used as water oxygen and urea
Oxidation catalyst has catalysis activity higher.
Test result indicate that, the present invention prepare metallic composite as oxygen evolution catalysts, in urea oxygen
Change in reaction, when current potential is 1.42V, its current density can reach 100mA/cm2；In the all-hydrolytic reaction of urea auxiliary, electricity
When position is for 1.55V, its current density can reach 100mA/cm2。
Brief description of the drawings
Fig. 1 is the stereoscan photograph of metallic composite obtained in the embodiment of the present invention 1；
Fig. 2 is the transmission electron microscope photo of metallic composite obtained in the embodiment of the present invention 1；
Fig. 3 is the XRD curve maps of metallic composite obtained in the embodiment of the present invention 1；
Fig. 4 is the stereoscan photograph of metallic composite obtained in the embodiment of the present invention 2；
Fig. 5 is the stereoscan photograph of metallic composite obtained in the embodiment of the present invention 3；
Fig. 6 is the stereoscan photograph of metallic composite obtained in the embodiment of the present invention 4；
Fig. 7 is aoxidized as elctro-catalyst for the metallic composite obtained in the embodiment of the present invention 1 in water oxygen and urea
The linear sweep voltammetry experiment curv figure of reaction.
Specific embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Based in the present invention
Embodiment, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made, all
Belong to the scope of protection of the invention.
The invention provides a kind of metallic composite, including：
Three-dimensional carrier；
With the composite oxide of metal being supported on three-dimensional carrier；The composite oxide of metal is by high in protective gas
The nickel molybdenum oxide of temperature calcining is formed；
Wherein, the three-dimensional carrier is three-dimensional carrier well known to those skilled in the art, has no special limitation, this
One or more in nickel foam, carbon cloth and foam copper, more preferably nickel foam are preferably in invention.
Composite oxide of metal is loaded with the three-dimensional carrier；The composite oxide of metal is by high in protective gas
The nickel molybdenum oxide of temperature calcining is formed；Wherein, the protective gas is protective gas well known to those skilled in the art, and
Without special limitation, argon gas is preferably in the present invention；The temperature of the high-temperature calcination is preferably 200 DEG C~600 DEG C, more preferably
300 DEG C~600 DEG C, be further preferably 300 DEG C~500 DEG C, is further preferably 350 DEG C~450 DEG C, most preferably 400 DEG C；The high temperature
The time of calcining is preferably 1~3h, more preferably 2~3h, is further preferably 2h；The composite oxide of metal is preferably a wiener
Rice rod array, the i.e. structure of the metallic composite that the present invention is provided support monodimension nano stick array for three-dimensional substrates；Described one
Preferably there is nanoscale duct in the nanometer rods for tieing up nanometer stick array；The diameter of the composite oxide of metal is preferably 40~
80nm；The draw ratio of the metal oxide complex is preferably (10~80)：1.
The mass fraction of nickel is preferably 25%~40% in the metallic composite that the present invention is provided, more preferably 25%~
30%；The mass fraction of molybdenum is preferably 45%~60%, more preferably 45%~50%；The mass fraction of the oxygen is preferably 0
~30%.
The metallic composite that the present invention is provided has catalysis activity higher as water oxygenization and urea oxidation catalyst.
Present invention also offers a kind of preparation method of above-mentioned metallic composite, including：S1) by nickel source compound, molybdenum
Source compound mixes with three-dimensional carrier in water, heating response, obtains the three-dimensional carrier of nickel-loaded molybdenum oxide；S2) will be described
The three-dimensional carrier of nickel-loaded molybdenum oxide is calcined in protective gas high temperature, obtains metallic composite.
The present invention is not particularly limited to the source of all raw materials, is commercially available.
