CN101413624B - Hydrogen storing apparatus of metal hydrides and manufacturing method thereof - Google Patents

Hydrogen storing apparatus of metal hydrides and manufacturing method thereof Download PDF

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CN101413624B
CN101413624B CN2008101622158A CN200810162215A CN101413624B CN 101413624 B CN101413624 B CN 101413624B CN 2008101622158 A CN2008101622158 A CN 2008101622158A CN 200810162215 A CN200810162215 A CN 200810162215A CN 101413624 B CN101413624 B CN 101413624B
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hydrogen
storage
alloy
material sheet
center hole
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CN101413624A (en
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陈立新
陈长聘
肖学章
杭州明
王新华
李寿权
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Zhejiang University ZJU
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Zhejiang University ZJU
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/32—Hydrogen storage

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Abstract

The invention relates to a metal hydride hydrogen storage device and a preparation method thereof; wherein, the device comprises a shell which is filled in superposed hydrogen-storage material sheet which consists of a spumescent metal substrate which absorbs no hydrogen and mixture of hydrogen-storage alloy powder and adhesive which are filled in the gap of the spumescent metal substrate; the hydrogen-storage material sheet is provided with a central hole which is coincident to the central hole of the shell head and is connected with the central hole of the head by a filter sheet which is embedded in the head; the central hole of the head is fixed with a joint pipe which is provided with a valve. The hydrogen storage device can effectively improve the heat transmission performance of the hydrogen storage alloy and hydride powder, effectively prevents the flowing and accumulating of the hydrogen-storage alloy and the hydride, solves the hydrogen absorption expansion problem of the hydrogen storage alloy powder, thus having the advantages of high-efficiency running, safety and reliability and being suitable for the production of meta hydride hydrogen-storage devices applied to various sites.

