CN103539066A - NiF2-dopped LiBH4-LiNH2-CaH2 composite hydrogen storage material and preparation method thereof - Google Patents

NiF2-dopped LiBH4-LiNH2-CaH2 composite hydrogen storage material and preparation method thereof Download PDF

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CN103539066A
CN103539066A CN201210243988.5A CN201210243988A CN103539066A CN 103539066 A CN103539066 A CN 103539066A CN 201210243988 A CN201210243988 A CN 201210243988A CN 103539066 A CN103539066 A CN 103539066A
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孙立贤
刘慧�
徐芬
曹忠
司晓亮
李志宝
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Dalian Institute of Chemical Physics of CAS
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Abstract

The invention relates to a preparation method of an NiF2-dopped LiBH4-LiNH2-CaH2 composite hydrogen storage material, in particular relates to a hydrogen storage material which improves the hydrogen desorption performance of an LiBH4-LiNH2-CaH2 system through doping NiF2 and a preparation method thereof, and belongs to the technical field of modification. The composite material is prepared by utilizing a mechanical milling method, when the doping amount of NiF2 is 5wt%, the system starts greatly desorbing hydrogen at 47 DEG C, the main hydrogen desorption peak temperature is 234 DEG C, and the hydrogen desorption amount reaches 3.75wt% at 175 DEG C within 5000s; the hydrogen desorption amount reaches 5.03wt% within 5h; the hydrogen desorption amount reaches 6wt% at 200 DEG C within 5000s; the hydrogen desorption amount reaches 6.55wt% at 270 DEG C within 1000s. The composite hydrogen storage material which is prepared by ball milling has good hydrogen storage and desorption performances, and the prepared NiF2-dopped LiBH4-LiNH2-CaH2 composite hydrogen storage material has good hydrogen desorption performance at low temperatures.

