CN102925773A - Preparation and application of magnesium titanium matrix composite hydrogen storage alloy of body-centered cubic (BCC) structure - Google Patents
Preparation and application of magnesium titanium matrix composite hydrogen storage alloy of body-centered cubic (BCC) structure Download PDFInfo
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Abstract
The invention discloses preparation and application of a magnesium titanium matrix composite hydrogen storage alloy of a body-centered cubic (BCC) structure. Chemical constitution of the magnesium titanium matrix composite hydrogen storage alloy is Mg70-xTi12+xNi12Mn6, wherein x=8, 16, 24 and 32. The preparation of the magnesium titanium matrix composite hydrogen storage alloy of the BCC structure includes: under the protection of inert gas, metal powder of Mg, Ti, Ni and Mn with 99.9% purity is placed in a ball milling pot according to atomic ratio of Mg: Ti: Ni: Mn = (70-x): (12+x): 12: 6, wherein x=8, 16, 24 and 32, and mechanical alloying is performed on the metal powder to obtain the magnesium titanium matrix composite hydrogen storage alloy of the BCC structure. The magnesium titanium matrix composite hydrogen storage alloy is made into fuel cells which are mainly applied to a hydrogen energy storage system. The preparation and the application of the magnesium titanium matrix composite hydrogen storage alloy of the BCC structure have the advantage that after 200-hour mechanical ball milling is performed on the Mg70-xTi12+Xni12Mn6 (x=8, 16, 24 and 32) alloy manufactured by a mechanical alloying method, a magnesium titanium matrix BCC structure occurs in corresponding alloys when x is equal to 24 and x is equal to 32, and the preparation and the application lay the foundation for research of magnesium titanium matrix BCC structure hydrogen storage alloys.
Description
Technical field
The present invention relates to a kind of composite hydrogen occluding alloy, specifically preparation of a kind of BCC structure magnesium titanium base composite hydrogen storage alloy and uses thereof.
Technical background
At present, environmental issue is perplexing All Around The World, and the traditional energy products of combustion is just paid attention to by people the pollution of environment.Hydrogen burning generates water, and environment is not polluted, and caused people to the showing great attention to of Hydrogen Energy, yet the problem that storage and transportation face becomes the obstacle of its development.One of effective way that hydrogen and metal, hydrogen and intermetallic compound reaction generation metal hydride are considered to address this problem.In the metal hydride, hydrogen atom mainly occupies on the interstitial site between atoms metal, therefore, and the hydrogen-storage amount that how much directly affects metal hydride of interstitial site.Hydrogen storage alloy with BCC structure is compared with the hydrogen storage alloy with FCC structure or HCP structure, and its interstitial site is more, can store the position favors that are subject to numerous scholars of hydrogen atom more.In this class hydrogen storage alloy, because having higher energy density, magnesium and Mg base hydrogen bearing alloy be considered to one of hydrogen storage material of tool development prospect.
Summary of the invention
The purpose of this invention is to provide preparation of a kind of BCC structure magnesium titanium base composite hydrogen storage alloy and uses thereof.
The technical scheme that the present invention solves the problems of the technologies described above is as follows:
1. the chemical constitution of a BCC structure magnesium titanium base composite hydrogen storage alloy is Mg
70-xTi
12+xNi
12Mn
6, x=8 in the formula, 16,24,32.