Description

A kind of hydrogen storing apparatus of metal hydrides and manufacture method thereof
Technical field
The present invention relates to is a kind of hydrogen storing apparatus of metal hydrides and manufacture method thereof, belongs to storage, conveying and the compression technique area of hydrogen.
Background technique
Hydrogen is a kind of desirable clean fuel and following important secondary energy.The hydrogen storage of practical application at present and the mode of conveying mainly contain three kinds: i.e. high-pressure bottle storage hydrogen, liquid hydrogen tank storage hydrogen and the solid-state storage hydrogen of hydride hydrogen storage device.Storing, carry the outstanding advantage of hydrogen with hydrogen storing apparatus of metal hydrides is that Security is good, and unit weight storage hydrogen density is far above high-pressure bottle and liquid hydrogen tank.
The container of the metal hydride hydrogen storing alloy being put into a band valve just can constitute a hydrogen storing apparatus of metal hydrides.There is thermal effect in hydrogen storing alloy in the container in the process of inhaling, putting hydrogen, the thermal effect value is different different because of hydrogen storing alloy, is generally 20～80 Kilojoule/moles.Keep hydrogen storing alloy in the hydrogen storage device suction, put carrying out smoothly of hydrogen, just must import heat or from hydrogen storage device derivation heat to hydrogen storage device.Hydrogen storing alloy can produce volumetric expansion when suction hydrogen changes hydride into, specific volumetric dilatation is generally 10～25%, and efflorescence is micron-sized fine powder gradually.
The problem that exists is at present: on the one hand, because the thermal conductivity very poor (suitable) of metal hydride powder itself with the thermal conductivity of glass, sandstone, can not be in time in hydrogen storage device input heat or from the hydrogen storage device quantity of heat given up, make that the hydrogen storing alloy temperature sharply raises when sucking hydrogen, the hydrogen storing alloy temperature descends again fast during releasing hydrogen gas, thereby causes speed for hydrogen absorbing and releasing slowly even stop; On the other hand, the good fluidity of hydrogen storing alloy fine powder is put in the hydrogen operating process in suction, because of the driving meeting that is subjected to hydrogen flow forms local excessive accumulation easily in hydrogen storage device, and causes container deformation or destruction.Therefore, effectively improve the temperature conductivity and the local excessive accumulation that prevents powder of powder in the hydrogen storage device, need just to have become the key issue of solution.
Document " M.Ron and M.Elemelach.Heat transfer characteristics of porousmetallic matrix metal-hydrides.Proceeding of International Symposium onHydrides for Energy Storage, Pergamon, Oxford, 1978, pp.417-430. " and document " M.Ron, D.Gruen, M.Mendelsohn and I.Sheft.Preparation and properties of porousmetal hydride compacts.Journal of the Less-Common Metals, Vol.74,1980, pp.445-448. " in reported a kind of metal hydride hydrogen-storage alloy powder briquetting sintering technology.Promptly adopt the metallic dust do not inhale hydrogen, as aluminium powder, copper powder, nickel powder and hydrogen-storage alloy powder mixed sintering method, because sinter can not provide material suction hydrogen-expansion required space, the failure of an experiment as a result.Made afterwards that hydrogen storing alloy was carried out several to tens of suctions in advance into and put the hydrogen operation, under suction hydrogen state, fed SO then 2, alloy is poisoned to keep the volumetric expansion state, carry out the technology of briquetting sintering again.Though this method briquetting is put the hydrogen circulation and not cracked through inhaling for 1000 times, the preparation process complexity, and also hydrogen storing alloy can make the storage hydrogen capacity reduce more than 15% through poisoning and sintering.
Reported another kind of sintering method in the document " Qi-dong Wang, Jing Wu and Hui Gao.Vacuum sintered porous metalHydride Compacts.Z.f ü er Phys.Chem., Vol.164,1989, pp.1367-1372. ".Be about to metal hydride hydrogen storing alloy and aluminium powder and pore creating material and constitute mixture, and be pressed into bulk; After most of pore creating material was removed in 60～80 ℃ of bakings, sintering was finalized the design under vacuum again.This briquetting is inhaled through 1000 circulations and is put hydrogen and not chipping.Omitted repeatedly to inhale in advance and put hydrogen circulation and " poisoning " operation, and the operation simplification, cost reduces, but the storage hydrogen capacity still reduces about 15%.
Document " H.Ishikawa, K.Oguro, A.Kato, H.Suzuki and E.Ishii.Preparation andproperties of hydrogen storage alloy-copper microcapsules.Journal of theLess-Common Metals, Vol.107,1985, pp.105-110. " in a kind of preparation method of copper facing-briquetting is provided.The metal hydride hydrogen-storage alloy powder is put into copper plating solution copper facing after sensitization is handled; Hydrogen-storage alloy powder behind the plating heats in vacuum or argon gas and discharges hydrogen (in the copper facing process alloyed powder absorb hydrogen); Under 100～1000MPa pressure, be pressed into bulk then.Before the copper facing, hydrogen-storage alloy powder must carry out suction more than 10 times in advance puts the hydrogen circulation, to guarantee alloy pulverization fully and particle size stable, avoids the alloyed powder after the copper facing to destroy coating because of inhaling hydrogen-expansion.Obviously, this scheme has increased the suction more than 10 times and has put hydrogen operation and copper facing operation, and cost obviously improves, and the copper layer of plating can not inhale hydrogen, stores hydrogen capacity and has also descended more than 10%.
