CN1598018A - Technology of preparing high purity and activity magnesium-base hydrogen-storage alloy - Google Patents
Technology of preparing high purity and activity magnesium-base hydrogen-storage alloy Download PDFInfo
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- CN1598018A CN1598018A CN 200410041862 CN200410041862A CN1598018A CN 1598018 A CN1598018 A CN 1598018A CN 200410041862 CN200410041862 CN 200410041862 CN 200410041862 A CN200410041862 A CN 200410041862A CN 1598018 A CN1598018 A CN 1598018A
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Abstract
This invention provides a preparation technics of high purity and activity magnesian radicle hydrogen storage alloy. This technics weighs up the raw materials of every compositive metal powder according to the designed constituent mole proportion of magnesian radicle alloy and mixes them symmetrically, then sets them into a reactor with certain pressure preserved or deoxidized atmosphere, the synthesis temperature is 350-500deg.C, 1-8 hours, the obtain high purity magnesian radicle alloy. The magnesian radicle alloy in this technics can absorb hydrogen more than 3.0wt% without activation treatment for the first time. The advantages are low synthesis temperature, simple technics, low energy consumption.
Description
Technical field
The invention belongs to the material preparation field of powder metallurgy, particularly relate to a kind of high-purity high-activity Mg base hydrogen bearing alloy preparation technology.
Background technology
Characteristics such as that Mg base hydrogen bearing alloy has is in light weight, hydrogen-storage density is high, earth resources is abundant are to be known as the hydrogen storage material that has the application and development prospect most.The present industrial preparation of Magnuminium adopts the melting teeming practice.With magnesium-nickel alloy (Mg
2Ni) be example, since the fusing point lower (650 ℃) of magnesium, the fusing point of nickel higher (1455 ℃), cause a large amount of vaporization losseses of magnesium in the fusion process, product is formed and is departed from a mole proportioning, need be according to the alloy cast ingot chemical analysis, repeatedly melt after adding magnesium, just can obtain the high-purity magnesium base hydrogenous alloy.As hydrogen storage material, the smelting method for preparing Magnuminium also need activate processing, after normally ingot casting is pulverized, inhales hydrogen and dehydrogenation cycle repeatedly under certain hydrogen pressure and temperature, just can obtain the high reactivity hydrogen storage alloy.
Summary of the invention
The object of the present invention is to provide a kind of Processes and apparatus simple, economize and can save time, the product high-purity high-activity, be suitable for the Mg base hydrogen bearing alloy technology of preparing of large-scale industrial production.
Purpose of the present invention can realize by following measure:
A kind of high-purity high-activity Mg base hydrogen bearing alloy preparation technology; the powder that takes by weighing each component metals by the mole proportioning of Magnuminium design component is a raw material; mix; place the reactor of certain pressure protective atmosphere or reducing atmosphere; synthesis temperature 350-500 ℃; generated time 1-8 hour, product was the high purity Magnuminium.
Described high-purity high-activity Mg base hydrogen bearing alloy preparation technology, its interalloy each component raw metal powder uniform mixing is a mechanically mixing; Mechanically mixing can be dry mixed or wet-mixed.
Described high-purity high-activity Mg base hydrogen bearing alloy preparation technology, wherein wet-mixed is meant alloy each component raw metal powder joined in the anhydrous organic solvent and mixes; Anhydrous organic solvent can be dehydrated alcohol, acetone.
Described high-purity high-activity Mg base hydrogen bearing alloy preparation technology, wherein magnesium metal-powder purity is more than 99.0%, and granularity is below 250 microns, and other metal-powder purity is more than 99.5%, and granularity is below 15 microns.
Described high-purity high-activity Mg base hydrogen bearing alloy preparation technology, wherein demagging is outside the low melting point in the alloy component, and other component is the refractory metal element, and these refractory metal elements can be Ni, Cu.
Described high-purity high-activity Mg base hydrogen bearing alloy preparation technology, wherein the metal mixed powder does not have pressing treatment, piles up with loose density to place reactor.
Described high-purity high-activity Mg base hydrogen bearing alloy preparation technology, wherein protective atmosphere is that argon gas, reducing atmosphere are hydrogen in the reactor, atmosphere pressures is 0.1-1.5MPa.
Described high-purity high-activity Mg base hydrogen bearing alloy preparation technology, wherein atmosphere purity is more than 99.99% in the reactor.
Described high-purity high-activity Mg base hydrogen bearing alloy preparation technology, wherein temperature of reaction is preferably 400-500 ℃, and the reaction times is preferably 3-6 hour.
Beneficial effect of the present invention:
The present invention is with respect to present Magnuminium industrially scalable preparation method's outstanding feature:
1, synthesis temperature is well below the fusing point of MAGNESIUM METAL, even is lower than the alloy system eutectic point, fundamentally avoided the vaporization losses of MAGNESIUM METAL, guaranteed to meet the high purity Magnuminium of design component mole proportioning.
2, synthesis temperature is below 500 ℃, and generated time is a several hrs, has remarkable energy-efficient effect.
3, synthesis pressure is below 1.5MPa, and reactor can adopt general anti-hydrogen high pressure tubular Reaktionsofen, greatly reduces the technical requirements to synthesis device, is suitable for industrial applications.
4, adopt the mechanically mixing metal-powder, and directly be piled up in naturally in the example boat, need not other pressing process, simplify technical process greatly, and help reaction and carry out, be suitable for large-scale industrialization promotion with loose density.
5, synthetic product has high storage hydrogen activity, does not have to activate and handles hydrogen 3.0wt% above (theoretical value is 3.6wt%) first.
Description of drawings
460 ℃ of synthetic product Mg of Fig. 1
2The X ray diffracting spectrum of Ni.