The nickel source compound is soluble nickel source compound well known to those skilled in the art, has no special limit
System, is preferably nickel nitrate in the present invention；The molybdenum source compound is soluble molybdenum source compound well known to those skilled in the art
, special limitation is had no, sodium molybdate is preferably in the present invention；The nickel source compound is excellent with the mol ratio of molybdenum source compound
Elect 1 as：(1~1.2), more preferably 1：1.
The three-dimensional carrier is three-dimensional carrier well known to those skilled in the art, has no special limitation, the present invention
In be preferably nickel foam, carbon cloth and foam copper in one or more.In the present invention, the three-dimensional carrier preferably carries out pre- place
Mix with nickel source compound and molybdenum source compound again after reason, the method for the pretreatment is method well known to those skilled in the art
, have no special limitation.
When three-dimensional carrier is nickel foam and foam copper, preferably follow the steps below：Nickel foam or foam copper are soaked
Steep in organic solvent, remove surface and oil contaminant；The organic solvent is organic solvent well known to those skilled in the art, and
Without special limitation, acetone is preferably in the present invention；The time of the immersion is preferably 1~2h；Used again after organic solvent immersion
Water is cleaned, and is then soaked in nickel oxide or cupric oxide that 15~30min in 1~6mol/L hydrochloric acid removes surface, finally spend from
Sub- water is cleaned with ethanol, after drying, obtains pretreated nickel foam or foam copper；The drying is preferably vacuum drying；Institute
State dry temperature and be preferably 50 DEG C~80 DEG C；The dry time is preferably 4~24h.
When three-dimensional carrier is carbon cloth, pretreatment is preferably followed the steps below：Carbon cloth is soaked in organic solvent,
Remove surface and oil contaminant；The organic solvent is organic solvent well known to those skilled in the art, has no special limitation, this
Acetone is preferably in invention；The time of the immersion is preferably 1~2h；Cleaned with water and ethanol again after organic solvent immersion, done
After dry, pretreated carbon cloth is obtained；The drying is preferably vacuum drying；The dry temperature is preferably 50 DEG C~80
℃；The dry time is preferably 4~24h.
Nickel source compound, molybdenum source compound are mixed with three-dimensional carrier in water, preferably first by nickel source compound and molybdenum source
Compound mixes in water, is preferably uniformly mixed on magnetic stirring apparatus, the mixed solution clarified, then again by three
In dimension carrier immersion mixed solution；Wherein described nickel source compound, molybdenum source compound and ratio is preferably (1~4) mol in water：
(1~4) mol：35ml.
Then heating response；The temperature of the heating response is preferably 120 DEG C~180 DEG C, more preferably 130 DEG C~160
DEG C, more preferably 150 DEG C；The time of the heating response is preferably 4~12h, more preferably 6~10h.After reaction terminates, obtain
It is the product of yellow to surface.
After reaction, preferably product is washed, the three-dimensional carrier of nickel-loaded molybdenum oxide is obtained after drying；The drying
Preferably it is vacuum dried；The dry temperature is preferably 50 DEG C~100 DEG C, more preferably 60 DEG C~90 DEG C；It is described dry
Time is preferably 12~15h.
The three-dimensional carrier of the nickel-loaded molybdenum oxide is calcined in protective gas high temperature, metallic composite is obtained；
The protective gas is that special limitation is had no by protective gas well known to those skilled in the art, and argon is preferably in the present invention
Gas；The temperature of the high-temperature calcination is preferably 300 DEG C~600 DEG C, more preferably 300 DEG C~500 DEG C, further preferably for 350 DEG C~
450 DEG C, most preferably 400 DEG C；The time of the high-temperature calcination is preferably 1~3h, more preferably 2~3h, is further preferably 2h.
Preparation method of the present invention is simple, and cost is relatively low, is suitable to large-scale industrialization promotion.
Present invention also offers a kind of above-mentioned metallic composite as anode material application.
Present invention also offers a kind of above-mentioned metallic composite as anode electrocatalyst application, preferably oxygen analysis
Go out catalyst, more preferably water oxygen and urea oxidation reaction catalyst.
