CN105406032B - The preparation method and applications of hydrogen bearing alloy and nanoporous nickel composite material (HSAs/NPNi) - Google Patents
The preparation method and applications of hydrogen bearing alloy and nanoporous nickel composite material (HSAs/NPNi) Download PDFInfo
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- CN105406032B CN105406032B CN201510996773.4A CN201510996773A CN105406032B CN 105406032 B CN105406032 B CN 105406032B CN 201510996773 A CN201510996773 A CN 201510996773A CN 105406032 B CN105406032 B CN 105406032B
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/24—Electrodes for alkaline accumulators
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/24—Electrodes for alkaline accumulators
- H01M4/242—Hydrogen storage electrodes
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- H—ELECTRICITY
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- H—ELECTRICITY
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Abstract
The present invention relates to a kind of AB5Application of the type hydrogen storage alloy (HSAs) with the preparation method of nanoporous nickel (NPNi) composite (HSAs/NPNi) and its as nickel-hydrogen battery negative pole material.HSAs/NPNi composites are prepared for by such a simple method of hydro-thermal method and subsequent annealing.Specific preparation process is as follows：A, under argon gas protective condition, by arc melting rare earth element and other metallic elements, its ingot casting is obtained；B, ingot casting is annealed under argon atmosphere and mechanical lapping obtains alloy powder, its average particulate diameter is 50 μm；C, Ni (OH) is prepared with simple hydrothermal method2Powder；D, by prepared Ni (OH)2Integrate, mixture is dried in electric dry oven, then in tube furnace Ar/H with HSAs2Annealing makes Ni (OH) in gaseous mixture atmosphere2Reduction, prepare HSAs/NPNi composites.The composite has excellent high-rate discharge ability as the negative material of Ni-MH battery, is 3000mAg in discharge current density‑1When, its capacity retention rate is up to 43.11%, is 3.2 times of independent hydrogen-bearing alloy electrode.
Description
Technical field：
Application the present invention relates to the preparation of HSAs/NPNi composites and its as nickel-hydrogen battery negative pole material.
Background technology：
In recent years, as environmental problem is increasingly serious, the continuous aggravation of energy crisis, new-energy automobile receives increasingly
More concerns.Electric automobile (EV), mixed power electric car (HEV) and fuel cell electric vehicle (FCVs) are new energy vapour
The main body of car.And the key for developing EVs, HEVs and FCVs be exactly high efficiency, low cost, safety, environmentally friendly battery should
With.It is well known that good battery performance is to realize the key changed from the oil gas epoch to the electric power epoch.Some advanced batteries
Technology, such as nickel metal hydride (Ni/MH) battery, lithium ion battery and PEM (PEM) fuel cell etc., exist
Mobile electronic device, electric tool, electric automobile etc. are widely used.And Ni-MH battery due to its it is low into
Originally, long-life and excellent security and thermal adaptability are the first choices of Hybrid Vehicle battery.Above-mentioned application is to nickel
The requirement of hydrogen battery energy density is relatively low, and the requirement to power density is then very high.In addition, electric tool is existing with some
It is also very high for requirement of the military equipment to power density.Therefore, in order to meet the needs of market is to high-capacity nickel-hydrogen battery, enter
One step improves the competitiveness of Ni-MH battery, it is necessary to constantly improves the high-rate discharge ability (HRD) of hydrogen bearing alloy.
The content of the invention：
It is an object of the invention to provide a kind of preparation of HSAs/NPNi composites and its as nickel-hydrogen battery negative pole material
Application.It is related to a kind of AB5The preparation of type hydrogen storage alloy (HSAs) and nanoporous nickel (NPNi) composite (HSAs/NPNi)
Method and its application as nickel-hydrogen battery negative pole material.The invention is prepared by simple hydro-thermal method and subsequent annealing
HSAs/NPNi composites.The unique architectural characteristic of the composite makes it have faster electronics and ion transmission speed,
So as to substantially increase its high-rate discharge ability.