2. the preparation method of a BCC structure magnesium titanium base composite hydrogen storage alloy, preparation process is as follows:
1) under protection of inert gas, with purity all at the Mg more than 99.9%, Ti, Ni, Mn metal-powder according to Mg:Ti:Ni:Mn=(70-x): (12+x): the atomic ratio of 12:6, x=8 in the formula, 16,24,32, place ball grinder;
2) Stainless Steel Ball take ball material mass ratio as 20:1 places ball grinder, and wherein large ball is 4, and diameter is 8mm, and all the other diameters are respectively middle ball and the bead of 4mm and 2mm, and the number ratio of middle ball and bead is 1:1;
3) for the first time begin ball milling before, ball grinder is vacuumized, took out in advance 4 minutes first, then be filled with the 3atm argon gas, 3 times so repeatedly, carry out ball milling after being filled with at last the 3atm argon gas, Ball-milling Time is 30 hours for the first time;
4) since the ball milling second time, ball grinder was opened in 10 hours in every interval, and ball grinder is processed, and avoided powdered alloy to glue tank, was to carry out in vacuum glove box when opening ball grinder, and adding 1atm purity is 99.9% argon gas in the vacuum glove box;
5) rotating speed of planetary ball mill is 300 rev/mins in mechanical milling process, and every operation 30 minutes stops to reverse after 10 minutes again, and Ball-milling Time is 400 hours altogether, obtains BCC structure magnesium titanium base composite hydrogen storage alloy.
3. the preparation method of a BCC structure magnesium titanium base composite hydrogen storage alloy, preparation process is as follows:
1) under protection of inert gas, with purity all at the Mg more than 99.9%, Ti, Ni, Mn metal-powder according to Mg:Ti:Ni:Mn=(70-24): (12+24): 12: 6 atomic ratio places ball grinder;
2) place ball grinder take ball material mass ratio as 20: 1 Stainless Steel Ball, wherein large ball is 4, and diameter is 8mm, and all the other diameters are respectively middle ball and the bead of 4mm and 2mm, and the number ratio of middle ball and bead is 1: 1;
3) for the first time begin ball milling before, ball grinder is vacuumized, took out in advance 4 minutes first, then be filled with the 3atm argon gas, 3 times so repeatedly, carry out ball milling after being filled with at last the 3atm argon gas, Ball-milling Time is 30 hours for the first time;
4) since the ball milling second time, ball grinder was opened in 10 hours in every interval, and ball grinder is processed, and avoided powdered alloy to glue tank, was to carry out in vacuum glove box when opening ball grinder, and adding 1atm purity is 99.9% argon gas in the vacuum glove box;
5) rotating speed of planetary ball mill is 300 rev/mins in mechanical milling process, and every operation 30 minutes stops to reverse after 10 minutes again, and Ball-milling Time is 200 hours altogether, obtains BCC structure magnesium titanium base composite hydrogen storage alloy.
4. the preparation method of a BCC structure magnesium titanium base composite hydrogen storage alloy, preparation process is as follows:
1) under protection of inert gas, with purity all at the Mg more than 99.9%, Ti, Ni, Mn metal-powder according to Mg:Ti:Ni:Mn=(70-32): (12+32): 12: 6 atomic ratio places ball grinder;
2) place ball grinder take ball material mass ratio as 20: 1 Stainless Steel Ball, wherein large ball is 4, and diameter is 8mm, and all the other diameters are respectively middle ball and the bead of 4mm and 2mm, and the number ratio of middle ball and bead is 1: 1;
3) for the first time begin ball milling before, ball grinder is vacuumized, took out in advance 4 minutes first, then be filled with the 3atm argon gas, 3 times so repeatedly, carry out ball milling after being filled with at last the 3atm argon gas, Ball-milling Time is 30 hours for the first time;
4) since the ball milling second time, ball grinder was opened in 10 hours in every interval, and ball grinder is processed, and avoided powdered alloy to glue tank, was to carry out in vacuum glove box when opening ball grinder, and adding 1atm purity is 99.9% argon gas in the vacuum glove box;
5) rotating speed of planetary ball mill is 300 rev/mins in mechanical milling process, and every operation 30 minutes stops to reverse after 10 minutes again, and Ball-milling Time is 200 hours altogether, obtains BCC structure magnesium titanium base composite hydrogen storage alloy.
The purposes of above-mentioned magnesium titanium base composite hydrogen storage alloy is to be prepared into fuel cell with magnesium titanium base composite hydrogen storage alloy, is mainly used in the Hydrogen Energy storage system.
Advantage of the present invention:
Mg through the mechanical alloying method preparation
70-xTi
12+xNi
12Mn
6(x=8,16,24,32) alloy behind 200 hours mechanical ball milling, magnesium titanium base BCC structure occurs, for the later on research of magnesium titanium base BCC structure hydrogen storage alloy lays the foundation in x=24 and the corresponding alloy of x=32.
