CN1091157C - Ferro-titanium base hydrogen storage alloy - Google Patents
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- 239000001257 hydrogen Substances 0.000 title claims abstract description 82
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 82
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 59
- 239000000956 alloy Substances 0.000 title claims abstract description 59
- 238000003860 storage Methods 0.000 title claims abstract description 40
- 229910001200 Ferrotitanium Inorganic materials 0.000 title claims description 6
- 239000000126 substance Substances 0.000 claims abstract description 11
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 5
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 5
- 229910052779 Neodymium Inorganic materials 0.000 claims abstract description 3
- 229910052777 Praseodymium Inorganic materials 0.000 claims abstract description 3
- 229910052772 Samarium Inorganic materials 0.000 claims abstract description 3
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 3
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 3
- 239000010936 titanium Substances 0.000 claims description 36
- 229910052751 metal Inorganic materials 0.000 claims description 12
- 239000002184 metal Substances 0.000 claims description 9
- 150000002431 hydrogen Chemical class 0.000 claims description 7
- 229910001122 Mischmetal Inorganic materials 0.000 claims description 2
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical group [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 2
- 239000002828 fuel tank Substances 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 4
- 238000005984 hydrogenation reaction Methods 0.000 abstract description 4
- 229910052791 calcium Inorganic materials 0.000 abstract description 3
- 230000003213 activating effect Effects 0.000 abstract description 2
- 229910011212 Ti—Fe Inorganic materials 0.000 abstract 2
- 229910010340 TiFe Inorganic materials 0.000 description 34
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 23
- 230000004913 activation Effects 0.000 description 14
- 150000004678 hydrides Chemical class 0.000 description 9
- 229910052719 titanium Inorganic materials 0.000 description 9
- 238000000034 method Methods 0.000 description 8
- 229910052742 iron Inorganic materials 0.000 description 7
- 239000006104 solid solution Substances 0.000 description 5
- 239000011232 storage material Substances 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 239000011575 calcium Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 229920006395 saturated elastomer Polymers 0.000 description 4
- 239000007858 starting material Substances 0.000 description 4
- 238000005275 alloying Methods 0.000 description 3
- 229910002056 binary alloy Inorganic materials 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910052761 rare earth metal Inorganic materials 0.000 description 3
- YZCKVEUIGOORGS-IGMARMGPSA-N Protium Chemical compound [1H] YZCKVEUIGOORGS-IGMARMGPSA-N 0.000 description 2
- 241000720974 Protium Species 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000011534 incubation Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 230000002441 reversible effect Effects 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 229910000882 Ca alloy Inorganic materials 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- -1 Hydride Chemical compound 0.000 description 1
- 240000003936 Plumbago auriculata Species 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000004378 air conditioning Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
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- 229910052804 chromium Inorganic materials 0.000 description 1
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- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
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- 230000006872 improvement Effects 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052752 metalloid Inorganic materials 0.000 description 1
- 150000002738 metalloids Chemical class 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 230000007420 reactivation Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000010583 slow cooling Methods 0.000 description 1
- 229910002058 ternary alloy Inorganic materials 0.000 description 1
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- 229910000687 transition metal group alloy Inorganic materials 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Abstract
The present invention relates to a titanium-ferrum-base hydrogen storage alloy. The present invention is characterized in that the chemical formula is Ti<1+x>Fe+ywt%M, wherein 0<x<0.3, 0<y<8, and M is one of Mm, Ml, La, Ce, Pr, Nd, Sm, Li, Mg, Ca, etc. The present invention is a titanium-ferrum-base hydrogen storage alloy without Ti-Fe stoichiometric proportion, special Ti-Fe activating treatment is not needed, once hydrogenation can be carried out at room temperature and under the hydrogen pressure of 4.0MPa, and the hydrogen storage capacity reaches more than 1.7 wt%; the present invention has the advantages of large hydrogen storage capacity, light weight, low cost, convenient operation, etc., is particularly suitable for being applied to movable or portable hydrogen storage devices, such as hydrogen purifiers, hydrogen fuel tanks, etc.
Description
The present invention relates to a kind of metal matrix alloy, particularly a kind of non-stoichiometric ferro-titanium base hydrogen storage alloy.
Because the resource and environment problem, human from fossil oil progressively then utilize renewable energy sources such as sun power, Hydrogen Energy, will be the inexorable trend of energy field development from now on.Hydrogen storage material be energy storage material be again functional materials, except the storage and conveying that are applied to hydrogen, the purification and the fields such as compression, electrochemistry (secondary cell), energy transformation (accumulation of heat, refrigeration, air-conditioning, heating, hot machine etc.) and chemical industry catalysis of also widening hydrogen.Have characteristics such as safe, flexible and effective when especially hydrogen storage material is as Hydrogen Energy storage transmission carrier, the hydrogen fuel cell of current booming zero release and the application of hydrogen-burning automobile fuel tank are had wide prospect.
