CN104891434A - Borohydride/graphite fluoride nanocomposite hydrogen storage material and preparation method thereof - Google Patents
Borohydride/graphite fluoride nanocomposite hydrogen storage material and preparation method thereof Download PDFInfo
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- CN104891434A CN104891434A CN201510218718.2A CN201510218718A CN104891434A CN 104891434 A CN104891434 A CN 104891434A CN 201510218718 A CN201510218718 A CN 201510218718A CN 104891434 A CN104891434 A CN 104891434A
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Abstract
The invention discloses a nanometer borohydride/graphite fluoride composite hydrogen storage material and a preparation method thereof. The composite hydrogen storage material comprises borohydride and graphite fluoride, wherein the mass percentage of graphite fluoride in the borohydride/graphite fluoride composite hydrogen storage material is 40%. The composite method for preparing the composite hydrogen storage material is a high-energy ball milling method. The borohydride/graphite fluoride nanocomposite hydrogen storage material provided by the invention has medium and low temperature hydrogen desorption kinetic performances and high hydrogen desorption capacity, has a hydrogen desorption capacity at about 200DEG C reaching above 7.0wt%, and can be used in fields of small mobile equipment, notebook power supplies, and hydrogen supply sources of independent electric pile systems.
Description
The divisional application that patent application of the present invention is the applying date is on June 4th, 2013, application number is 201310218490.8, name is called the Chinese patent application of Hydroboron/graphite fluoride nano-composite hydrogen storage material and preparation method thereof.
Technical field
The present invention relates to hydrogen storage material, especially, a kind of nanometer Hydroboron/graphite fluoride nano-composite hydrogen storage material and preparation method thereof.
Background technology
The energy is the source of human social development, hydrogen is a kind of very superior new forms of energy, also be the energy the cleanest in the world, be devoted to the common recognition that the clean reproducible energy technology developed using hydrogen as energy carrier has become the whole world, the research and apply of wherein relevant to fuel cell hydrogen source system novel high-capacity hydrogen storage material is subject to the pay abundant attention of countries in the world.So far, the successful operation on hydrogen-burning automobile or electromobile all of the liquid hydrogen in hydrogen storage technology, lightweight high pressure vessel and Metal hydride systems.In above-mentioned three kinds of hydrogen storage systems, the security of solid-state hydrogen storage material is good, volume hydrogen-storage density is the highest, but conventional metals hydride is (as LaNi
5, TiMn
2deng) gravimetric hydrogen storage density lower than 2.0wt.%, be difficult to the hydrogen-storage density requirement meeting practical application; And MgH
2although hydrogen storage capability is up to 7.6wt.%, MgH
2effectively need could inhale more than 300 DEG C and put hydrogen, and it inhales its practical application of hydrogen desorption kinetics performance limitations " L.Schlapbach, A.Z ü ttel, Nature, 414 (2001) 353 – 358. " slowly.
Research shows, the various new hydrogen storage material be made up of lightweight element, as alanate, hydroborate and aminocompound etc., have higher theoretical hydrogen storage capability (>5.0wt.%), the breakthrough for hydrogen storage material utilisation technology brings new hope.Wherein, with LiBH
4for the coordination hydroborate of Typical Representative, its theoretical weight hydrogen-storage density, up to 18.4wt.%, is the high power capacity storage hydrogen material that a class has application potential.But, LiBH
4remain at two hang-ups as the application of storage hydrogen: 1) thermodynamic property is too stable, and it is put the hydrogen balance pressure hydrogen discharging temperature reached needed for 1bar and is about 400 DEG C; 2) inhale hydrogen desorption kinetics poor-performing, put hydrogen fast temperature required more than 450 DEG C, and inhale pressure needed for hydrogen again more than 35MPa " J.Graetz.Chem.Soc.Rev., 2009,38,73 – 82. ".
Summary of the invention
The object of the present invention is to provide the simple nanometer hydroborate/fluorographite composite hydrogen storage material of a kind of preparation method, quick hydrogen discharging performance can be realized under middle cold condition.
For achieving the above object, the present invention is by the following technical solutions:
A kind of nanometer hydroborate/fluorographite composite hydrogen storage material, described composite hydrogen storage material comprises hydroborate and fluorographite, and wherein fluorographite accounts for the per-cent of described hydroborate/fluorographite composite hydrogen storage material oeverall quality is 40%.
Preferably, described hydroborate is LiBH
4or NaBH
4alkali metal borohydride in any one.