Description

NiF 2li doped BH 4-LiNH 2-CaH 2composite hydrogen storage material and preparation method thereof
Technical field
The present invention relates to a kind of hydrogen storage material modification technology field, particularly utilize NiF 2doping improves LiBH 4-LiNH 2-CaH 2hydrogen storage material of system hydrogen storage property and preparation method thereof.
Background technology
Hydrogen Energy is complete cleaning, resourceful secondary energy, utilizes Hydrogen Energy to replace the focus that fossil oil has become global concern.In order to realize the sizable application of Hydrogen Energy, the cheapness that need to solve hydrogen is produced, safe and efficient accumulating and the large technology of large-scale application three, and hydrogen storage technology is the Main Bottleneck that current Hydrogen Energy is utilized.Solid-state storage hydrogen is a kind of efficient hydrogen storage technology with development prospect, the hydrogen storage material performance requriements proposing in order to reach International Energy Agency, and researcher has carried out a large amount of research extensively and profoundly.After conventional high-tension storage hydrogen, liquefaction hydrogen storage, researchist has developed LaNi 5, Mg 2the hydrogen storage alloy such as Ni, TiFe, has opened new era that hydrogen storage material is studied.Subsequently, various novel hydrogen storage materials receive publicity in succession, from simple binary hydrogen storage alloy, develop into multi-element metal alloy that performance is more excellent and inorganic hydride, organic compound, novel active carbon material and carbon nanotube, metal-organic framework materials, covalency organic framework material, molecular sieve imidazoles framework material etc.
Yet, the performance of existing hydrogen storage material also cannot meet or can not meet simultaneously the application requiring of the secondary energy carrier of the renewable energy sources such as on-board hydrogen source system and wind energy, biomass energy, so the research and development of novel hydrogen storage material becomes Hydrogen Energy applied research personnel's top priority.At present, more and more receive everybody concern with the light hydrogen occluding material headed by Metal-B-N-H system, lightweight element hydrogen storage material has become the new direction of research.
Li-B-N-H system hydrogen storage material has higher hydrogen discharging temperature, can effectively reduce the hydrogen discharging temperature of system by adding magnesium-yttrium-transition metal catalyzer.LiBH 4-3LiNH 2system has the hydrogen desorption capacity of 11.12wt.%, but hydrogen discharging temperature is higher, and puts to follow in hydrogen process and discharge NH 3.In order further to address these problems, Pinkerton and Meyer NiCl 2catalysis LiBH 4-3LiNH 2compound system, can put hydrogen 7.5wt% at 160-260 ℃, but in system, still have a small amount of NH 3emit (Pinkerton F.E., Meyer M.S..Hydrogen Desorption Behavior of Nickel-Chloride-Catalyzed Stoichiometric Li 4bN 3h 10[J] .J.Phys.Chem.C2009,113,11172).Have report to point out, LiH can reduce LiBH 4-3LiNH 2system is put NH in hydrogen process 3amount (Zheng X.l., Xiong Zh.T., Lim Y.H., Wu G.T., Chen P., Chen H..Improving Effects of LiH and Co-Catalyst on the Dehydrogenation of Li 4bN 3h 10[J] .J.Phys.Chem.C2011,115,8840).Our preliminary study shows, LiBH 4-LiNH 2-CaH 2the NH of system 3burst size obviously reduces, but this system thermodynamics and kinetics performance is all to be improved, NiF 2doping is to LiBH 4-LiNH 2-CaH 2the effect of improving of system dehydrogenation have not been reported.This patent adopts NiF first 2as doping agent, studied it to LiBH 4-LiNH 2-CaH 2the impact of system dehydrogenation.
Summary of the invention
The object of patent of the present invention is to solve LiBH 4-LiNH 2the above-mentioned hydrogen discharging temperature of system is too high and put the problem of following foreign gas to produce in hydrogen process, improves LiBH 4-LiNH 2the storage hydrogen discharging performance of system, the invention provides a kind of NiF 2li doped BH 4-LiNH 2-CaH 2system is improved hydrogen storage material of its reversible hydrogen adsorption and desorption performance and preparation method thereof.
NiF 2li doped BH 4-LiNH 2-CaH 2composite hydrogen storage material, prepares the awt%LiBH of different ratios content by the additive of doping different content 4-bwt%LiNH 2-c wt%CaH 2-d wt% NiF 2, wherein, a=10-20, b=45-55, c=25-35, d=3-7.
Preferred feedstock consists of:
Figure BDA00001885874600021
The present invention relates to a kind of NiF 2li doped BH 4-LiNH 2-CaH 2the preparation method of composite hydrogen storage material, its concrete operation step is as follows:
A. take raw material;
The composition of described raw material and quality percentage composition are:
Figure BDA00001885874600022
