CN103320668B - For the hydrogen storage alloy of metal hydride-high pressure composite hydrogen occluding - Google Patents

For the hydrogen storage alloy of metal hydride-high pressure composite hydrogen occluding Download PDF

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CN103320668B
CN103320668B CN201310218535.1A CN201310218535A CN103320668B CN 103320668 B CN103320668 B CN 103320668B CN 201310218535 A CN201310218535 A CN 201310218535A CN 103320668 B CN103320668 B CN 103320668B
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hydrogen
hydrogen storage
alloy
storage alloy
metal hydride
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CN103320668A (en
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陈立新
陈志文
肖学章
范修林
刘朗夏
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Zhejiang University ZJU
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Abstract

The invention provides a kind of hydrogen storage alloy for metal hydride-high pressure composite hydrogen occluding, described alloy has Ti xcr yfe zmn 2-y-zb 0.01chemical general formula, wherein: 1.01≤x≤1.08,1≤y≤1.4,0.5≤z≤0.7, y+z < 2.318 of this hydrogen storage alloy? does K put hydrogen level ground platform pressure more than 35? does MPa, put hydrogen enthalpy change value lower than 20? kJ/mol? H 2does hydrogen storage capability reach 1.6? more than wt%, and inhale hydrogen first just can activate, there is height and put the advantages such as hydrogen level ground platform pressure, low heat enthalpy value, higher hydrogen storage capability and easy activation, be specially adapted to the hydrogen storage material being used as metal hydride-high pressure Composite hydrogen storage device.