Further, the form of described hydroborate is the powder particle of nanoscale, and the form of described fluorographite is the powder solid of the lamellar of micro-meter scale, and described nanometer borohydride powder uniform particles is distributed in described fluorographite powder solid on the surface.
Preferably, the particle size of described hydroborate is 90nm.
The preparation method of aforesaid hydroborate/fluorographite composite hydrogen storage material, it comprises the following steps:
The first step, prepare fluorographite (general formula is FGi), tetrafluoroethylene and carbon black fine powder are cold-pressed into after 5:1 mixing the disk of 10mm diameter under a certain pressure, then electric tube furnace is put into and logical argon shield, furnace temperature rises to 250 DEG C from room temperature subsequently, be incubated 5h and furnace cooling, the fluorographite of powdery can be obtained;
Second step, preparation Hydroboron/graphite fluoride nano-composite hydrogen storage material, example takes hydroborate and fluorographite in mass ratio, carries out mechanical ball milling after both evenly being mixed under high-purity hydrogen condition.
Preferably, in preceding method in step 2, described hydroborate is LiBH
4or NaBH
4alkali metal borohydride in any one.
Preferably, fluorographite accounts for the per-cent of described hydroborate/fluorographite composite hydrogen storage material oeverall quality is 40%.
Preferably, Ball-milling Time is 1 ~ 10h, and filling hydrogen protection pressure is 0.5 ~ 2.0MPa.
More preferred, Ball-milling Time is 2h, and filling hydrogen protection pressure is 1.0MPa.
The hydroborate that the present invention adopts mechanical ball milling method to prepare/fluorographite composite hydrogen storage material, shown by scanning electron microscope analysis, in composite hydrogen storage material, the particle size of hydroborate is all less than 100nm, putting in hydrogen process, the hydroborate of nanometer and fluorographite react releasing hydrogen gas and heat, as numerous nano dot firearm, elevate the temperature instantaneously, light corresponding LiBH
4hydrogen discharge reaction, and form chain reaction with quick releasing hydrogen gas.This composite hydrogen storage material, without the need to reactivation process, directly can carry out hydrogen storage performance measurement.Directly can release the hydrogen up to more than 7.0wt.% within about 200 DEG C of several seconds, there is good middle low temperature solid-state H_2-producing properties.
The present invention has the following advantages:
(1) preparation method used only at room temperature need utilize a simple step mechanical ball milling technology, hydroborate nano particle can be evenly distributed in the surface of fluorographite, to prepare the nanocomposite hydrogen storage material of high dispersive particle, preparation process can make the particle size of hydroborate be reduced to below 100nm, and that significantly improves this hydroborate system thus puts hydrogen thermomechanical property.
(2) compared with hydroborate modification technology, composite hydrogen storage material prepared by the present invention is without the need to mixing specific catalyzer, C-F functional group in fluorographite used with borohydride solid material, certain interaction can occur makes it be attached to graphite surface equably, and C-F functional group can effectively limit growing up further of hydroborate nano particle, the particle size of hydroborate is made to remain on below 100nm.
(3) this composite hydrogen storage material has good middle low temperature hydrogen discharging performance, simultaneously because graphite self has the hydrogen desorption kinetics performance that good thermal conductivity can improve nanocomposite hydrogen storage material effectively, this composite hydrogen storage material can release at about 200 DEG C the pure hydrogen being up to more than 7.0wt.% fast, not containing other foreign gas.
(4) fluorographite preparation used is simple, and raw materials cost is low, is applicable to large-scale development application.Prepared composite hydrogen storage material can be applicable to small mobile phones, the fields such as the hydrogen source hydrogen of laptop and independent galvanic pile system.
Accompanying drawing explanation
Fig. 1 is LiBH in embodiment 1
4(a), FGi (b), LiBH
4the XRD figure spectrum of/40FGi ball milling 2h matrix material (c).
Fig. 2 a is LiBH in embodiment 1
4the SEM collection of illustrative plates of (a).
Fig. 2 b is the SEM collection of illustrative plates of FGi (b) in embodiment 1.
Fig. 2 c is LiBH in embodiment 1
4the SEM collection of illustrative plates of/40FGi ball milling 2h matrix material (c).
Fig. 3 is LiBH in embodiment 2
4(a), LiBH
4/ 50FGi ball milling 10h matrix material (b) with 5 DEG C/min of temperature rise rates from room temperature to the Hydrogen desorption isotherms of 200 DEG C.