B. in the glove box under argon gas atmosphere protection, by LiBH 4, LiNH 2, CaH 2and NiF 2in the ratio of 10-20wt%: 45-55w%: 25-35wt%: 3-7wt%, pack in the ball grinder of 100mL together with 5-15 10mm Stainless Steel Ball (3.5g/).After ball milling mixing 3-15h, again bring back that in glove box, to fill sample standby.
D., it is 200r/min-400r/min that rotational speed of ball-mill is set, and Ball-milling Time is 3-15h.
NiF 2the LiBH of powder doping 4-LiNH 2-CaH 2system can lower temperature transfer hydrogen according to being, in mechanical milling process, generated Li 4bN 3h 10mixture and Ca-N-B-H compound, in temperature-rise period, Ni ion may participate in the dehydrogenation reaction of mixture, has weakened B-H key and N-H key, impels the activation energy that dissociates of H to reduce.
NiF 2as additive, can effectively reduce LiBH 4-LiNH 2-CaH 2the hydrogen discharging temperature of system.NiF provided by the present invention 2li doped BH 4-LiNH 2-CaH 2composite highly effective hydrogen storage material and preparation method thereof tool has the following advantages and is: utilize at LiBH 4-LiNH 2-CaH 2ni doped F in system 2method, in mechanical milling process, form Li 4bN 3h 10mixture and Ca-N-B-H compound, and in temperature-rise period with NiF 2by interacting, generate product Li 3bN 2with Ca-N-H compound, thus the hydrogen storage property of the system of acceleration.Particularly, work as NiF 2when doping is 5wt%, system starts to put in a large number hydrogen at 47 ° of C, and in the time of 175 ℃, in 5000s, hydrogen desorption capacity has reached 3.75wt%, puts hydrogen 5.03wt% in 5h, in the time of 200 ℃, in 5000s, hydrogen desorption capacity has reached 6wt%, and in the time of 270 ℃, in 1000s, hydrogen desorption capacity has reached 6.55wt%.。
Accompanying drawing explanation
Fig. 1 .LiBH 4-LiNH 2-CaH 2system Ni doped F 2the thermogravimetric of front and back composite hydrogen storage material (being called for short TG, 5 ℃/min) correlation curve.
Fig. 2 .LiBH 4-LiNH 2-CaH 2system Ni doped F 2the mass spectrum of front and back composite hydrogen storage material (being called for short MS, 5 ℃/min) correlation curve.
Fig. 3 A.NiF 2li doped BH 4-LiNH 2-CaH 2differential scanning calorimetry (the be called for short DSC) curve of system under different temperature rise rates (2 ℃/min, 5 ℃/min, 10 ℃/min, 12 ℃/min).
Fig. 3 B.LiBH 4-LiNH 2-CaH 2system Ni doped F 2the DSC correlation curve of front and back composite hydrogen storage material.
Fig. 4 .NiF 2li doped BH 4-LiNH 2-CaH 2the PCT Hydrogen desorption isotherms of system under differing temps (175 ℃, 200 ℃, 270 ℃).
Fig. 5 .NiF 2li doped BH 4-LiNH 2-CaH 2after system ball milling and in differing temps (175 ℃, 200 ℃, 270 ℃), transfer the XRD figure spectrum contrast figure after hydrogen.
Fig. 6 .NiF 2li doped BH 4-LiNH 2-CaH 2after system ball milling and in differing temps (175 ℃, 200 ℃, 270 ℃), transfer the FTIR collection of illustrative plates contrast figure after hydrogen.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment 1:NiF 2li doped BH 4-LiNH 2-CaH 2the preparation of composite hydrogen storage material
In the glove box under argon shield, 15wt%:50wt%:30wt%:5wt% takes the LiBH of common heavy 0.5g in mass ratio 4, LiNH 2, CaH 2and NiF 2raw material, pours in the 100mL ball grinder that 5 10mm Stainless Steel Balls (17.5g) are housed, and will after ball grinder sealing, from glove box, take out; Ball grinder is loaded on planetary ball mill QM-3SP2; Rotational speed of ball-mill is made as 200r/min, and Ball-milling Time is 15h, after ball milling completes, ball grinder is relay to turn round and stretch out the hand in casing samples.
By changing the doping of additive and additive, prepare different composite hydrogen storage materials; Described raw material is LiBH 4, LiNH 2, CaH 2and NiF 2; Additive is NiF 2.
Embodiment 2: the NiF of embodiment 1 preparation 2li doped BH 4-LiNH 2-CaH 2the TG-MS of composite hydrogen storage material analyzes
The sample that takes 90mg from glove box carries out thermogravimetric-mass spectrum (TG-MS) analysis.What this test adopted is TherMax 500 gentle GAM 200 mass spectrometries in hot high pressure sky, Ar gas carrier gas flux is controlled at 1.7%(-145mL/min), after dress sample, first system is vacuumized to (5-10min) ventilation, intensification scope is RT-400 ℃, and temperature rise rate is 5 ℃/min.Analytical results shows, does not add the LiBH of catalyzer 4-LiNH 2-CaH 2it is slow that sample was put hydrogen before 300 ℃, and weight loss only reaches 2.7wt% left and right.Add NiF 2sample 250 ℃ of left and right, completed and put in a large number hydrogen, total weight loss surpasses 13wt%, as shown in Figure 1, NiF is described 2to LiBH 4-LiNH 2-CaH 2compound system has obvious catalytic effect, can accelerate system dehydrogenation rate and increase weight loss.Doping 5wt%NiF 2the initial hydrogen discharging temperature of compound system be 47 ℃, and finish in the time of 268 ℃, it is main, and to put hydrogen peak temperature be 234 ℃, than not adding NiF 2time reduced by 110 ℃, as shown in Figure 2, NiF is described 2can reduce LiBH 4-LiNH 2-CaH 2the hydrogen discharging temperature of compound system.