The above-mentioned purpose of the present invention is achieved through the following technical solutions, and particular content is as follows：
The preparation method of a kind of hydrogen bearing alloy and nanoporous nickel composite material (HSAs/NPNi), comprises the following steps：
A, in high-purity argon gas atmosphere by the lanthanum of method melting purity >=99.5 of electric arc melting, cerium, yttrium, nickel, cobalt,
Manganese, aluminium, obtain its ingot casting；
B, ingot casting is annealed under argon atmosphere and mechanical lapping obtains master alloy powder, its average particulate diameter is
50μm；
C, Ni (OH) is prepared with simple hydro-thermal method2Powder, by 1.4~1.5g Ni (NO3)2, 1.3~1.5g, six methylenes
The mixture of urotropine (HMT) and 30~40ml ultra-pure waters is added to the stainless steel autoclave with polytetrafluoroethyllining lining
In；The reactor of sealing is put into 10~12h of insulation in 100~120 DEG C of electric dry ovens, by green product Ni (OH)2Pass through centrifugation
Collect；
D, by prepared Ni (OH)2Grind in agate mortar with foundry alloy and uniformly integrated；By mixture in electricity
Dried in baking oven, then in tube furnace Ar/H25~6h is heat-treated in gaseous mixture atmosphere under the conditions of 400~450 DEG C, prepares HSAs/
NPNi composites.
The composition of ingot casting is not limited solely to AB in the step a5Or AB2, AB3Type hydrogen storage alloy.
Ni (OH) is prepared in the step c2When, Ni (NO3)2Can be the different quality of same ratio with HMT.
The Elevated Temperature Conditions of tube furnace are 1~3 DEG C/min in step d.
Described hydrogen bearing alloy and nanoporous nickel composite material (HSAs/NPNi), it carries out electrification as electrode material
Test is learned, is comprised the following steps：
A, first by 0.25~0.255g active materials, i.e. HSAs/NPNi composites or foundry alloy and 1.0~1.02g carbonyls
Base nickel powder is well mixed, then is pressed into a diameter of 10~15mm electrode slice under 8~20MPa pressure by tablet press machine, by electricity
Pole is immersed in 2~4h in 25~35wt% KOH solution, it is soaked completely before electro-chemical test；
B, electro-chemical test is carried out in the three-electrode system of a standard, and the electrode prepared in wherein step a is made
For working electrode, sintering Ni (OH)2/ NiOOH electrodes are used as to electrode, mercury/mercury oxide (Hg/HgO) electrode as reference electrode,
25~35wt% KOH solution is as electrolyte；
C, carrying out discharge capacity test as working electrode by the use of the HSAs/NPNi combination electrodes is surveyed in ARBIN batteries
Carried out on test system, under the conditions of 25 DEG C of room temperature, electrode is with 60mAg-1The current density charging 7.5h of (0.2C), stands
30min, then with 60mAg-1The current density of (0.2C) be discharged to blanking voltage reach relative to Hg/HgO reference electrodes-
0.74V, circulate 4 times and activated, reach maximum discharge capacity Cmax；
D, completely after activation, high-rate discharge ability test is carried out, electrode is with 300mAg-1The current density charging of (1C),
Then with 300,600,900,1200,1500,2400,3000mAg-1The current density of (10C) is discharged to blanking voltage respectively：-
0.65, -0.6, -0.5, -0.45, -0.4, -0.35, -0.3V, the blanking voltage are relative to Hg/HgO reference electrodes；
E, electrochemical property test is carried out on IVIUM electrochemical workstations.It is 5mV in the amplitude relative to OCP
Shi Jinhang ac impedance measurements, the frequency range of test is by 100kHz to 5mHz；Under the conditions of 50% depth of discharge, relative to
When OCP potential scan scope is -5 to 5mV, carry out sweeping linear polarisation curves test of the speed for 0.05mV/s；In 50% electric discharge
Under depth conditions, when being 0 to 1.5V relative to OCP potential scan scope, carry out sweeping the anodic polarization curves that speed is 5mV/s
Test；Under 100% charged state, under the potential step relative to Hg/HgO+500mV, carry out 4000s electric current-when
The test of half interval contour；
F, the hydrogen bearing alloy prepared and negative pole of the nanoporous nickel composite material (HSAs/NPNi) as Ni-MH battery, tool
There is excellent high-rate discharge ability.It is 3000mAg in discharge current density-1When, its capacity retention rate is up to 43.11%, is
3.2 times of independent foundry alloy electrode.