Fig. 4 is LiBH in embodiment 2
4/ 50FGi ball milling 10h matrix material with 5 DEG C/min of temperature rise rates from room temperature to the mass spectrometry profile of 500 DEG C.(I) hydrogen; (II) diborane; (III) fluorine gas; (IV) hydrogen fluoride.
Fig. 5 is LiBH
4(a), LiBH in embodiment 3
4/ 30FGi ball milling 2h matrix material (b), LiBH in embodiment 2
4/ 50FGi ball milling 10h matrix material (c) with 5 DEG C/min of temperature rise rates from room temperature to the Hydrogen desorption isotherms comparison diagram of 200 DEG C.
Fig. 6 is NaBH in embodiment 4
4/ 45FGi ball milling 2h matrix material with 5 DEG C/min of temperature rise rates from room temperature to the Hydrogen desorption isotherms of 250 DEG C.
Embodiment
Hydroborate provided by the present invention/fluorographite composite hydrogen storage material and preparation method thereof is described in detail below with reference to accompanying drawing.
The hydroborate that the technical program provides/fluorographite composite hydrogen storage material, it comprises hydroborate and fluorographite.This hydroborate is general formula is LiBH
4or NaBH
4alkali metal borohydride in any one, the general formula of this fluorographite is FGi.The per-cent that fluorographite accounts for this hydroborate/fluorographite composite hydrogen storage material oeverall quality is 30% ~ 50%.
Embodiment 1
The first step, prepares fluorographite (general formula: FGi).
Tetrafluoroethylene and carbon black fine powder are cold-pressed into after 5:1 mixing under 12MPa pressure the disk of 10mm diameter; then put into electric tube furnace and logical argon shield, furnace temperature rises to 250 DEG C from room temperature subsequently, and insulation 5h reacts; and furnace cooling, the fluorographite of powdery can be obtained.This fluorographite chemical general formula is FGi.
Second step, prepares hydroborate/fluorographite composite hydrogen storage material.
Test LiBH used
4for commercial material, its purity>=95%.Be the LiBH of 6:4 by mass percent
4under 2.0MPa high-purity hydrogen condition, mechanical ball milling is carried out after evenly mixed with FGi (that is: the per-cent that FGi accounts for this hydroborate/fluorographite composite hydrogen storage material oeverall quality is 40%), Ball-milling Time is 2h, finally prepare hydroborate/fluorographite composite hydrogen storage material, that is: LiBH
4/ 40FGi composite hydrogen storage material.
Fig. 1 is prepared LiBH
4the XRD figure spectrum of/40FGi composite hydrogen storage material.As seen from Figure 1, LiBH
4the principal phase of/40FGi composite hydrogen storage material is still by LiBH
4with FGi two phase composite, and LiBH
4xRD diffraction peak there is obvious broadening, show LiBH in prepared composite hydrogen storage material thus
4grain-size reduce to some extent.
Fig. 2 a is LiBH
4raw-material SEM photo, Fig. 2 b is the raw-material SEM photo of FGi, and Fig. 2 c is the LiBH of preparation
4the SEM photo of/40FGi composite hydrogen storage material.As can be seen from Fig. 2 a-2c, LiBH
4with FGi after composite ball-milling, LiBH
4particle size obviously reduce, its average particle size particle size is 90nm, and LiBH
4nano particle can be evenly distributed in fluorographite on the surface, agglomeration does not occur.And general is without the graphite of fluorine process and LiBH
4carry out compound, all cannot reach and make LiBH
4the effect of homodisperse nano particle is formed at graphite surface.
Embodiment 2
Test LiBH used
4with the raw materials parameter of FGi with embodiment 1, be the LiBH of 5:5 by mass percent
4under 0.5MPa high-purity hydrogen condition, carry out mechanical ball milling after evenly mixed with FGi (that is: the per-cent that FGi accounts for this hydroborate/fluorographite composite hydrogen storage material oeverall quality is 50%), Ball-milling Time is 10h, finally prepares LiBH
4/ 50FGi composite hydrogen storage material, wherein LiBH
4the average particle size particle size of hydroborate is 80nm.