Document " J.J.Reilly and J.R.Johnson.The kinetics of the absorption ofhydrogen byLaNi 5H x-n-undecane suspensions.Journal of the Less-CommonMetals, Vol.104,1985, pp.175-190. " and document " J.J.Reilly, J.R.Johnson and T.Gamo.The effect of methane on the rate of hydrogen absorption by LaNi 5H xInliquid suspension.Journal of the Less-Common Metals, Vol.131,1987, pp.41-49. " in proposed to adopt chemical solvent and hydrogen storing alloy particle to form the method for suspension by U.S. Brookhaven National Laboratory: in the container of splendid attire metal hydride hydrogen storing alloy, inject n-undecane, normal octane or silicone oil and so on organic solvent.Hydrogen storing alloy can carry out the reversible hydrogen adsorption and desorption reaction in the same old way in this class organic solvent, temperature conductivity improves, container can not expand bad yet, but owing to added the organic solvent of not inhaling hydrogen in a large number, the unit weight of hydrogen storage device and the storage hydrogen density of per unit volume is all reduced significantly.
Summary of the invention
In order to overcome the deficiencies in the prior art, it is good to the objective of the invention is to propose a kind of temperature conductivity, can effectively prevent simultaneously flowing, piling up of hydrogen-storage alloy powder, put hydrogen storing apparatus of metal hydrides and the manufacture method thereof that can not damage hydrogen storage container in the hydrogen process inhaling repeatedly.
Hydrogen storing apparatus of metal hydrides of the present invention comprises end sealing, the other end has the housing of end socket, center hole is arranged on the end socket, be full of the storage hydrogen material sheet of repeatedly putting in the housing, storage hydrogen material sheet is by the foamed metal substrate of not inhaling hydrogen and be filled in hydrogen-storage alloy powder in the foamed metal substrate hole and the mixture of Bond constitutes, storage hydrogen material sheet has center hole, the center hole of storage hydrogen material sheet overlaps with the center hole of end socket, and be connected with the center hole of end socket by the filter sheet that is embedded in end socket, on the center hole of end socket, be fixed with the adapter of band valve.
Among the present invention, the said foamed metal substrate of not inhaling hydrogen can be a kind of in foamed aluminium substrate, foamed nickel substrate, foam copper substrate, foam aluminium alloy substrate, foamed nickel alloy substrate and the foam copper alloy substrate, perhaps is wherein two or more.
Among the present invention, the porosity ratio of not inhaling the foamed metal substrate of hydrogen is 91～98%, and thickness is 2～15 millimeters.
During the present invention put, said hydrogen storing alloy was a rare earth based hydrogen storage alloy, ti-based hydrogen-storing alloy, zirconium series hydrogen storage alloy, vanadium series hydrogen storage alloy, one or more in magnesium series hydrogen storage alloy and the calcium series hydrogen storage alloy.
Among the present invention, the aperture of said storage hydrogen material sheet center hole and end socket center hole is 3～10mm.
The manufacture method of hydrogen storing apparatus of metal hydrides of the present invention, its step is as follows:
Earlier prefabricated end sealing, the housing of the other end opening; To insert behind hydrogen-storage alloy powder and the binder solution mixing in the foamed metal substrate hole, become storage hydrogen material sheet 30～60 ℃ of oven dry; Dry storage hydrogen material sheet is cut into external diameter and the identical disk of storage hydrogen housing internal diameter, and be 3～10 millimeters circular hole in making aperture, disk center; To store the hydrogen material sheet lamination housing of packing into successively; With embedded filter sheet and have the end socket and the housing opening end welded seal of center hole, the interface of fixing belt valve on the end socket center hole.
Beneficial effect of the present invention is:
1) hydrogen-storage alloy powder in the hydrogen storage device be distributed in the hole of foamed metal substrate and with foam base plate network skeleton tight bond, thereby can effectively prevent flowing and local accumulation of hydrogen storing alloy and hydride powder thereof; Store hydrogen material sheet simultaneously and have center hole, can make things convenient for the turnover of hydrogen, the suction hydrogen volume expansion for hydrogen storing alloy leaves yielding space, distortion, the destruction that can effectively prevent hydrogen storage device again.
2) in the storage hydrogen material sheet do not inhale hydrogen foamed metal substrate have good heat conductivity (as the heat conductivity of Al, Ni, Cu be respectively 222,92,394J (msk) -1), and the heat conductivity of hydrogen-storage alloy powder than the end (as LaNi 5The heat conductivity of hydrogen-storage alloy powder and TiFe hydrogen-storage alloy powder only is 1.32 and 1.49J (msk) -1), the former thermal conductivity ratio latter heat conductivity is big 60～300 times, thereby can improve hydrogen-storage alloy powder and the material bed temperature conductivity of whole storage hydrogen effectively.Simultaneously, the porosity ratio of not inhaling hydrogen foamed metal substrate can reach 98% more than 91%, and the charge space of hydrogen-storage alloy powder is very big, and total hydrogen storage amount is reduced
Influence obviously reduce.
3) the metal hydride hydrogen storing alloy in this hydrogen storage device needn't carry out copper facing, briquetting, poisoning, sintering in advance, processing or processing such as hydrogen circulation are put in suction repeatedly, so its method is more superior, and has efficient, the safe and reliable characteristics of long-time running.
This hydrogen storing apparatus of metal hydrides has safety, characteristics of high efficiency, both has been applicable to fixed storage hydrogen application, also is applicable to portable or portable storage and the occasion of carrying hydrogen, as the fuel tank of hydrogen fuel cell, combustion hydrogen internal combustion engine vehicle etc.
Description of drawings
Fig. 1 is the structural representation of hydrogen storing apparatus of metal hydrides of the present invention;
Fig. 2 is the schematic cross-section of foamed metal substrate.
Embodiment
Further specify the present invention below in conjunction with drawings and Examples.