Embodiment 3: the NiF of embodiment 1 preparation 2li doped BH 4-LiNH 2-CaH 2the dsc analysis of composite hydrogen storage material
That this test adopts is the Q1000DSC that U.S. TA company produces, and Ar gas carrier gas flux is controlled at 50mL/min.Oxidized for avoid filling in sample process material in crucible, this operates in glove box and carries out.
Fig. 3 A is the 5wt%NiF that adulterates under different temperature rise rates 2the DSC curve of compound system.Result shows: when changing temperature rise rate (2 ℃/min, 5 ℃/min, 10 ℃/min, 12 ℃/min), and the variation of Development pattern thereupon of the peak temperature of system,, along with the rising of temperature rise rate, the fusing point of system progressively raises.Meanwhile, the LiBH being prepared by ball milling under similarity condition 4-LiNH 2-CaH 2sample after system and doping contrasts, as shown in Figure 3 B.Result shows: 5wt% NiF has adulterated 2compound system heat effect obviously weaken, may be conducive to strengthen the reversible hydrogen adsorption and desorption performance of system.
Embodiment 4: the NiF of embodiment 1 preparation 2li doped BH 4-LiNH 2-CaH 2the hydrogen desorption kinetics performance analysis of composite hydrogen storage material under differing temps
On the gas reaction control device Sieverts-type PCT that this test Shi U.S. Advanced Materials Corporation company produces, carry out.
In Fig. 4, a, b, c are respectively doping 5wt% NiF 2liBH 4-LiNH 2-CaH 2compound system is at the PCT Hydrogen desorption isotherms of 175 ℃, 200 ℃, 270 ℃.As can be seen from Figure 4 the doping 5wt% NiF, preparing in the present invention 2liBH 4-LiNH 2-CaH 2composite hydrogen storage material in the time of 175 ℃ in 5000s hydrogen desorption capacity reached 3.75wt%, in 5h, put hydrogen 5.03wt%, in the time of 200 ℃, hydrogen desorption capacity has reached 6wt% in 5000s, in the time of 270 ℃, in 1000s, hydrogen desorption capacity has reached 6.55wt%.
Embodiment 5: the NiF of embodiment 1 preparation 2li doped BH 4-LiNH 2-CaH 2system composite hydrogen storage material and transfer the XRD analysis of hydrogen after product in differing temps
The material phase analysis of this compound system is to carry out on Dutch PANalytical company X-ray diffractometer (X ' Pert MPD PRO, CuKa, 40kV, 40mA), to doping 5wt% NiF 2liBH 4-LiNH 2sample after compound system ball milling and the phase of transferring after hydrogen in differing temps (175 ℃, 200 ℃, 270 ℃) are analyzed.For avoiding in XRD test process material oxidized, in glove box, with amorphous film, cover the material surface of testing.
In Fig. 5, a, b, c, d are respectively doping 5wt% NiF 2liBH 4-LiNH 2-CaH 2after compound system ball milling, 175 ℃, 200 ℃, 270 ℃ XRD figure spectrums of putting hydrogen after product.As can be seen from the figure: in mechanical milling process, generated Li 4bN 3h 10mixture, along with the rising of temperature, in system its peak intensity more and more a little less than, simultaneously in product, Li detected 3bN 2, Li is described 4bN 3h 10occurred progressively to decompose, and generated Li 3bN 2; In addition, in mechanical milling process, also there are other mixtures in the appearance explanation at ball milling after product peak, 35.2 ° of positions 35.5 ° of positions and in putting hydrogen product, its composition may be the compound of Ca-B-N-H, and putting hydrogen, to put the product that should generate afterwards may be Ca-N-H compound.
Embodiment 6: the NiF of embodiment 1 preparation 2li doped BH 4-LiNH 2-CaH 2composite hydrogen storage material and analyzing at the FTIR that differing temps is transferred hydrogen after product
The material phase analysis of this compound system carries out on Nicolet 380 infrared spectroscopy instrument, to doping 5wt% NiF 2liBH 4-LiNH 2-CaH 2sample after compound system ball milling and the phase of transferring after hydrogen in differing temps (175 ℃, 200 ℃, 270 ℃) are analyzed.
In Fig. 6, a, b, c, d are respectively doping 5wt% NiF 2liBH 4-LiNH 2-CaH 2after compound system ball milling, 175 ℃, 200 ℃, the 270 ℃ FTIR collection of illustrative plates of putting hydrogen after product.As can be seen from the figure: 3240cm -1the characteristic peak of position N-H key shows to have generated in mechanical milling process Li 4bN 3h 10mixture, along with temperature raises, this peak weakens gradually, 2200-2400cm -1b-H key stretching vibration peak intensity and the 3400cm of position -1the N-H key stretching vibration peak intensity of left and right also weakens gradually, and Li is described along with temperature raises 4bN 3h 10mixture decomposes gradually, releasing hydrogen gas; Put hydrogen product at 3150cm simultaneously -1the peak that left and right occurs is Li 2the stretching vibration peak of the N-H key of NH, showing has Li in reaction 2nH generates.