Description

For the hydrogen storage alloy of metal hydride-high pressure composite hydrogen occluding
Technical field
The present invention relates to a kind of alloy, particularly a kind of hydrogen storage alloy for metal hydride-high pressure composite hydrogen occluding.
Background technology
The energy is the source of human development, faces the dual-pressure of the day by day deficient of petroleum resources and the deterioration of the ecological environment, utilizes this clean energy of Hydrogen Energy existing energy replaced based on fossil oil to become the common recognition in the whole world.
In the process of the various novelty teabag of exploitation hydrogen, the storage mode of hydrogen is more and more subject to people's attention.The storage hydrogen mode used at present comprises the solid-state storage hydrogen of metal hydride, high-pressure gaseous storage hydrogen and low temperature liquid Chu Qing etc.Wherein, the volume hydrogen-storage density of metal hydride solid-state storage hydrogen is higher, gravimetric hydrogen storage density is relatively low; And the volume hydrogen-storage density of high-pressure gaseous storage hydrogen is lower, gravimetric hydrogen storage density is relatively high.If both are effectively combined, adopt the technology of metal hydride-high pressure composite hydrogen occluding, just can realize higher weight and volume hydrogen-storage density simultaneously, namely by arranging adding portion metal hydride (hydrogen storage alloy) in high-pressure gaseous hydrogen storage vessel inside, thus improve volume hydrogen-storage density (the N. Takeichi of high-pressure hydrogen storage, H. Senoh, T. Yokota, H. Tsuruta, K. Hamada, H.T. Takeshita, H. Tanaka, T. Kiyobayashi, T. Takano, N. Kuriyama. Int. J. Hydrogen Energy, 2003, 28 (10): 1121-1129).At present, Toyota Company of Japan is at trial-production novel metal hydride-high pressure Composite hydrogen storage device, General Motors Overseas Corporation is also carrying out the research of this respect, and development of new metal hydride-high pressure Composite hydrogen storage device is the current important channel solving efficient storage hydrogen in the world.
Because existing high-pressure gaseous hydrogen storage vessel has the storage hydrogen pressure of 35 MPa or more mostly, the height that therefore should have 35 MPa or more for the hydrogen storage alloy of metal hydride-high pressure Composite hydrogen storage device puts hydrogen level ground platform pressure.Meanwhile, because hydrogen storage alloy needs when putting hydrogen to absorb auxiliary heat (putting hydrogen enthalpy change), therefore require that the hydrogen storage alloy of metal hydride-high pressure Composite hydrogen storage device should have low heat enthalpy value and (namely lowly put hydrogen enthalpy change value, as being less than 20 kJ/mol H 2).When metal hydride-high pressure Composite hydrogen storage device externally puts hydrogen use, hydrogen in device in hydrogen storage alloy just can discharge under a small amount of auxiliary heat effect thereupon, and make hydrogen pressure maintain higher scope, hydrogen discharging speed and the service efficiency of Composite hydrogen storage device can be improved like this.
In existing different series hydrogen storage alloy, TiCr 2alloy has relatively high puts hydrogen level ground platform pressure, but its effective hydrogen-storage amount (being less than 1.2 wt%) on the low side, activation performance is poor, still can not meet the application requiring of metal hydride-high pressure composite hydrogen occluding container.
Summary of the invention
The object of the present invention is to provide a kind of hydrogen storage alloy that there is height and put hydrogen level ground platform pressure, low heat enthalpy value, higher hydrogen storage capability and easily activate.
For achieving the above object, the present invention takes following technical scheme:
High level ground provided by the present invention platform pressure hydrogen storage alloy, has following chemical general formula: Ti xcr yfe zmn 2-y-zb 0.01,
Wherein the scope of x is: 1.01≤x≤1.08, and wherein the scope of y is: 1≤y≤1.4, and wherein the scope of z is: 0.5≤z≤0.7,
And y+z < 2.
Preferably, 1.01≤x≤1.03,1.05≤y≤1.2,0.55≤z≤0.65.
Preferred, 1.02≤x≤1.03,1.1≤y≤1.2,0.6≤z≤0.65.
The hydrogen storage alloy proposed in the present invention can adopt induction melting to prepare, specifically: (purity is: Ti >=99% first to weigh the pure raw material of simple substance of each component respective quality by design proportion, Cr >=99%, Fe >=99%, Mn >=99%, B >=99%), because the fusing point of Mn is lower, easily volatilize during melting, so Mn needs the weight additionally adding 3% by proportional quantity again during batching.Then melting under raw material being protected by argon gas atmosphere in induction furnace.In order to ensure the homogeneity of alloy, alloy cast ingot overturns melting three times repeatedly.
Compared with prior art, tool of the present invention has the following advantages:
318 K of hydrogen storage alloy of the present invention are put hydrogen level ground platform pressure and are reached 35 more than MPa, and it puts hydrogen enthalpy change value lower than 20 kJ/mol H 2, hydrogen-storage amount reaches 1.6 more than wt%.
Alloy is very easy to activation simultaneously, is specially adapted to the hydrogen storage material as metal hydride-high pressure Composite hydrogen storage device.
Further, in preferred embodiment, hydrogen storage alloy hydrogen-storage amount of the present invention reaches 1.79 wt%.
In sum, this hydrogen storage alloy has the advantages that height is put hydrogen level ground platform pressure, low heat enthalpy value, higher hydrogen storage capability and easily activated, and has good application prospect in metal hydride-high pressure Composite hydrogen storage device field.
