CN103320668A - Hydrogen-storing alloy used for metal-hydride and high-pressure combined hydrogen storage - Google Patents
Hydrogen-storing alloy used for metal-hydride and high-pressure combined hydrogen storage Download PDFInfo
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- CN103320668A CN103320668A CN2013102185351A CN201310218535A CN103320668A CN 103320668 A CN103320668 A CN 103320668A CN 2013102185351 A CN2013102185351 A CN 2013102185351A CN 201310218535 A CN201310218535 A CN 201310218535A CN 103320668 A CN103320668 A CN 103320668A
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Abstract
The invention provides a hydrogen-storing alloy used for metal-hydride and high-pressure combined hydrogen storage. The alloy has a chemical formula as Ti<x>Cr<y>Fe<z>Mn<2>-y-zB<0.01>, wherein x is not smaller than 1.01 and not larger than 1.08, y is not smaller than 1 and not larger than 1.4, z is not smaller than 0.5 and not larger than 0.7, and the sum of y and z is smaller than 2. The pressure of the 318 K hydrogen-discharging platform of the hydrogen-storing alloy is over 35 MPa, hydrogen-discharging enthalpy change value is lower than 20 kJ/mol H2, and the hydrogen storage capacity is larger than 1.6 wt%. The hydrogen-storing alloy is capable of being activated when absorbing hydrogen for the first time, has the advantages of high hydrogen-discharging platform pressure, low thermal enthalpy value, higher hydrogen storage capacity and easy activation, and is especially suitable for being used as hydrogen storage materials of metal-hydride and high-pressure combined hydrogen storage devices.
Description
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 and deterioration of the ecological environment of petroleum resources, utilizes this clean energy of Hydrogen Energy replaces has become the whole world as the existing energy on basis take fossil oil common recognition.
In the process of the various new purposes of developing hydrogen, the storage mode of hydrogen more and more is subject to people's attention.The storage hydrogen mode of using 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 the solid-state storage hydrogen of metal hydride is higher, the weight hydrogen-storage density is relatively low; And the volume hydrogen-storage density of high-pressure gaseous storage hydrogen is lower, the weight 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 simultaneously higher weight and volume hydrogen-storage density, namely add part metals hydride (hydrogen storage alloy) by arranging in high-pressure gaseous hydrogen storage vessel inside, thereby 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, Japan Toyota Company 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 an important channel that solves in the world efficient storage hydrogen now.
Because existing high-pressure gaseous hydrogen storage vessel has 35 MPa or above storage hydrogen pressure mostly, the hydrogen storage alloy that therefore is used for metal hydride-high pressure Composite hydrogen storage device should have 35 MPa or above height is put hydrogen level ground platform pressure.Simultaneously, because hydrogen storage alloy need to absorb auxiliary heat (putting the hydrogen enthalpy change) when putting hydrogen, (i.e. the low hydrogen enthalpy change value of putting is as less than 20 kJ/mol H therefore require hydrogen storage alloy that metal hydride-the high pressure Composite hydrogen storage device is used should have low heat enthalpy value
2).When metal hydride-high pressure Composite hydrogen storage device is externally put the hydrogen use, hydrogen in the device in the hydrogen storage alloy just can discharge under a small amount of auxiliary heat effect thereupon, and make hydrogen pressure maintain higher scope, can improve like this hydrogen discharging speed and the service efficiency of Composite hydrogen storage device.
In existing different series hydrogen storage alloy, TiCr
2Alloy has the relatively high hydrogen level ground platform pressure of putting, but its effective hydrogen-storage amount (less than 1.2 wt%) on the low side, activation performance is relatively poor, still can not satisfy 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 height is put hydrogen level ground platform pressure, low heat enthalpy value, higher hydrogen storage capability and easily activated that has.
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, 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 that proposes among the present invention can adopt induction melting to prepare, specifically: (purity is: Ti 〉=99% by the pure raw material of simple substance of each component respective quality of design proportion weighing first, Cr 〉=99%, Fe 〉=99%, Mn 〉=99%, B 〉=99%), because the fusing point of Mn is lower, Mn easily volatilizees during melting, so need to additionally add by proportional quantity 3% weight again when preparing burden.Then with raw material in induction furnace with melting under the argon gas atmosphere protection.In order to guarantee the homogeneity of alloy, the alloy cast ingot melting three times of repeatedly overturning.