So far, the hydrogen storage material with actual application value mainly is some alloys of reversible hydrogen adsorption and desorption at room temperature, as AB
5Rare earth system and the AB type and the AB of type
2The titanium alloy of type.If be applied to hydrogen storing or make the hydrogen storage alloy of fuel tank. put the hydrogen operation except that should be able at room temperature inhaling, high hydrogen storage capability, suitable equilibrium pressure also will be arranged, be easy to the activatory fundamental property.The TiFe alloy is typical case's representative of AB type hydrogen storage alloy, and TiFe alloy and H-H reaction generate TiFeH
1.04Hydride (β phase) and TiFeH
1.95Two platforms appear in hydride (γ phase) on the P-C-T curve, β distinguishes low pressure platform and high voltage platform on the corresponding curve mutually with γ mutually.The γ of high hydrogen storage capability obtains when the back continues to increase hydrogen pressure mutually at formation β.GIFeH
1.95Be meant the maximum saturation hydride under 0 ℃ and the 6.5MPa.The hydrogen-storage amount of extrapolating according to this formula was 1.8% (referring to weight percent, down together), apparently higher than the general rare earth (AB of system
5Type) 1.4% of alloy.Except that high this advantage of hydrogen storage capability, the decomposition pressure of TiFe alloy hydride is several normal atmosphere, and Fe and Ti are abundant at the occurring in nature reserves, and low price helps industrial scale applications.
But also there are some fatal shortcomings in the TiFe alloy as hydrogen storage material, and wherein topmost is exactly to be difficult to activation, and can't at room temperature carry out the reversible hydrogen adsorption and desorption operation without the alloy that activation treatment is crossed.GIFe reactivation process according to document [1] report is as follows: the TiFe alloy is broken into pack into after the particulate state reactor sealing, exhaust, reactor is heated to 400 ℃-450 ℃, continue exhaust simultaneously in heating, fill hydrogen to 0.7MPa to reactor afterwards, final vacuum half an hour and slow cooling are to room temperature, thereafter fill hydrogen again to 6.5MPa, still fail to inhale hydrogen, then repeat above-mentioned activation act until activation fully as TiFe alloy in 15 minutes.Practice shows that above-mentioned activating treatment process will carry out repeatedly could beginning to inhale hydrogen usually repeatedly, and will just can reach maximum hydrogen after putting the hydrogen circulation through inhaling for surplus ten times, and time-consuming and manufacturing cost increases.
So far, the main method of improving TiFe alloy activation performance is by alloying, and for example with Ti or Fe in the partly alternative TiFe alloy of transition metals such as Cr, Mn, Zr, Ni, Co, Nb, Al, V, forming with TiFe is the ternary or the multicomponent alloy of base.Wherein, with Mn be the TiFe that substitute element is formed
1-xMn
x, x=0.1 in the formula～0.3, alloy property is best, referring to document [2].Though this ternary alloy system by stoichiometry design can be under room temperature and 4～5MPa hydrogen pressure, but maximum storage hydrogen quantity is more much lower than TiFe binary alloy less than 1.6%.Also propose partly to substitute other a series of alloy TiFe of Ti in the document with Mn
1-xMn
x, x=0.1 in the formula～0.3, but its hydrogen-storage amount reduces too many (less than 1%), does not more have actual application value.The other method of improving TiFe alloy activation performance that proposes is to make the Ti content in the TiFe alloy excessive, constitutes the nonstoichiometric composition alloy, as Ti
1+xFe, X is respectively 0.1,0.2 in the formula, 0.3,0.4,0.5, referring to document [3], studies show that this method can be improved the alloy activation performance, it is big more to improve activation effect if the X amount is high more, but because the high more Ti of X nonstoichiometry more, β-the Ti that occurs in the alloy structure is many more mutually, and the hydride of desorb hydrogen is not many more under the formation normal temperature after its hydrogenation, so hydrogen storage capability reduces big more.According to document [1], as being divided into 49.2%Ti and 50.5%Fe (is equivalent to chemical formula Ti
1.14Fe) time, the solid solution hydrogen capacity of desorb hydrogen does not account for 15% of (on the P-C-T curve) saturated hydrogen-storage amount; And further to be increased to composition be 63.2%Ti as Ti, and 36.7%Fe (quite is stored in chemical formula Ti
2Fe) time, the solid solution hydrogen capacity of desorb hydrogen does not account for 56%, and is too big with former TiFe binary alloy gap on the hydrogen storage capability.Document [4] has proposed the method for the another kind of TiFe of improvement alloy activation performance, is to add 4.5% norium Mm in the TiFe alloy, promptly constitutes the TiFe+4.5%Mm alloy.Think that this new alloy puts the hydrogen operation and just can activate fully through inhaling for three times under room temperature (27.1 ℃) and 6.0MPa.The hydrogen storage capability that this alloy P-C-T opisometer that provides according to document is calculated is about 1.56%, and is obviously also low much than typical TiFe alloy.