The solution have the advantages that：
Hydrogen bearing alloy produced by the present invention and nanoporous nickel composite material (HSAs/NPNi), due to being received in composite
The loose structure of the unique three-dimensional co-continuous of rice porous nickel, accelerates the transmission speed of electronics and ion, accelerates electrode surface
Electrochemical reaction rates and alloy inside hydrogen atom diffusion velocity, significantly improve its high-rate discharge ability.
Brief description of the drawings：
High-rate discharge ability curve under Fig. 1, different discharge current densities.
The optical photograph for preparing schematic diagram and electrode slice of Fig. 2, HSAs/NPNi composite, wherein：
A, the preparation method schematic diagram of HSAs/NPNi composites；
B, the optical photograph of use for electrochemical tests electrode slice.
Fig. 3, foundry alloy SEM photograph.
The SEM photograph of Fig. 4, HSAs/NPNi composite.
Fig. 5, NPNi SEM photograph.
Fig. 6, NPNi TEM photos.
Fig. 7, NPNi HRTEM photos.
Fig. 8, foundry alloy and HSAs/NPNi composites XRD diffracting spectrums.
Fig. 9, the linear polarisation curves under 50% depth of discharge.
Figure 10, the electrochemical impedance collection of illustrative plates under 50% depth of discharge.
Figure 11, the anodic polarization curves under 50% depth of discharge.
Discharge current-the time graph of Figure 12, anodic current density under 100% charged state.
Embodiment
Illustrate the embodiment of the present invention with reference to example：
Embodiment
Preparation process and step in the present embodiment is as follows：
(1) in high-purity argon gas atmosphere by the lanthanum of method melting purity >=99.5 of electric arc melting, cerium, yttrium, nickel, cobalt,
Manganese, aluminium, obtain its ingot casting；Ingot casting is annealed under argon atmosphere and mechanical lapping obtains the powder of foundry alloy, it is average
Particle diameter is 50 μm；Ni (OH) is prepared with simple hydrothermal method2Powder, by 1.45g Ni (NO3)2, six methylene of 1.4g
The mixture of tetramine (HMT) and 35ml ultra-pure waters is added in the stainless steel autoclave with polytetrafluoroethyllining lining.Will
The reactor of sealing is put into 100 DEG C of electric dry ovens and is incubated 10h, by green product Ni (OH)2By being collected by centrifugation；
(2) by prepared Ni (OH)2Grind in agate mortar with foundry alloy and uniformly integrated.By mixture in electricity
Dried in baking oven, then in tube furnace Ar/H25h is heat-treated in gaseous mixture atmosphere under the conditions of 400 DEG C, wherein Elevated Temperature Conditions are 1
DEG C/min, prepare HSAs/NPNi composites；
(3) 0.25g active materials, i.e. HSAs/NPNi composites or foundry alloy are well mixed with 1.0g carbonyl nickel powders,
It is pressed into a diameter of 15mm electrode slice under 8MPa pressure by tablet press machine again, electrode is immersed in 30wt% KOH solution
3h, it is set to be soaked completely before electro-chemical test；Using this electrode slice as working electrode, Ni (OH)2/ NiOOH pieces are used as to electricity
Pole, mercury/mercuric oxide electrode is as reference electrode, and 30wt% KOH solution is electrolyte, and the three-electrode system for forming standard is carried out