Accompanying drawing explanation
Fig. 1 is Ti in embodiment 1 1.02cr 1.2fe 0.6mn 0.2b 0.01p-C-T (Pressure-Composition-temperature) graphic representation of alloy when 243 K, 253 K, 263 K.
Fig. 2 is Ti in embodiment 1 1.02cr 1.2fe 0.6mn 0.2b 0.01the Van't Hoff rectilinear of alloy, the relation of hydrogen Ping Tai pressure and temperature is put in display.
In figure, dotted line corresponds to 318 K temperature positions.
Fig. 3 is Ti in embodiment 2 1.01cr 1.1fe 0.6mn 0.3b 0.01p-C-T (Pressure-Composition-temperature) graphic representation of alloy when 243 K, 253 K, 263 K.
Fig. 4 is Ti in embodiment 2 1.01cr 1.1fe 0.6mn 0.3b 0.01the Van't Hoff rectilinear of alloy, the relation of hydrogen level ground platform pressure and temperature is put in display.
In figure, dotted line corresponds to 318 K temperature positions.
Fig. 5 is Ti in embodiment 3 1.02cr 1.1fe 0.6mn 0.3b 0.01p-C-T (Pressure-Composition-temperature) graphic representation of alloy when 243 K, 253 K, 263 K.
Fig. 6 is Ti in embodiment 3 1.02cr 1.1fe 0.6mn 0.3b 0.01the Van't Hoff rectilinear of alloy, the relation of hydrogen level ground platform pressure and temperature is put in display.
In figure, dotted line corresponds to 318 K temperature positions.
Fig. 7 is Ti in embodiment 4 1.03cr 1.1fe 0.6mn 0.3b 0.01p-C-T (Pressure-Composition-temperature) graphic representation of alloy when 243 K, 253 K, 263 K.
Fig. 8 is Ti in embodiment 4 1.03cr 1.1fe 0.6mn 0.3b 0.01the Van't Hoff rectilinear of alloy, the relation of hydrogen level ground platform pressure and temperature is put in display.
In figure, dotted line corresponds to 318 K temperature positions.
Embodiment
Be further elaborated the present invention below in conjunction with specific embodiment, wherein in the following example, per-cent is all weight percentage.
embodiment 1
Design a kind of hydrogen storage alloy, its chemical formula is Ti 1.02cr 1.2fe 0.6mn 0.2b 0.01, the add-on of each raw material is calculated by chemical formula.The material purity of Ti, Cr, Fe, Mn, B all reaches more than 99%.Above-mentioned starting material are through cleaning and weighing by the add-on calculated after drying, and wherein Mn additionally adds the weight of 3% again by proportional quantity.Load weighted sample is placed in the water jacketed copper crucible of magnetic levitation stove; be vented to < 0.13 Pa vacuum tightness through finding time after; melting is carried out under 0.1 MPa argon shield; for making uniform composition; repetition melting need be stood up three times; obtained hydrogen storage alloy ingot, analyzes the obtained composition of alloy and the hydrogen storage alloy chemical formula Ti of design through plasma emission spectrometer (ICP) 1.02cr 1.2fe 0.6mn 0.2b 0.01be consistent.
Load reactor after obtained hydrogen storage alloy ingot being broken for the particle of particle diameter less than 200 microns, carry out hydrogen storage property mensuration.Hydrogen storage alloy is first vacuumized 30 minutes under 400 DEG C of heating conditions, then high pressure hydrogen is filled with, alloy is easy to inhale hydrogen activation (just to start after contacting with hydrogen to inhale hydrogen, and can reach suction hydrogen at 30 minutes saturated), the P-C-T curve of this alloy respectively at 243 K, 253 K, 263 K temperature is shown in Fig. 1.As can be seen from Figure 1, the maximum storage hydrogen quantity of this hydrogen storage alloy reaches 1.78 wt%, at 243 K, 253 K, at 263 K temperature put hydrogen Ping Tai pressure be 5.19 MPa respectively, 7.19 MPa, 9.73 MPa.Fig. 2 is Ti 1.02cr 1.2fe 0.6mn 0.2b 0.01the Van't Hoff rectilinear of alloy, the Ping Tai pressure of this alloy known under 318 K is 36.3 MPa, and it puts hydrogen enthalpy change value is 16.68 kJ/mol H 2.
embodiment 2
Design chemical formula is Ti 1.01cr 1.1fe 0.6mn 0.3b 0.01hydrogen storage alloy, calculate the add-on of each raw material by chemical formula.The material purity of Ti, Cr, Fe, Mn, B all reaches more than 99%.Above-mentioned starting material are through cleaning and weighing by the add-on calculated after drying, and wherein Mn additionally adds the weight of 3% again by proportional quantity.Load weighted sample is placed in the water jacketed copper crucible of magnetic levitation stove; be vented to < 0.13 Pa vacuum tightness through finding time after; melting is carried out under 0.1 MPa argon shield; for making alloying constituent even; repetition melting need be stood up three times; obtained hydrogen storage alloy ingot, analyzes the obtained composition of alloy and the hydrogen storage alloy chemical formula Ti of design through plasma emission spectrometer (ICP) 1.01cr 1.1fe 0.6mn 0.3b 0.01be consistent.
Load reactor after obtained hydrogen storage alloy ingot being broken for the particle of particle diameter less than 200 microns, carry out hydrogen storage property mensuration.Hydrogen storage alloy is first vacuumized 30 minutes under 400 DEG C of heating conditions, is then filled with high pressure hydrogen, alloy is easy to inhale hydrogen activation (just start after contacting with hydrogen to inhale hydrogen, and can reach suction hydrogen at 30 minutes saturated).The P-C-T curve of this alloy respectively at 243 K, 253 K, 263 K temperature is shown in Fig. 3.As can be seen from Figure 3, the maximum storage hydrogen quantity of this hydrogen storage alloy reaches 1.69 wt%, and the hydrogen Ping Tai pressure of putting at 243 K, 253 K, 263 K temperature is respectively 7.3 MPa, 10.02 MPa, 13.21 MPa.Fig. 4 is Ti 1.01cr 1.1fe 0.6mn 0.3b 0.01the Van't Hoff rectilinear of alloy, the put hydrogen level ground platform pressure of this alloy known when 318 K is 46.08 MPa, and it puts hydrogen enthalpy change is 15.76 kJ/mol H 2.