In order to further illustrate the present invention, with reference to embodiments to the present invention provide a kind of metallic composite, its
Preparation method and application is described in detail.
Reagent used is commercially available in following examples.
Embodiment 1
The pretreatment of 1.1 nickel foams：Commercial foam nickel is immersed in 2 hours in acetone, then is washed with deionized, removed
Acetone, then, gained nickel foam is immersed in 20 minutes in 3mol/L hydrochloric acid, rinsed repeatedly with deionized water after taking-up ten times with
On, then with alcohol flushing 1~3 time, then gained nickel foam is put into 60 DEG C of vacuum drying chambers dries 12h.
1.2 hydrothermal growth process grow NiMoO in foam nickel skeleton4Nanometer stick array：By 2mmol Ni (NO3)2·6H2O and
2mmol Na2MoO4·2H2O is dissolved in 17.5ml deionized waters respectively, stirring fully dissolving, by above-mentioned Na2MoO4Solution adds
Enter to being added to Ni (NO3)2In solution, stir 10 minutes, form homogeneous solution；The mixed solution solution is transferred to 50ml anti-
Answer in kettle, add the nickel foam (about 2 × 4cm obtained in cut 1.12), it is inclined by a reservoir and complete by solution
Full submergence, puts into 150 DEG C of baking ovens, reacts 6h；Deionized water and ethanol cyclic washing are used after taking out foam nickel base, removes table
The powder of face attachment, obtains being loaded with the nickel foam of nickel molybdenum oxide.
1.3 nickel foams for being loaded with nickel molybdenum oxide that will be obtained in 1.2 obtain metal composite in the calcining of argon gas high temperature
Material, calcining heat is 400 DEG C, and calcination time is 2h.
The metallic composite obtained in embodiment 1 is analyzed using SEM, obtains its scanning electricity
Mirror photo is as shown in Figure 1.As seen from Figure 1, metallic composite maintains the nickel molybdenum oxidation of three-dimensional foam nickel surface growth
The one-dimentional structure of thing nanometer rods.
The metallic composite obtained in embodiment 1 is analyzed using transmission electron microscope, obtains its transmission electricity
Mirror photo is as shown in Figure 2.Figure it is seen that the NiMoO of dehydration4Nanorod surfaces occur than more uniform without particle.
The metallic composite obtained in embodiment 1 is analyzed using X-ray diffraction, obtains its XRD curve map, such as
Shown in Fig. 3.Metals composite material prepared as can be seen from Figure 3 and pure NiMoO4JCPDS cards be consistent.
Embodiment 2
Embodiment 1 is repeated, there is following difference：High-temperature calcination temperature in step 1.3 is changed to 200 DEG C, obtains metal and answers
Condensation material.
The metallic composite obtained in embodiment 2 is analyzed using SEM, obtains its scanning electricity
Mirror photo is as shown in Figure 4.As seen from Figure 4, metallic composite maintains the nickel molybdenum oxidation of three-dimensional foam nickel surface growth
The one-dimentional structure of thing nanometer rods, pattern is than more uniform.
Embodiment 3
Embodiment 1 is repeated, there is following difference：High-temperature calcination temperature in step 1.3 is changed to 300 DEG C, obtains metal and answers
Condensation material.
The metallic composite obtained in embodiment 3 is analyzed using SEM, obtains its scanning electricity
Mirror photo is as shown in Figure 5.As seen from Figure 5, metallic composite maintains the nickel molybdenum oxidation of three-dimensional foam nickel surface growth
The one-dimentional structure of thing nanometer rods.
Embodiment 4
Embodiment 1 is repeated, there is following difference：High-temperature calcination temperature in step 1.3 is changed to 500 DEG C, obtains metal and answers
Condensation material.