The object of the present invention is to provide a kind of ferro-titanium base hydrogen storage alloy that needn't special activation treatment, this alloy storage Hydrogen Energy is the level that can keep former TiFe binary alloy, can depress a hydrogenation in room temperature with than low hydrogen, therefore concrete big, in light weight, the low cost and other advantages of hydrogen-storage amount is particularly suitable for aspects such as portable or portable storage hydrogen device such as hydrogen purification device and fuel tank and uses.
A kind of ferrotianium hydrogen storage alloy, the chemical formula that it is characterized in that this hydrogen storage alloy is Ti
1+xFe+yM, 0＜x in the formula＜0.3, y is for being not more than Ti
1+x8% of Fe weight, M is cerium-rich mischmetal metal M m, perhaps lanthanum rich norium M1, perhaps a kind of among metal La, Ce, Pr, Nd, Sm, Li, Mg, the Ca.In the alloy system of the present invention, titanium content has surpassed the stoichiometric ratio scope of the Ti in the typical TiFe alloy, is added with the metallic element M of certain percentage ratio again, this metalloid M neither solid solution in Ti also not solid solution in Fe, certainly also not solid solution but is easy to inhale hydrogen evolution hydride in TiFe.Alloy of the present invention needn't carry out the such activation treatment process of TiFe, just begin to inhale hydrogen after the incubation period that only under room temperature (as 25 ℃) and 4.0MPa hydrogen pressure, contacts with hydrogen for the first time surplus several minutes or ten minute, and it is saturated to reach suction hydrogen within tens of minutes, just can inhale afterwards to put the hydrogen application.Studies show that, alloy of the present invention is because the Ti over-stoichiometric is added with easy suction protium again, alloy structure has not been single TiFe phase structure, but by β-Ti and the netted eutectic structure that is inlaid with a small amount of suction hydrogen metallic element M particulate TiFe phase composite, as shown in Figure 1.Because β-Ti and easily suction hydrogen metallic element M particle the two prior to TiFe mutually and H-H reaction, and form hydride and volumetric expansion takes place, cause in the alloy occurring a large amount of micro-flaws and TiFe mutually with clean surface, hydrogen then arrives cleaning TiFe surface by these micro-flaws easily, thereby makes TiFe be easy to hydrogenation.Optimization proportioning by alloying constituent of the present invention, not only solved room temperature activation problem, simultaneously making not again, the hydride of desorb hydrogen reduces to minimum, hydrogen storage capability has then reached more than 1.7% under the 4.0MPa, approach the highest level of TiFe alloy under the 6.0MPa, room temperature is inhaled hydrogen balance pressure and then is in the 1.0MPa.
Compared with the prior art, alloy of the present invention has the following advantages: (1) and TiFe alloy ratio needn't special activation treatment, and be easy to use, cost is low; (2) the reach capacity suction hydrogen pressure of hydrogen-storage amount (1.7%) is 4.0MPa, is lower than the 6.0MPa of TiFe; (3) not only allowed Ti over-stoichiometric but also be added with easy suction protium in the alloying constituent, hydrogen storage capability has reached more than 1.7%, is higher than TiFe
1-xMm
xSystem, Ti
1+xVarious ferro-titanium base hydrogen storage alloys such as Fe system and TiFe+4.5% Mm.
Fig. 1 is that chemical formula is Ti
1.2The metallographic microstructure figure (200 *) of Fe+6.0% Mm alloy.
Fig. 2 is that chemical formula is Ti
1.2The P-C-T graphic representation of Fe+6.0% Mm alloy under differing temps, X-coordinate are hydrogen-storage amount (H/M), and ordinate zou is put hydrogen balance pressure (MPa) for inhaling.