embodiment 3
Design chemical formula is Ti 1.02cr 1.1fe 0.6mn 0.3b 0.01hydrogen storage alloy, calculate the add-on of each raw material by chemical formula.The material purity of Ti, Cr, Fe, Mn, B all reaches more than 99%.Above-mentioned starting material are through cleaning and weighing by the add-on calculated after drying, and wherein Mn additionally adds the weight of 3% again by proportional quantity.Load weighted sample is placed in the water jacketed copper crucible of magnetic levitation stove; be vented to < 0.13 Pa vacuum tightness through finding time after; melting is carried out under 0.1 MPa argon shield; for making alloying constituent even; repetition melting need be stood up three times; obtained hydrogen storage alloy ingot, analyzes the obtained composition of alloy and the hydrogen storage alloy chemical formula Ti of design through plasma emission spectrometer (ICP) 1.02cr 1.1fe 0.6mn 0.3b 0.01be consistent.
Load reactor after obtained hydrogen storage alloy ingot being broken for the particle of particle diameter less than 200 microns, carry out hydrogen storage property mensuration.Hydrogen storage alloy is first vacuumized 30 minutes under 400 DEG C of heating conditions, then high pressure hydrogen is filled with, alloy is easy to inhale hydrogen activation (just to start after contacting with hydrogen to inhale hydrogen, and can reach suction hydrogen at 30 minutes saturated), the P-C-T curve of this alloy respectively at 243 K, 253 K, 263 K temperature is shown in Fig. 5.As can be seen from Figure 5, this hydrogen storage alloy maximum storage hydrogen quantity reaches 1.72 wt%, at 243 K, 253 K, 263 K temperature put hydrogen Ping Tai pressure be 6.12 MPa respectively, 8.56 MPa, 11.57 MPa.Fig. 6 is Ti 1.02cr 1.1fe 0.6mn 0.3b 0.01the Van't Hoff rectilinear of alloy, this alloy known when 318K to put hydrogen level ground platform pressure be 41.3 MPa, putting hydrogen enthalpy change is 16.24 kJ/mol H 2.
embodiment 4
Design chemical formula is Ti 1.03cr 1.1fe 0.6mn 0.3b 0.01hydrogen storage alloy, calculate the add-on of each raw material by chemical formula.The material purity of Ti, Cr, Fe, Mn, B all reaches more than 99%.Above-mentioned starting material are through cleaning and weighing by the add-on calculated after drying, and wherein Mn additionally adds the weight of 3% again by proportional quantity.Load weighted sample is placed in the water jacketed copper crucible of magnetic levitation stove; be vented to < 0.13 Pa vacuum tightness through finding time after; melting is carried out under 0.1 MPa argon shield; for making alloying constituent even; repetition melting need be stood up three times; obtained hydrogen storage alloy ingot, analyzes the obtained composition of alloy and the hydrogen storage alloy chemical formula Ti of design through plasma emission spectrometer (ICP) 1.03cr 1.1fe 0.6mn 0.3b 0.01be consistent.
Load reactor after obtained hydrogen storage alloy ingot being broken for the particle of particle diameter less than 200 microns, carry out hydrogen storage property mensuration.Hydrogen storage alloy is first vacuumized 30 minutes under 400 DEG C of heating conditions, then high pressure hydrogen is filled with, alloy is easy to inhale hydrogen activation (just to start after contacting with hydrogen to inhale hydrogen, and can reach suction hydrogen at 30 minutes saturated), the P-C-T curve of this alloy respectively at 243 K, 253 K, 263 K temperature is shown in Fig. 7.As can be seen from Figure 7, the maximum storage hydrogen quantity of this hydrogen storage alloy reaches 1.79 wt.%, 243 K, at 253 K, 263 K temperature put hydrogen Ping Tai pressure be 5.05 MPa respectively, 7.01 MPa, 9.54 MPa.Fig. 8 is Ti 1.03cr 1.1fe 0.6mn 0.3b 0.01the Van't Hoff rectilinear of alloy, this alloy known when 318K to put hydrogen level ground platform pressure be 36.1 MPa, putting hydrogen enthalpy change is 16.98 kJ/mol H 2.
Table 1 is hydrogen storage material obtained in above-described embodiment 1-4 analytical results through plasma emission spectrometer (ICP), and particular content is as shown in table 1.
Table 1 hydrogen storage material plasma emission spectrometer (ICP) analytical results
Although the present invention with preferred embodiment openly as above; but it is not for limiting the present invention; any those skilled in the art without departing from the spirit and scope of the present invention; the Method and Technology content of above-mentioned announcement can be utilized to make possible variation and amendment to technical solution of the present invention; therefore; every content not departing from technical solution of the present invention; the any simple modification done above embodiment according to technical spirit of the present invention, equivalent variations and modification, all belong to the protection domain of technical solution of the present invention.

Claims (3)

1. for a hydrogen storage alloy for metal hydride-high pressure composite hydrogen occluding, it is characterized in that, described alloy has Ti xcr yfe zmn 2-y-zb 0.01chemical general formula, wherein: 1.01≤x≤1.08,1≤y≤1.4,0.5≤z≤0.7, y+z < 2.
2. hydrogen storage alloy according to claim 1, is characterized in that,
1.01≤x≤1.03，
1.05≤y≤1.2，
0.55≤z≤0.65。
3. hydrogen storage alloy according to claim 1, is characterized in that: 1.02≤x≤1.03,1.1≤y≤1.2,0.6≤z≤0.65.
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CN103695754A (en) * 2013-12-18 2014-04-02 浙江大学 Easy-to-activate high-plateau pressure hydrogen storage alloy and preparation method thereof
CN108977715A (en) * 2017-05-31 2018-12-11 全球能源互联网研究院 It is a kind of suitable for high pressure-hydride hydrogen-storing hydrogen bearing alloy and preparation method thereof
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