Description of drawings
Fig. 1 is Mg
62Ti
20Ni
12Mn
8Alloy is through the XRD figure of different Ball-milling Times.
Among the figure, X-coordinate is scanning angle, represents with 2 θ, and ordinate zou is diffraction peak intensity, represents with Intensity.
Fig. 2 is Mg
54Ti
28Ni
12Mn
6Alloy is through the XRD figure of different Ball-milling Times.
Among the figure, X-coordinate is scanning angle, represents with 2 θ, and ordinate zou is diffraction peak intensity, represents with Intensity.
Fig. 3 is Mg
46Ti
36Ni
12Mn
6Alloy is through the XRD figure of different Ball-milling Times.
Among the figure, X-coordinate is scanning angle, represents with 2 θ, and ordinate zou is diffraction peak intensity, represents with Intensity.
Fig. 4 is Mg
38Ti
44Ni
12Mn
6Alloy is through the XRD figure of different Ball-milling Times.
Among the figure, X-coordinate is scanning angle, represents with 2 θ, and ordinate zou is diffraction peak intensity, represents with Intensity.
Fig. 5 is Mg
70-xTi
12+xNi
12Mn
6The DTA curve of 200 hours hydride of (x=8,16,24,32) alloy ball milling.
Among the figure, X-coordinate is Heating temperature, represents with Temperature, and ordinate zou is differential thermal, represents with Heat flow.
Embodiment
The invention will be further described below in conjunction with drawings and Examples.
Embodiment 1
The present invention is with Mg: Ti: Ni: Mn=62: 20: 12: 6 atomic ratio configures sample; take ratio of grinding media to material as 20: 1; rotating speed is to carry out mechanical ball milling in 300 rev/mins of situations; ball mill for the first time working time be 30 hours; then in vacuum glove box; under argon shield; open the ball grinder alloy and carry out break process; for preventing the sticking tank of powdered alloy and slimeball; from for the second time operation; every interval 10 hours alloy powder under argon shield is processed, and be 400 hours working time altogether.Secondly minute different time periods (at 50 hours, 100 hours, 200 hours, respectively getting one time sample in 400 hours) collected specimens, each sample that gathers is about 3g, and is constant for guaranteeing ratio of grinding media to material, accordingly abrading-ball taken out simultaneously when taking out sample each.Sample after the collection is crossed 200 mesh sieves through after grinding, and the magnesium-titanium-based hydrogen storage alloy after will sieving at last carries out XRD and DTA test.The XRD test result as shown in Figure 1, Mg
62Ti
20Ni
12Mn
8Alloy is in 50 hour stage of ball milling, and phase structure is mainly by having HCP and the FCC structure forms in the mixture; When Ball-milling Time is 100 hours, Mn and part Ni are solidly soluted in the Ti element; After Ball-milling Time was 200 hours, Ni further was affixed in Mg and the Ti intracell; After Ball-milling Time was increased to 400 hours, the diffraction peak with HCP structure almost all disappeared, and simple substance is solid-solubilized in together mutually basically fully in the alloy, only occurs FCC and BCC structure in the alloy.DTA test result such as Fig. 5 are through Mg behind 200 hours ball millings
62Ti
20Ni
12Mn
8The hydride of (corresponding x=8) alloy two endotherm(ic)peaks occur in heat-processed, and first endotherm(ic)peak is 397 ℃, and the position at second dehydrogenation peak is 553 ℃.