Claims (6)

1.NiF 2li doped BH 4-LiNH 2-CaH 2composite hydrogen storage material, is characterized in that:
By the additive of doping different content, prepare a wt%LiBH of different ratios content 4-b wt%L iNH 2-c wt% CaH 2-d wt%Ni F 2, wherein, a=10-20, b=45-55, c=25-35, d=3-7.
2. composite hydrogen storage material according to claim 1, is characterized in that:
It adopts following operation steps to obtain:
A. take dusty raw materials;
The composition of described raw material and quality percentage composition are:
B. in being full of the glove box of argon gas, the raw material that is 1:30-1:100 by mass ratio and abrading-ball are inserted in ball grinder;
C., it is 200r/min-400r/min that rotational speed of ball-mill is set, and Ball-milling Time is 3-15h.
3. composite hydrogen storage material according to claim 2, is characterized in that: during ball milling, described ratio of grinding media to material is 30:1, and Ball-milling Time is 15h, and rotating speed is 200r/min.
4. composite hydrogen storage material according to claim 1, is characterized in that:
Preferred feedstock consists of:
Figure FDA00001885874500012
5. the NiF described in a claim 1,2,3 or 4 2li doped BH 4-LiNH 2-CaH 2the preparation method of composite hydrogen storage material, is characterized in that:
It adopts following operation steps to obtain:
A. take dusty raw materials;
The composition of described raw material and quality percentage composition are:
Figure FDA00001885874500013
B. in being full of the glove box of argon gas, the raw material that is 1:30-1:100 by mass ratio and abrading-ball are inserted in ball grinder;
C., it is 200r/min-400r/min that rotational speed of ball-mill is set, and Ball-milling Time is 3-15h.
6. the preparation method of composite hydrogen storage material according to claim 5, is characterized in that: during ball milling, described ratio of grinding media to material is 30:1, and Ball-milling Time is 15h, and rotating speed is 200r/min.
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Cited By (8)

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CN104724672A (en) * 2015-03-13 2015-06-24 桂林电子科技大学 (NH4) 2TiF6 doped boryl hydrogen storage material and preparation method thereof
CN106145031A (en) * 2016-07-06 2016-11-23 扬州大学 A kind of LiNH improving hydrogen storage property2the preparation method of LiH hydrogen storage material
CN106430097A (en) * 2016-08-31 2017-02-22 北京理工大学 Composite hydrogen storage material and preparation method thereof
CN106564859A (en) * 2016-11-15 2017-04-19 复旦大学 Efficient composite hydrogen storage material NaAlH4@CeO2 and preparation method therefor
CN107253697A (en) * 2017-06-16 2017-10-17 扬州大学 A kind of multi-walled carbon nanotube that adulterates improves the Li of hydrogen storage property3N hydrogen storage materials and preparation method thereof
CN107934913A (en) * 2017-11-14 2018-04-20 桂林电子科技大学 The preparation and its application in hydrogen storage material of a kind of composite hydrogen storage material of transition metal fluorides doping
CN108689384A (en) * 2018-08-22 2018-10-23 燕山大学 A kind of composite hydrogen storage material and its preparation method and application
CN112110425A (en) * 2020-08-14 2020-12-22 浙江工业大学 Synthesis method of amino lithium potassium

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104724672A (en) * 2015-03-13 2015-06-24 桂林电子科技大学 (NH4) 2TiF6 doped boryl hydrogen storage material and preparation method thereof
CN106145031A (en) * 2016-07-06 2016-11-23 扬州大学 A kind of LiNH improving hydrogen storage property2the preparation method of LiH hydrogen storage material
CN106430097A (en) * 2016-08-31 2017-02-22 北京理工大学 Composite hydrogen storage material and preparation method thereof
CN106430097B (en) * 2016-08-31 2019-09-10 北京理工大学 Composite hydrogen storage material and preparation method thereof
CN106564859A (en) * 2016-11-15 2017-04-19 复旦大学 Efficient composite hydrogen storage material NaAlH4@CeO2 and preparation method therefor
CN106564859B (en) * 2016-11-15 2019-04-05 复旦大学 A kind of efficient composite hydrogen storage material NaAlH4@CeO2And preparation method thereof
CN107253697A (en) * 2017-06-16 2017-10-17 扬州大学 A kind of multi-walled carbon nanotube that adulterates improves the Li of hydrogen storage property3N hydrogen storage materials and preparation method thereof
CN107934913A (en) * 2017-11-14 2018-04-20 桂林电子科技大学 The preparation and its application in hydrogen storage material of a kind of composite hydrogen storage material of transition metal fluorides doping
CN107934913B (en) * 2017-11-14 2020-01-21 桂林电子科技大学 Preparation of transition metal fluoride doped composite hydrogen storage material and application thereof in hydrogen storage material
CN108689384A (en) * 2018-08-22 2018-10-23 燕山大学 A kind of composite hydrogen storage material and its preparation method and application
CN108689384B (en) * 2018-08-22 2020-04-28 燕山大学 Composite hydrogen storage material and preparation method and application thereof
CN112110425A (en) * 2020-08-14 2020-12-22 浙江工业大学 Synthesis method of amino lithium potassium

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