460 ℃ of synthetic product Mg of Fig. 2
2Inhale the hydrogen kinetic curve for 330 ℃ of Ni.
460 ℃ of synthetic product Mg of Fig. 3
2NiH
4X ray diffracting spectrum.
460 ℃ of synthetic product Mg of Fig. 4
2NiH
4330 ℃ inhale the hydrogen kinetic curves.
Embodiment
Metal magnesium powder, purity 99.2%, granularity-200 order, nickel powder purity is 99.7%, granularity is 2-3 μ m.With the mole proportioning is that 2: 1 10.0g magnesium nickel mixed powder mixes in agate mortar, mixed powder directly is piled up in example boat with loose density, and place high-pressure reactor, reactor vacuumizes, charge into 0.1MPa purity then and be 99.99% argon gas, heated sample to 460 ℃ is incubated 5 hours, is cooled to room temperature.Embodiment 1 product is single thing phase Mg
2Ni, its X ray diffracting spectrum is seen Fig. 1, does not have the suction of activation hydrogen kinetic curve and sees Fig. 2.
Metal magnesium powder, purity 99.5%, granularity-177 μ m, nickel powder purity is 99.9%, granularity is 2-3 μ m.With the mole proportioning is that 2: 1 10.0g magnesium nickel mixed powder is poured the beaker that fills acetone into, ultrasonic vibration mixes, directly be piled up in example boat after the seasoning with loose density, and place high-pressure reactor, reactor vacuumizes, and charges into 1.0MPa purity then and be 99.995% hydrogen, heated sample to 460 ℃, be incubated 5 hours, be cooled to room temperature.Embodiment 2 products are single thing phase Mg
2NiH
4, its X ray diffracting spectrum is seen Fig. 3, does not have the suction of activation hydrogen kinetic curve and sees Fig. 4.
Claims (9)
1, a kind of high-purity high-activity Mg base hydrogen bearing alloy preparation technology; it is characterized in that the powder that mole proportioning by Magnuminium design component takes by weighing each component metals is a raw material; mix; place the protective atmosphere or the reducing atmosphere reactor of certain pressure; synthesis temperature 350-500 ℃; generated time 1-8 hour, product was the high purity Magnuminium.
2, high-purity high-activity Mg base hydrogen bearing alloy preparation technology according to claim 1 is characterized in that alloy each component raw metal powder uniform mixing is a mechanically mixing; Mechanically mixing can be dry mixed or wet-mixed.
3, high-purity high-activity Mg base hydrogen bearing alloy preparation technology according to claim 2, it is characterized in that wet-mixed is meant alloy each component raw metal powder joined in the anhydrous organic solvent mixes; Anhydrous organic solvent can be dehydrated alcohol, acetone.
4, high-purity high-activity Mg base hydrogen bearing alloy preparation technology according to claim 1 is characterized in that magnesium metal-powder purity is more than 99.2%, and granularity is below 250 microns, and other metal-powder purity is more than 99.5%, and granularity is below 15 microns.
5, high-purity high-activity Mg base hydrogen bearing alloy preparation technology according to claim 1 is characterized in that demagging is outside the low melting point in the alloy component, and other component is the refractory metal element.
6, high-purity high-activity Mg base hydrogen bearing alloy preparation technology according to claim 1 is characterized in that the metal mixed powder does not have pressing treatment, piles up with loose density to place reactor.
7, high-purity high-activity Mg base hydrogen bearing alloy preparation technology according to claim 1 is characterized in that protective atmosphere is that argon gas, reducing atmosphere are hydrogen in the reactor, and atmosphere pressures is 0.1-1.5MPa.
8, high-purity high-activity Mg base hydrogen bearing alloy preparation technology according to claim 1 is characterized in that temperature of reaction is preferably 400-500 ℃, and the reaction times is preferably 3-6 hour.
9,, it is characterized in that atmosphere purity is more than 99.99% in the reactor according to claim 1 or 7 described high-purity high-activity Mg base hydrogen bearing alloy preparation technologies.
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| Application Number | Priority Date | Filing Date | Title |
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| CN200410041862.5A CN1281772C (en) | 2004-09-03 | 2004-09-03 | Technology of preparing high purity and activity magnesium-base hydrogen-storage alloy |
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| CN200410041862.5A CN1281772C (en) | 2004-09-03 | 2004-09-03 | Technology of preparing high purity and activity magnesium-base hydrogen-storage alloy |
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| CN1598018A true CN1598018A (en) | 2005-03-23 |
| CN1281772C CN1281772C (en) | 2006-10-25 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100432249C (en) * | 2006-06-27 | 2008-11-12 | 上海大学 | Production of magnesium-based hydrogen-storage material under equalized strong magnetic field and its producer |
| CN114505475A (en) * | 2022-02-18 | 2022-05-17 | 广东省科学院新材料研究所 | Low-temperature high-capacity magnesium-based hydrogen storage powder and preparation method thereof |
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2004
- 2004-09-03 CN CN200410041862.5A patent/CN1281772C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100432249C (en) * | 2006-06-27 | 2008-11-12 | 上海大学 | Production of magnesium-based hydrogen-storage material under equalized strong magnetic field and its producer |
| CN114505475A (en) * | 2022-02-18 | 2022-05-17 | 广东省科学院新材料研究所 | Low-temperature high-capacity magnesium-based hydrogen storage powder and preparation method thereof |
| CN114505475B (en) * | 2022-02-18 | 2023-12-05 | 广东省科学院新材料研究所 | Low-temperature high-capacity magnesium-based hydrogen storage powder and preparation method thereof |
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| CN1281772C (en) | 2006-10-25 |
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