Electro-chemical test；
(4) it is in ARBIN battery test systems that HSAs/NPNi combination electrodes carry out discharge capacity test as working electrode
Upper progress.Under the conditions of 25 DEG C of room temperature, electrode is with 60mAg-1The current density charging 7.5h of (0.2C), stands 30min, then
With 60mAg-1The current density of (0.2C) is discharged to blanking voltage and reaches -0.74V relative to Hg/HgO reference electrodes, circulates 4 times
Activated, reach maximum discharge capacity Cmax；Completely after activation, high-rate discharge ability test is carried out, electrode is with 300mAg-1
The current density charging of (1C), then with 300,600,900,1200,1500,2400,3000mAg-1The current density of (10C) point
Blanking voltage is not discharged to it：- 0.65, -0.6, -0.5, -0.45, -0.4, -0.35, -0.3V, the blanking voltage are relative to Hg/
HgO reference electrodes；
(5) electrochemical property test is carried out on IVIUM electrochemical workstations.It is 5mV in the amplitude relative to OCP
Shi Jinhang ac impedance measurements, the frequency range of test is by 100kHz to 5mHz；Under the conditions of 50% depth of discharge, relative to
When OCP potential scan scope is -5 to 5mV, carry out sweeping linear polarisation curves test of the speed for 0.05mV/s；In 50% electric discharge
Under depth conditions, when being 0 to 1.5V relative to OCP potential scan scope, carry out sweeping the anodic polarization curves that speed is 5mV/s
Test；Under 100% charged state, under the potential step relative to Hg/HgO+500mV, carry out 4000s electric current-when
The test of half interval contour.
The pattern and structural characterization of HSAs/NPNi composites：
Foundry alloy, HSAs/NPNi composites and NPNi surface topography are observed by ESEM (SEM), referring to figure
3- Fig. 5.Foundry alloy surface is smooth as can be seen from Figure 3.Compared with the smooth surface of foundry alloy, HSAs/NPNi composite woods
The surface of material is relatively rough, and alloy surface is by nanoporous nickel coated (see Fig. 4).In H2400 DEG C of conditions in/Ar gaseous mixture atmosphere
Under, Ni (OH)2NPNi is reduced to, forms the hole of three-dimensional co-continuous, its intermediate pore size is about 200nm, and ligament size is about
150nm (see Fig. 5).Fig. 6 is NPNi transmission electron microscope (TEM) photo, can be seen that NPNi has three-dimensional doubly-linked with reference to Fig. 5, Fig. 6
Continuous nano-porous structure, and NPNi ligaments show bi-curved characters and appearances, wherein positive camber form ligament and negative cruvature
Form nano-pore.Fig. 7 is NPNi HRTEM photos, it can be seen that (111), interplanar distance corresponding to (010) and (200) crystal face
Respectively 0.203,0.233 and 0.176nm, corresponded with the feature interplanar distance of nickel.Fig. 8 is foundry alloy and HSAs/NPNi
The XRD spectrum of composite, the characteristic diffraction peak of foundry alloy correspond to CaCu5The hexagonal structure of type.However, HSAs/NPNi is answered
Condensation material not only has the hexagonal structure of CaCu5 types, and has the characteristic peak of nickel.