With reference to Fig. 1, hydrogen storing apparatus of metal hydrides of the present invention comprises: end sealing, the other end has the housing 1 of end socket 7, on the end socket 7 center hole is arranged, be full of the storage hydrogen material sheet of repeatedly putting 2 in the housing, storage hydrogen material sheet 2 is by the foamed metal substrate of not inhaling hydrogen and be filled in hydrogen-storage alloy powder in the foamed metal substrate hole and the mixture of Bond constitutes, storage hydrogen material sheet 2 has center hole 3, the center hole of storage hydrogen material sheet overlaps with the center hole of end socket, and be connected with the center hole of end socket by the filter sheet 6 that is embedded in end socket 7, on the center hole of end socket, be fixed with the adapter 5 of band valve 4.
The foamed metal substrate has latticed skeleton (see figure 2), and porosity ratio is 91～98%, and thickness is 2～15 millimeters.
The housing of described hydrogen storage device can be selected stainless steel or aluminum alloy material for use.
Embodiment 1:
The hydrogen foamed metal substrate of not inhaling in the hydrogen storing apparatus of metal hydrides adopts the foamed aluminium substrate, and its porosity ratio is 91%, and thickness is 15 millimeters.The cylindrical housings of hydrogen storage device is an aluminum alloy material, and internal diameter is 80 millimeters; Hydrogen storing alloy is rare earth based hydrogen storage alloy Mm 0.8Ca 0.2Ni 5, Mm is a norium in the formula.Earlier with Mm 0.8Ca 0.2Ni 5The broken particle diameter that forms of alloy is not more than 0.2 millimeter powder; Again with Mm 0.8Ca 0.2Ni 5Alloyed powder and mass concentration are 3% the PVA aqueous solution (its addition be hydrogen-storage alloy powder weight 1/10th) mixing furnishing paste, smear then in the hole of inserting the foamed aluminium substrate, and under 30 ℃ fully oven dry form storage hydrogen material sheet; Again the storage hydrogen material sheet of drying is cut into external diameter and be 80 millimeters disk, and make the aperture at the disk center be 10 millimeters circular hole; To store then hydrogen material sheet successively lamination pack in the housing; End socket and storage hydrogen housing opening end welded seal with built-in filter sheet; To be fixed on the end socket with the adapter of valve again.
To 133Pa, importing purity under the atmospheric pressure of 3.0MPa is 99.99% hydrogen with the hydrogen storing apparatus of metal hydrides vacuumizing and exhausting.Hydrogen storing alloy in the hydrogen storage device begins to inhale hydrogen, and gradates and be hydride, inhales hydrogen and is converted into the hydride powder fully after saturated, and activation is first finished, and this hydrogen storage device can come into operation.Measured result: the weight storage hydrogen density of storage hydrogen material sheet is 1.45%, and heat conductivity is 17.8J (msk) -1At room temperature, inhale hydrogen and 0.1MPa air pressure is put hydrogen by 3.0MPa pressure, inhale repeatedly put hydrogen cycling 1000 times after, any dilatancy or damage do not appear in the hydrogen storage device tank body.
Embodiment 2:
The hydrogen foamed metal substrate of not inhaling in the hydrogen storing apparatus of metal hydrides adopts the foam copper substrate, and its porosity ratio is 95%, and thickness is 10 millimeters.The housing of hydrogen storage device is a stainless steel, and internal diameter is 63 millimeters; Hydrogen storing alloy is that titanium is TiFe 0.85Mn 0.15Alloy.Earlier with TiFe 0.85Mn 0.15The broken particle diameter that forms of alloy is not more than 0.2 millimeter powder, be 1.5% the CMC aqueous solution (its addition be alloyed powder weight 1/10th) mixing furnishing paste with mass concentration again, smear then in the hole of inserting the foam copper substrate, and under 50 ℃, dry formation storage hydrogen material sheet fully; Again the storage hydrogen material sheet of drying is cut into external diameter and be many disks of 63 millimeters, and make the aperture at the disk center be 6 millimeters circular hole; To store then hydrogen material sheet successively lamination pack in the housing; End socket and storage hydrogen housing opening end welded seal with built-in filter sheet; To be fixed on the end socket with the adapter of valve again.Activation process is identical with embodiment 1.Measured result: the weight storage hydrogen density of storage hydrogen material sheet is 1.65%, and heat conductivity is 25.2J (msk) -1After at room temperature the hydrogen cycling was put in suction repeatedly through 1000 times, this hydrogen storage device was excellent.
Embodiment 3:
The hydrogen foamed metal substrate of not inhaling in the hydrogen storing apparatus of metal hydrides adopts foamed nickel substrate, and its porosity ratio is 98%, and thickness is 2 millimeters.The housing of hydrogen storage device is a stainless steel, and internal diameter is 50 millimeters; Hydrogen storing alloy is BCC alloy Ti for the titanium vanadium 0.16Cr 0.22V 0.52Fe 0.05Zr 0.05Earlier with Ti 0.16Cr 0.22V 0.52Fe 0.05Zr 0.05The broken particle diameter that forms of alloy is not more than 0.15 millimeter powder, be 3% the PVA aqueous solution (its addition be alloyed powder weight 1/10th) mixing furnishing paste with mass concentration again, smear then in the hole of inserting foamed nickel substrate, and under 60 ℃, dry formation storage hydrogen material sheet fully; Again the storage hydrogen material sheet of drying is cut into external diameter and be many disks of 50 millimeters, and make the aperture at the disk center be 3 millimeters circular hole; To store then hydrogen material sheet successively lamination pack in the housing; End socket and storage hydrogen housing opening end welded seal with built-in filter sheet; To be fixed on the end socket with the adapter of valve again.Activation process: hydrogen storage device is evacuated to 50Pa, and heat temperature raising to 200 ℃ is held degree of vacuum in the hydrogen storage device in the continuation of insurance of intensification heating process relaying; Importing purity then under the atmospheric pressure of 4.0MPa is 99.99% hydrogen, and is cooled to room temperature, at this moment Ti 0.16Cr 0.22V 0.52Fe 0.05Zr 0.05Alloy begins to inhale the hydrogen activation, and activation was finished when suction hydrogen was saturated.Measured result: the weight storage hydrogen density of storage hydrogen material sheet is 3.26%, and heat conductivity is 13.3J (msk) -1After inhaling hydrogen and 200 ℃ and put the cycling repeatedly of hydrogen through 1000 normal temperature, this hydrogen storage device is excellent.