The metallic composite obtained in embodiment 4 is analyzed using SEM, obtains its scanning electricity
Mirror photo is as shown in Figure 6.As seen from Figure 6, metallic composite maintains the nickel molybdenum oxidation of three-dimensional foam nickel surface growth
The one-dimentional structure of thing nanometer rods, high temperature does not destroy its one-dimensional pattern.
To the metallic composite that is obtained by embodiment 1 as elctro-catalyst in water oxygen and the electricity of urea oxidation reaction
Catalytic performance is measured, linear sweep voltammetry experiment curv as a result shown in Figure 7.From figure 7 it can be seen that implementing
The metallic composite obtained in example 1 has preferable water oxygen and urea oxidizing property, wherein in water oxidation reaction, it is necessary to
1.52V, 1.62V, 1.68V reach 10mA/cm2、100mA/cm2、250mA/cm2Current density；In urea oxidation reaction,
The voltage that it needs only to 1.37V, 1.42V, 1.50V can just reach 10mA/cm2、100mA/cm2、250mA/cm2Electric current it is close
Degree.
Claims (10)
1. a kind of metallic composite, it is characterised in that including：
Three-dimensional carrier；
With the composite oxide of metal being supported on three-dimensional carrier；The composite oxide of metal is forged by protective gas high temperature
The nickel molybdenum oxide of burning is formed.
2. metallic composite according to claim 1, it is characterised in that the three-dimensional carrier be nickel foam, carbon cloth with
One or more in foam copper.
3. metallic composite according to claim 1, it is characterised in that the quality of nickel point in the metallic composite
Number is 25%~40%；The mass fraction of molybdenum is 45%~60%；The mass fraction of oxygen is 0~30%.
4. metallic composite according to claim 1, it is characterised in that the composite oxide of metal is 1-dimention nano
Rod array.
5. metallic composite according to claim 4, it is characterised in that a diameter of the 40 of the composite oxide of metal
~80nm；The draw ratio of the metallic composite is (10~80)：1.
6. metallic composite according to claim 1, it is characterised in that the temperature of the high-temperature calcination is 200 DEG C~
600℃；The time of high-temperature calcination is 1~3h.
7. a kind of preparation method of metallic composite, it is characterised in that including：
S1) nickel source compound, molybdenum source compound are mixed with three-dimensional carrier in water, heating response, obtains the oxidation of nickel-loaded molybdenum
The three-dimensional carrier of thing；
S2) three-dimensional carrier of the nickel-loaded molybdenum oxide is calcined in protective gas high temperature, metallic composite is obtained.
8. preparation method according to claim 7, it is characterised in that the step S1) in the temperature of heating response be 120
DEG C~180 DEG C；The time of heating response is 4~12h.
9. the gold prepared by metallic composite described in claim 1~6 any one or claim 7~8 any one
Belong to application of the composite as anode material.
10. the gold prepared by metallic composite described in claim 1~6 any one or claim 7~8 any one
Belong to application of the composite as anode electrocatalyst.
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| CN107611453A (en) * | 2017-08-22 | 2018-01-19 | 哈尔滨工程大学 | Foamed nickel supported NiMoO for direct urea fuel cell4The preparation method of@C micron bar anode-array |
| CN108033518A (en) * | 2017-11-27 | 2018-05-15 | 山西大学 | A kind of method and apparatus for chloride urea in swimming pool water of degrading |
| CN110783574A (en) * | 2019-11-05 | 2020-02-11 | 江苏大学 | Direct alcohol fuel cell gas diffusion electrode and preparation method thereof and direct alcohol fuel cell |
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| CN108033518A (en) * | 2017-11-27 | 2018-05-15 | 山西大学 | A kind of method and apparatus for chloride urea in swimming pool water of degrading |
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| CN110783574A (en) * | 2019-11-05 | 2020-02-11 | 江苏大学 | Direct alcohol fuel cell gas diffusion electrode and preparation method thereof and direct alcohol fuel cell |
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| Publication number | Publication date |
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| CN106745525B (en) | 2020-04-24 |
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