At ambient temperature, the Electrochemical Characterization of foundry alloy and HSAs/NPNi composites：
When carrying out electro-chemical test, composite and foundry alloy the two electrodes are all easier to activate, and circulate 4 weeks
Reach maximum discharge capacity.As shown in figure 1, in all discharge current density IcUnder, the high magnification of HSAs/NPNi combination electrodes
Discharge performance is better than the high-rate discharge ability of foundry alloy, and both gaps are in IcBecome apparent from when larger.In electric discharge electricity
Current density is 3000mAg-1When, the capacity retention rate of composite is 3.2 times of foundry alloy capacity retention rate.Fig. 9 is two electrodes
Linear polarisation curves under 50% depth of discharge.Surface exchange current density value I0It can be calculated by the slope of figure cathetus
Arrive.The I of composite electrode0It is worth larger, i.e., its electrochemical reaction rates is than foundry alloy electrode more in the case where being bordering on poised state
It hurry up.This is due to that nanoporous nickel plays catalytic action to Hydrogen evolving reaction (HER), makes the electrochemical reaction rates of electrode surface
Accelerate, the loose structure of porous nickel three-dimensional co-continuous accelerates electronics and ion transmission speed, and then improves the electrochemistry of electrode
Dynamics, improve high-rate discharge ability.Figure 10 is the test result of electrochemical impedance collection of illustrative plates, it can be seen that each collection of illustrative plates is
It is made up of two semicircles of high frequency region and the straight line of low frequency range.What small and big semicircle reflected respectively be alloying pellet it
Between or the contact resistance (R between alloying pellet and current collector (being NPNi here)c) and electrode charge transfer resistance (Rct)。
And the straight line portion of low frequency range is then mainly due to Warburg impedances.Half circular diameter is smaller, and its impedance is smaller.Therefore, nanometer is more
Hole nickel composite material has less RCAnd RCTValue, nanometer is more in this bicontinuous structure and composite with nanoporous nickel
Close interaction between hole nickel and hydrogen storage alloy particle is relevant.Figure 11 gives foundry alloy and HSAs/NPNi composites
Anodic polarization curves.In process of anodic polarization, current density increases with the increase of overpotential first, then reaches most
Big value, the value are defined as limiting current density (IL)。ILIt is relevant with diffusion rate of the hydrogen atom inside alloy, ILIt is worth bigger, hydrogen
The diffusion velocity of atom is also bigger.The diffusion rate of the hydrogen atom of HSAs/NPNi combination electrodes is than foundry alloy electricity as seen from the figure
Pole it is big.Figure 12 is potential step figure, it can be seen that initial period, current density drastically decline, with the extension of time, electric
Current density linearly declines.It can be calculated by the linear segment in fitted figure：The hydrogen atom of HSAs/NPNi combination electrodes
Diffusion coefficient is bigger than foundry alloy electrode.To sum up, there is HSAs/NPNi composite electrodes faster surface electrochemistry to react
Speed and alloy internal hydrogen atomic diffusion rates, are effectively improved its high-rate discharge ability.The composite can be used as nickel
The negative material of hydrogen battery, there is good application prospect in high-power battery field.Preparation method of the present invention may be used also
To be extended to other hydrogen bearing alloy systems, new method and think of are provided further to improve Ni-MH battery high-rate discharge ability
Road.
Claims (5)
1. the preparation method of a kind of hydrogen bearing alloy and nanoporous nickel composite material (HSAs/NPNi), comprises the following steps：
A, in high-purity argon gas atmosphere by the lanthanum of method melting purity >=99.5 of electric arc melting, cerium, yttrium, nickel, cobalt, manganese and
Aluminium, obtain its ingot casting；
B, ingot casting is annealed under argon atmosphere and mechanical lapping obtains master alloy powder, its average particulate diameter is 50 μ
m；
C, Ni (OH) is prepared with simple hydro-thermal method2Powder, by 1.4~1.5g Ni (NO3)2, 1.3~1.5g, six methylene four
The mixture of amine (HMT) and 30~40ml ultra-pure waters is added in the stainless steel autoclave with polytetrafluoroethyllining lining；
The reactor of sealing is put into 10~12h of insulation in 100~120 DEG C of electric dry ovens, by green product Ni (OH)2Received by centrifuging
Collection；
D, by prepared Ni (OH)2Grind in agate mortar with foundry alloy and uniformly integrated；By mixture in electric dry oven
Dry, then in tube furnace Ar/H25~6h is heat-treated in gaseous mixture atmosphere under the conditions of 400~450 DEG C, HSAs/NPNi is prepared and answers
Condensation material.
2. the preparation side of a kind of hydrogen bearing alloy according to claim 1 and nanoporous nickel composite material (HSAs/NPNi)
Method, it is characterised in that the composition of ingot casting is AB in the step a5、AB2Or AB3Type hydrogen storage alloy.