Claims (6)

1. hydrogen storing apparatus of metal hydrides, it is characterized in that: comprise end sealing, the other end has the housing (1) of end socket (7), end socket has center hole on (7), be full of the storage hydrogen material sheet of repeatedly putting (2) in the housing, storage hydrogen material sheet (2) is by the foamed metal substrate of not inhaling hydrogen and be filled in hydrogen-storage alloy powder in the foamed metal substrate hole and the mixture of Bond constitutes, storage hydrogen material sheet (2) has center hole (3), the center hole of storage hydrogen material sheet overlaps with the center hole of end socket, and be connected with the center hole of end socket by the filter sheet (6) that is embedded in end socket (7), on the center hole of end socket, be fixed with the adapter (5) of band valve (4).
2. hydrogen storing apparatus of metal hydrides according to claim 1, it is characterized in that: the said foamed metal substrate of not inhaling hydrogen is a kind of in foamed aluminium substrate, foamed nickel substrate, foam copper substrate, foam aluminium alloy substrate, foamed nickel alloy substrate and the foam copper alloy substrate, perhaps is wherein two or more.
3. hydrogen storing apparatus of metal hydrides according to claim 1 is characterized in that: the porosity ratio of not inhaling the foamed metal substrate of hydrogen is 91～98%, and thickness is 2～15 millimeters.
4. hydrogen storing apparatus of metal hydrides according to claim 1, it is characterized in that: said hydrogen storing alloy is a rare earth based hydrogen storage alloy, ti-based hydrogen-storing alloy, zirconium series hydrogen storage alloy, the vanadium series hydrogen storage alloy, one or more in magnesium series hydrogen storage alloy and the calcium series hydrogen storage alloy.
5. hydrogen storing apparatus of metal hydrides according to claim 1 is characterized in that: the aperture of storage hydrogen material sheet center hole and end socket center hole is 3～10mm.
6. the manufacture method of hydrogen storing apparatus of metal hydrides according to claim 1 is characterized in that step is as follows:
Earlier prefabricated end sealing, the housing of the other end opening; To insert behind hydrogen-storage alloy powder and the binder solution mixing in the foamed metal substrate hole, become storage hydrogen material sheet 30～60 ℃ of oven dry; Dry storage hydrogen material sheet is cut into external diameter and the identical disk of storage hydrogen housing internal diameter, and be 3～10 millimeters circular hole in making aperture, disk center; To store the hydrogen material sheet lamination housing of packing into successively; With embedded filter sheet and have the end socket and the housing opening end welded seal of center hole, the interface of fixing belt valve on the end socket center hole.
CN2008101622158A 2008-11-27 2008-11-27 Hydrogen storing apparatus of metal hydrides and manufacturing method thereof Active CN101413624B (en)

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