Prepared composite hydrogen storage material all adopts " constant volume-pressure differential method " to measure its hydrogen storage property.It puts hydrogen condition: be heated to 200 DEG C with the temperature rise rate of 5 DEG C/min from 25 DEG C at vacuum condition.In Fig. 3, curve (a) is LiBH
4a (), with 5 DEG C/min of temperature rise rates from room temperature to the Hydrogen desorption isotherms of 200 DEG C, transverse axis is the time (minute), the longitudinal axis is for putting hydrogen capacity (wt%); Curve (b) is LiBH
4/ 50FGi ball milling 10h matrix material (b) is with 5 DEG C/min of temperature rise rates from room temperature to the Hydrogen desorption isotherms of 200 DEG C, and same transverse axis is the time (minute), and the longitudinal axis is for putting hydrogen capacity (wt%); Article 3 line is LiBH
4the temperature variation curve of/50FGi ball milling 10h matrix material (b), transverse axis is the time (minute), and the longitudinal axis is temperature (DEG C).As can be seen from Figure 3, the LiBH of preparation
4/ 50FGi composite hydrogen storage material is put hydrogen process first and can be started to put hydrogen at 100 DEG C, and it 195 DEG C time, a large amount of hydrogen discharge reaction occurs, and can release the hydrogen up to 7.2wt.% within 5 seconds, has very excellent thermomechanical property and hydrogen desorption kinetics characteristic.Fig. 4 is LiBH
4/ 50FGi ball milling 10h matrix material with 5 DEG C/min of temperature rise rates from room temperature to the mass spectrometry profile of 500 DEG C.As can be seen from Figure 4, prepared LiBH
4the gas that/50FGi composite hydrogen storage material is released is pure hydrogen, not containing other any foreign gas.
Embodiment 3
Test LiBH used
4with the raw materials parameter of FGi with embodiment 1, be the LiBH of 7:3 by mass percent
4under 1.0MPa high-purity hydrogen condition, carry out mechanical ball milling after evenly mixed with FGi (that is: the per-cent that FGi accounts for this hydroborate/fluorographite composite hydrogen storage material oeverall quality is 30%), Ball-milling Time is 1h, finally prepares LiBH
4/ 30FGi composite hydrogen storage material, wherein LiBH
4the average particle size particle size of hydroborate is 95nm.
Prepared composite hydrogen storage material all adopts " constant volume-pressure differential method " to measure its hydrogen storage property.It puts hydrogen condition: be heated to 200 DEG C with the temperature rise rate of 5 DEG C/min from 25 DEG C at vacuum condition.Fig. 5 is LiBH
4(a), LiBH
4/ 50FGi ball milling 10h matrix material (b) and LiBH
4the Hydrogen desorption isotherms comparison diagram of/30FGi ball milling 1h matrix material (c) three.In Fig. 5, in the picture of the leftmost side, curve (a) is LiBH
4a (), with 5 DEG C/min of temperature rise rates from room temperature to the Hydrogen desorption isotherms of 200 DEG C, transverse axis is the time (minute), the longitudinal axis is for putting hydrogen capacity (wt%), and another line is LiBH
4the temperature variation curve of (a), transverse axis is the time (minute), and the longitudinal axis is temperature (DEG C); In Fig. 5 intermediate picture, curve (b) is LiBH
4/ 50FGi ball milling 10h matrix material (b) is with 5 DEG C/min of temperature rise rates from room temperature to the Hydrogen desorption isotherms of 200 DEG C, and same transverse axis is the time (minute), and the longitudinal axis is for putting hydrogen capacity (wt%), and another line is LiBH
4the temperature variation curve of/50FGi ball milling 10h matrix material (b), transverse axis is the time (minute), and the longitudinal axis is temperature (DEG C); Curve (c) LiBH in the picture of Fig. 5 rightmost side
4it is the time (minute) that the alternating temperature of/30FGi ball milling 1h matrix material (c) puts the same transverse axis of hydrogen (TPD) curve, the longitudinal axis is for putting hydrogen capacity (wt%), another line is the temperature variation curve of LiBH4/30FGi ball milling 1h matrix material (c), transverse axis is the time (minute), and the longitudinal axis is temperature (DEG C).As can be seen from Figure 5, the LiBH of preparation
4/ 30FGi composite hydrogen storage material is put hydrogen process first and can be started to put hydrogen at 140 DEG C, and it 199 DEG C time, a large amount of hydrogen discharge reaction occurs, and can release the pure hydrogen up to 3.2wt.% within 8 seconds.
Embodiment 4
Test NaBH used
4for commercial material, mass percent, with embodiment 1, is the NaBH of 5.5:4.5 by the raw materials parameter of FGi
4under 2.0MPa high-purity hydrogen condition, carry out mechanical ball milling after evenly mixed with FGi (that is: the per-cent that FGi accounts for this hydroborate/fluorographite composite hydrogen storage material oeverall quality is 45%), Ball-milling Time is 2h, finally prepares NaBH
4/ 45FGi composite hydrogen storage material, wherein NaBH
4the average particle size particle size of hydroborate is 76nm.