Compared with prior art, the present invention has following advantage:
318 K of hydrogen storage alloy of the present invention are put hydrogen level ground platform pressure and are reached more than 35 MPa, and it is put hydrogen enthalpy change value and is lower than 20 kJ/mol H
2, hydrogen-storage amount reaches more than 1.6 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 the 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.
Description of drawings
Fig. 1 is Ti among the 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 among the embodiment 1
1.02Cr
1.2Fe
0.6Mn
0.2B
0.01The Van't Hoff rectilinear of alloy shows the relation of putting hydrogen Ping Tai pressure and temperature.
Dotted line is corresponding to 318 K temperature positions among the figure.
Fig. 3 is Ti among the 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 among the embodiment 2
1.01Cr
1.1Fe
0.6Mn
0.3B
0.01The Van't Hoff rectilinear of alloy shows the relation of putting hydrogen level ground platform pressure and temperature.
Dotted line is corresponding to 318 K temperature positions among the figure.
Fig. 5 is Ti among the 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 among the embodiment 3
1.02Cr
1.1Fe
0.6Mn
0.3B
0.01The Van't Hoff rectilinear of alloy shows the relation of putting hydrogen level ground platform pressure and temperature.
Dotted line is corresponding to 318 K temperature positions among the figure.
Fig. 7 is Ti among the embodiment 4
1.03Cr
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. 8 is Ti among the embodiment 4
1.03Cr
1.2Fe
0.6Mn
0.2B
0.01The Van't Hoff rectilinear of alloy shows the relation of putting hydrogen level ground platform pressure and temperature.
Dotted line is corresponding to 318 K temperature positions among the figure.
Embodiment
Below in conjunction with specific embodiment the present invention is further set forth, wherein per-cent all is weight percentage in the following example.
Embodiment 1
Design a kind of hydrogen storage alloy, its chemical formula is Ti
1.02Cr
1.2Fe
0.6Mn
0.2B
0.01, 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 weighed by the add-on that calculates after cleaning and drying, and wherein Mn additionally adds 3% weight again by proportional quantity.Load weighted sample is placed in the water jacketed copper crucible of magnetic levitation stove; be vented to through finding time＜0.13 Pa vacuum tightness after; under 0.1 MPa argon shield, carry out melting; for making homogeneous chemical composition; need stand up the repetition melting three times; make the hydrogen storage alloy ingot, analyze the composition of the alloy make 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.
The hydrogen storage alloy ingot that makes is broken for the reactor of packing into behind the particle of particle diameter below 200 microns, carries out hydrogen storage property and measure.Hydrogen storage alloy is vacuumized 30 minutes first under 400 ℃ of heating conditions, then be filled with high pressure hydrogen, alloy be easy to inhale hydrogen activation (with just begin to inhale hydrogen after hydrogen contacts, and can reach suction hydrogen at 30 minutes saturated), this alloy respectively P-C-T curve under 243 K, 253 K, 263 K temperature is seen 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, under the 263 K temperature to put that hydrogen Ping Tai presses be respectively 5.19 MPa, 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 under 318 K is 36.3 MPa as can be known, it puts hydrogen enthalpy change value is 16.68 kJ/mol H
2
Embodiment 2
The 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 weighed by the add-on that calculates after cleaning and drying, and wherein Mn additionally adds 3% weight again by proportional quantity.Load weighted sample is placed in the water jacketed copper crucible of magnetic levitation stove; be vented to through finding time＜0.13 Pa vacuum tightness after; under 0.1 MPa argon shield, carry out melting; for making alloying constituent even; need stand up the repetition melting three times; make the hydrogen storage alloy ingot, analyze the composition of the alloy make 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.
The hydrogen storage alloy ingot that makes is broken for the reactor of packing into behind the particle of particle diameter below 200 microns, carries out hydrogen storage property and measure.Hydrogen storage alloy is first vacuumized 30 minutes under 400 ℃ of heating conditions, then is filled with high pressure hydrogen, alloy be easy to inhale the hydrogen activation (with just begin to inhale hydrogen after hydrogen contact, and can reach suction hydrogen at 30 minutes saturated).This alloy respectively P-C-T curve under 243 K, 253 K, 263 K temperature is seen 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 under 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 when 318 K is 46.08 MPa as can be known, it puts the hydrogen enthalpy change is 15.76 kJ/mol H
2
Embodiment 3
The 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 weighed by the add-on that calculates after cleaning and drying, and wherein Mn additionally adds 3% weight again by proportional quantity.Load weighted sample is placed in the water jacketed copper crucible of magnetic levitation stove; be vented to through finding time＜0.13 Pa vacuum tightness after; under 0.1 MPa argon shield, carry out melting; for making alloying constituent even; need stand up the repetition melting three times; make the hydrogen storage alloy ingot, analyze the composition of the alloy make 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.