Embodiment 1:
Ti of the present invention
1.2The Fe+yM hydrogen storage alloy, x=0.2 in the formula, y are Ti
1.26% of Fe weight, M is Mm, presses earlier Ti
1.2The Fe chemical formula calculates required Ti and Fe add-on, calculates Ti again
1.2Fe and Mm add-on.In the starting material, Fe is the technically pure iron of purity 〉=99.5%, and Ti is the metal titanium of purity 〉=99%, rare earth element total content 〉=99% of norium Mm, wherein Ce 〉=40%.Above-mentioned starting material through cleaning and dry after weigh by the add-on that calculates, place non-consumable arc furnace, under the argon shield of 0.05MPa, carry out melting after finding time to be vented to 0.13Pa, and in water cooled mo(u)ld, solidify cooling.For making composition even, need the melting secondary.Take out alloy pig and be broken for the reactor (as storage hydrogen device, fuel tank or other hydride container) of packing into behind the fritter, import purity 〉=99.9% hydrogen to hydrogen pressure 4.0MPa after then reactor being found time to be vented to 1.3Pa, through some minutes to ten after surplus minute incubation period alloy begin to inhale hydrogen, it is saturated to inhale hydrogen after surplus hour of a few hours to ten, can come into operation thereafter.The P-C-T curve of this alloy under differing temps seen Fig. 2, reacted alloy hydrogen-storage amount and suction at each temperature on the figure and put hydrogen storage properties such as hydrogen balance pressure.The measured result hydrogen-storage amount reaches 1.73%, or 194 milliliters of every grams.
Embodiment 2:
Chemical formula is Ti in the preferred alloy of the present invention
1.2The Fe+3.0%Ca alloy calculates each metal add-on by chemical formula.In the starting material, the purity of Fe and Ti is identical with embodiment 1, and the purity of Ca is 99% calcium metal.The add-on weighing is pressed in starting material cleaning and dry back; place in the plumbago crucible of vacuum induction furnace; be vented to through finding time＜0.13Pa vacuum tightness after, under the 0.05MPa argon shield, carry out melting, refining is finished the back and is injected and be cooled to room temperature in the metal ingot mould take out under vacuum.The process of hydroprocessing first of alloy is with embodiment 1.Alloy needn't special activation treatment, contacts with hydrogen first and just is easy to inhale hydrogen, and the saturated hydride of formation is (Ti
1.2Fe+3.0%Ca) H
2.0, the actual measurement hydrogen-storage amount reaches 1.7%, 190 milliliters of perhaps every grams.
Document [1]: Inorganic Chemistry, Vol. 13, No.1,1974, P218-223
Document [2]: J.of the Less_Common134,1987, P275-286
Document [3]: J.of Alloys and Compounds, 177,1991, P.107-118
Document [4]: J.of the Less-Common Met., 108,1985, P313-325
Claims (1)
1. ferro-titanium base hydrogen storage alloy, it is characterized in that: the chemical formula of this hydrogen storage alloy is Ti
1+xFe+yM, 0＜x in the formula＜0.3, y is for being not more than Ti
1+x8% of Fe weight, M is cerium-rich mischmetal metal M m, perhaps lanthanum rich norium M1, perhaps a kind of among metal La, Ce, Pr, Nd, Sm, Li, Mg, the Ca.
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| CN99116897A CN1091157C (en) | 1999-09-21 | 1999-09-21 | Ferro-titanium base hydrogen storage alloy |
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| CN99116897A CN1091157C (en) | 1999-09-21 | 1999-09-21 | Ferro-titanium base hydrogen storage alloy |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100393628C (en) * | 2006-08-25 | 2008-06-11 | 西北大学 | Nano level modified solid hydrogen storage material of ferroferric oxide with single metal/bimetal being doped, and prepartion methpd |
| CN102443730B (en) * | 2010-10-13 | 2014-01-08 | 陈瑞凯 | Hydrogen storage alloy |
| CN105002422B (en) * | 2015-07-13 | 2017-01-04 | 苏州金业船用机械厂 | A kind of high rigidity Anti-pressure propeller blade |
| CN105132741B (en) * | 2015-09-25 | 2017-03-22 | 钢铁研究总院 | Rear earth-ferrotitanium hydrogen storage alloy for wind power storage |
| CN105779848A (en) * | 2016-04-14 | 2016-07-20 | 上海大学 | Ferrotitanium-based hydrogen storage alloy |
| WO2021033582A1 (en) * | 2019-08-19 | 2021-02-25 | 株式会社三徳 | Hydrogen storage material, hydrogen storage container, and hydrogen supply device |
| CN112391568A (en) * | 2020-11-10 | 2021-02-23 | 中国科学院上海微系统与信息技术研究所 | Hydrogen storage alloy resisting oxygen poisoning and preparation method thereof |
| CN112387976B (en) * | 2020-11-27 | 2022-11-22 | 中稀(山东)稀土开发有限公司 | Easily-activated RE-Ti-Fe alloy for fuel cell and preparation method thereof |
| CN114107856B (en) * | 2021-11-25 | 2022-09-20 | 武汉氢能与燃料电池产业技术研究院有限公司 | Hydrogen storage activity regeneration method of titanium hydrogen storage alloy |
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