Prepared composite hydrogen storage material all adopts " constant volume-pressure differential method " to measure its hydrogen storage property, and it is put hydrogen condition and is: be heated to 250 DEG C with the temperature rise rate of 5 DEG C/min from 25 DEG C at vacuum condition.The curve of Fig. 6 intermediate cam figurate number strong point composition is NaBH
4/ 45FGi ball milling 2h matrix material is with 5 DEG C/min of temperature rise rates from room temperature to the Hydrogen desorption isotherms of 250 DEG C, and transverse axis is the time (minute), and the longitudinal axis is for putting hydrogen capacity (wt%); Another line is NaBH
4the temperature variation curve of/45FGi ball milling 2h matrix material, transverse axis is the time (minute), and the longitudinal axis is temperature (DEG C).As can be seen from Figure 6 215 DEG C time, there is a large amount of hydrogen discharge reaction, NaBH
4/ 45FGi ball milling 2h matrix material 10 can release the pure hydrogen up to 5.0wt.% within second.
Claims (9)
1. a Hydroboron/graphite fluoride nano-composite hydrogen storage material, it is characterized in that: described composite hydrogen storage material comprises hydroborate and fluorographite, wherein fluorographite accounts for the per-cent of described hydroborate/fluorographite composite hydrogen storage material oeverall quality is 40%.
2. Hydroboron/graphite fluoride nano-composite hydrogen storage material as claimed in claim 1, is characterized in that: described hydroborate is LiBH
4or NaBH
4in any one.
3. Hydroboron/graphite fluoride nano-composite hydrogen storage material as claimed in claim 1 or 2, it is characterized in that: the form of described hydroborate is the powder particle of nanoscale, the form of described fluorographite is the powder solid of the lamellar of micro-meter scale, and described nanometer borohydride powder uniform particles is distributed in described fluorographite powder solid on the surface.
4. Hydroboron/graphite fluoride nano-composite hydrogen storage material as claimed in claim 3, is characterized in that: the particle size of described hydroborate is 90nm.
5. the preparation method of Hydroboron/graphite fluoride nano-composite hydrogen storage material as claimed in claim 1, it is characterized in that, it comprises the following steps:
The first step, prepare fluorographite, tetrafluoroethylene and carbon black fine powder are cold-pressed into after 5:1 mixing the disk of 10mm diameter under a certain pressure, then electric tube furnace is put into and logical argon shield, furnace temperature rises to 250 DEG C from room temperature subsequently, be incubated 5h and furnace cooling, the fluorographite of powdery can be obtained;
Second step, preparation Hydroboron/graphite fluoride nano-composite hydrogen storage material, example takes hydroborate and fluorographite in mass ratio, carries out mechanical ball milling after both evenly being mixed under high-purity hydrogen condition.
6. the preparation method of Hydroboron/graphite fluoride nano-composite hydrogen storage material as claimed in claim 5, it is characterized in that, in described second step, described hydroborate is LiBH
4or NaBH
4in any one.
7. the preparation method of Hydroboron/graphite fluoride nano-composite hydrogen storage material as claimed in claim 6, it is characterized in that, the per-cent that fluorographite accounts for described Hydroboron/graphite fluoride nano-composite hydrogen storage material oeverall quality is 40%.
8. the preparation method of the Hydroboron/graphite fluoride nano-composite hydrogen storage material as described in claim 5-7 any one, is characterized in that, Ball-milling Time is 1 ~ 10h, and filling hydrogen protection pressure is 0.5 ~ 2.0MPa.
9. the preparation method of Hydroboron/graphite fluoride nano-composite hydrogen storage material as claimed in claim 8, it is characterized in that, Ball-milling Time is 2h, and filling hydrogen protection pressure is 1.0MPa.
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| CN102718183A (en) * | 2012-07-13 | 2012-10-10 | 常州大学 | High-hydrogen-storage-capacity lithium borohydride/graphene (LiBH4/RGO) composite hydrogen storage material and preparation method thereof |
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| CN102718183A (en) * | 2012-07-13 | 2012-10-10 | 常州大学 | High-hydrogen-storage-capacity lithium borohydride/graphene (LiBH4/RGO) composite hydrogen storage material and preparation method thereof |
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