The hydrogen storage alloy ingot that makes is broken for the reactor of packing into behind the particle of particle diameter below 200 microns, carries out hydrogen storage property and measure.Hydrogen storage alloy is vacuumized 30 minutes first under 400 ℃ of heating conditions, then be filled with high pressure hydrogen, alloy be easy to inhale hydrogen activation (with just begin to inhale hydrogen after hydrogen contacts, and can reach suction hydrogen at 30 minutes saturated), this alloy respectively P-C-T curve under 243 K, 253 K, 263 K temperature is seen Fig. 5.As can be seen from Figure 5, this hydrogen storage alloy maximum storage hydrogen quantity reaches 1.72 wt%, under 243 K, 253 K, 263 K temperature to put that hydrogen Ping Tai presses be respectively 6.12 MPa, 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, as can be known this alloy when 318K to put hydrogen level ground platform pressure be 41.3 MPa, putting the hydrogen enthalpy change is 16.24 kJ/mol H
2
Embodiment 4
The design chemical formula is Ti
1.03Cr
1.2Fe
0.6Mn
0.2B
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 weighed by the add-on that calculates after cleaning and drying, and wherein Mn additionally adds 3% weight again by proportional quantity.Load weighted sample is placed in the water jacketed copper crucible of magnetic levitation stove; be vented to through finding time＜0.13 Pa vacuum tightness after; under 0.1 MPa argon shield, carry out melting; for making alloying constituent even; need stand up the repetition melting three times; make the hydrogen storage alloy ingot, analyze the composition of the alloy make and the hydrogen storage alloy chemical formula Ti of design through plasma emission spectrometer (ICP)
1.03Cr
1.2Fe
0.6Mn
0.2B
0.01Be consistent.
The hydrogen storage alloy ingot that makes is broken for the reactor of packing into behind the particle of particle diameter below 200 microns, carries out hydrogen storage property and measure.Hydrogen storage alloy is vacuumized 30 minutes first under 400 ℃ of heating conditions, then be filled with high pressure hydrogen, alloy be easy to inhale hydrogen activation (with just begin to inhale hydrogen after hydrogen contacts, and can reach suction hydrogen at 30 minutes saturated), this alloy respectively P-C-T curve under 243 K, 253 K, 263 K temperature is seen 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,, under 253 K, the 263 K temperature to put that hydrogen Ping Tai presses be respectively 5.05 MPa, 7.01 MPa, 9.54 MPa.Fig. 8 is Ti
1.03Cr
1.2Fe
0.6Mn
0.2B
0.01The Van't Hoff rectilinear of alloy, as can be known this alloy when 318K to put hydrogen level ground platform pressure be 36.1 MPa, putting the hydrogen enthalpy change is 16.98 kJ/mol H
2
Table 1 be the hydrogen storage material that makes among above-described embodiment 1-4 through the analytical results of plasma emission spectrometer (ICP), 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 to limit the present invention; any those skilled in the art without departing from the spirit and scope of the present invention; can utilize method and the technology contents of above-mentioned announcement that technical solution of the present invention is made possible change and modification; therefore; every content that does not break away from technical solution of the present invention; to any simple modification, equivalent variations and modification that above embodiment does, all belong to the protection domain of technical solution of the present invention according to technical spirit of the present invention.
Claims (3)
1. a hydrogen storage alloy that is used for metal hydride-high pressure composite hydrogen occluding 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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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN111705253A (en) * | 2020-06-24 | 2020-09-25 | 上海福绥宇海新能源有限公司 | Hydrogen storage alloy suitable for high pressure-metal hydride hydrogen storage and preparation method thereof |
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2013
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN111705253A (en) * | 2020-06-24 | 2020-09-25 | 上海福绥宇海新能源有限公司 | Hydrogen storage alloy suitable for high pressure-metal hydride hydrogen storage and preparation method thereof |
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