3. the preparation side of a kind of hydrogen bearing alloy according to claim 1 and nanoporous nickel composite material (HSAs/NPNi)
Method, it is characterised in that Ni (OH) is prepared in the step c2When, Ni (NO3)2It is the different quality of same ratio with HMT.
4. the preparation side of a kind of hydrogen bearing alloy according to claim 1 and nanoporous nickel composite material (HSAs/NPNi)
Method, it is characterised in that the Elevated Temperature Conditions of tube furnace are 1~3 DEG C/min in step d.
5. the hydrogen bearing alloy that preparation method according to claim 1 obtains and nanoporous nickel composite material (HSAs/
NPNi), it carries out electro-chemical test as electrode material, comprises the following steps：
A, first 0.25~0.255g active materials are well mixed with 1.0~1.02g carbonyl nickel powders, then by tablet press machine 8~
A diameter of 10~15mm electrode slice is pressed under 20MPa pressure, electrode is immersed in 2 in 25~35wt% KOH solution~
4h, it is set to be soaked completely before electro-chemical test；
B, electro-chemical test is carried out in the three-electrode system of a standard, and the electrode prepared in wherein step a is as work
Make electrode, sintering Ni (OH)2/ NiOOH electrodes are used as to electrode, mercury/mercury oxide (Hg/HgO) electrode as reference electrode, 25~
35wt% KOH solution is as electrolyte；
C, it is in ARBIN battery testings system to carry out discharge capacity test as working electrode by the use of the HSAs/NPNi combination electrodes
Carried out on system, under the conditions of 25 DEG C of room temperature, electrode is with 60mA g-1Current density charging 7.5h, stand 30min, then with
60mA g-1Current density be discharged to blanking voltage and reach -0.74V relative to Hg/HgO reference electrodes, circulation is lived for 4 times
Change, reach maximum discharge capacity Cmax；
D, completely after activation, high-rate discharge ability test is carried out, electrode is with 300mA g-1Current density charging, then with
300,600,900,1200,1500,2400,3000mA g-1Current density be discharged to blanking voltage respectively：-0.65,-0.6,-
0.5, -0.45, -0.4, -0.35, -0.3V, the blanking voltage are relative to Hg/HgO reference electrodes；
E, electrochemical property test is carried out on IVIUM electrochemical workstations, in the amplitude relative to OCP (OCP)
To carry out ac impedance measurement during 5mV, the frequency range of test is by 100kHz to 5mHz；Under the conditions of 50% depth of discharge,
When relative to OCP potential scan scope being -5 to 5mV, sweep speed and tested for 0.05mV/s linear polarisation curves；
Under the conditions of 50% depth of discharge, when being 0 to 1.5V relative to OCP potential scan scope, carry out sweeping the anode that speed is 5mV/s
Polarization curve is tested；Under 100% charged state, under the potential step relative to Hg/HgO+500mV, carry out 4000s's
The test of current versus time curve；
F, the hydrogen bearing alloy prepared and negative pole of the nanoporous nickel composite material (HSAs/NPNi) as Ni-MH battery, have excellent
Good high-rate discharge ability, it is 3000mAg in discharge current density-1When, its capacity retention rate is up to 43.11%, is independent
3.2 times of foundry alloy electrode.
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| CN106654212B (en) * | 2016-12-29 | 2019-07-30 | 吉林大学 | A kind of Co3O4The preparation method and application of/N-RGO/HSAs composite material |
| CN108054369A (en) * | 2017-12-15 | 2018-05-18 | 淄博君行电源技术有限公司 | A kind of preparation method of hydrogen bearing alloy and graphene composite material |
| CN110013864B (en) * | 2019-04-30 | 2021-07-27 | 西北师范大学 | Preparation of nickel cobaltate/bismuth oxychloride nanocomposite and application of nanocomposite in catalytic reduction of organic matters |
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