Embodiment 2
The present invention is with Mg: Ti: Ni: Mn=54: 28: 12: 6 atomic ratio configures sample; take ratio of grinding media to material as 20: 1; rotating speed is to carry out mechanical ball milling in 300 rev/mins of situations; ball mill for the first time working time be 30 hours; then in vacuum glove box; under argon shield; open the ball grinder alloy and carry out break process; for preventing the sticking tank of powdered alloy and slimeball; from for the second time operation; every interval 10 hours alloy powder under argon shield is processed, and be 400 hours working time altogether.Secondly minute different time periods (at 50 hours, 100 hours, 200 hours, respectively getting one time sample in 400 hours) collected specimens, each sample that gathers is about 3g, and is constant for guaranteeing ratio of grinding media to material, accordingly abrading-ball taken out simultaneously when taking out sample each.Sample after the collection is crossed 200 mesh sieves through after grinding, and the magnesium-titanium-based hydrogen storage alloy after will sieving at last carries out XRD and DTA test.The XRD test result as shown in Figure 2, Mg
54Ti
28Ni
12Mn
6Alloy is in 50 hour stage of ball milling, and phase structure is mainly by having HCP and the FCC structure forms in the mixture; When Ball-milling Time is 100 hours, Mn and part Ni are solidly soluted in the Ti element; When Ball-milling Time was 200 hours, Ni further was affixed in Mg and the Ti intracell; After Ball-milling Time was increased to 400 hours, the diffraction peak with HCP structure almost all disappeared, and simple substance is solid-solubilized in together mutually basically fully in the alloy, only occurs FCC and BCC structure in the alloy.DTA test result such as Fig. 5, among Fig. 5 through Mg behind 200 hours ball millings
54Ti
28Ni
12Mn
6The hydride of (corresponding x=16) alloy two endotherm(ic)peaks occur in heat-processed, and first endotherm(ic)peak is 415 ℃, and the position at second dehydrogenation peak is 555 ℃.
Embodiment 3
The present invention is with Mg: Ti: Ni: Mn=46: 36: 12: 6 atomic ratio configures sample; take ratio of grinding media to material as 20: 1; rotating speed is to carry out mechanical ball milling in 300 rev/mins of situations; ball mill for the first time working time be 30 hours; then in vacuum glove box; under argon shield; open the ball grinder alloy and carry out break process; for preventing the sticking tank of powdered alloy and slimeball; from for the second time operation; every interval 10 hours alloy powder under argon shield is processed, and be 400 hours working time altogether.Secondly minute different time periods (at 50 hours, 100 hours, 200 hours, respectively getting one time sample in 400 hours) collected specimens, each sample that gathers is about 3g, and is constant for guaranteeing ratio of grinding media to material, accordingly abrading-ball taken out simultaneously when taking out sample each.Sample after the collection is crossed 200 mesh sieves through after grinding, and the magnesium-titanium-based hydrogen storage alloy after will sieving at last carries out XRD and DTA test.The XRD test result as shown in Figure 3, Mg
46Ti
36Ni
12Mn
6Alloy is in 50 hour stage of ball milling, and phase structure is mainly by having HCP and the FCC structure forms in the mixture; When Ball-milling Time was 100 hours, Mn and part Ni were solidly soluted in the Ti element; When Ball-milling Time was increased to 200 hours, Ni further was affixed in Mg and the Ti intracell, near 2 θ=43.1 °, 63.1 ° and 70.7 °, BCC structure phase occurred; When Ball-milling Time was increased to 400 hours, the diffraction peak with HCP structure almost all disappeared, and simple substance is solid-solubilized in together mutually basically fully in the alloy, only occurs FCC and BCC structure in the alloy.DTA test result such as Fig. 5, among Fig. 5 through Mg behind 200 hours ball millings
46Ti
36Ni
12Mn
6The hydride of (corresponding x=24) alloy three endotherm(ic)peaks all occur in heat-processed, and first endotherm(ic)peak appears at 320 ℃ of positions, and second and the 3rd dehydrogenation peak position are respectively 386 ℃ and 538 ℃.
Embodiment 4
The present invention is with Mg: Ti: Ni: Mn=38: 44: 12: 6 atomic ratio configures sample; take ratio of grinding media to material as 20: 1; rotating speed is to carry out mechanical ball milling in 300 rev/mins of situations; ball mill for the first time working time be 30 hours; then in vacuum glove box; under argon shield; open the ball grinder alloy and carry out break process; for preventing the sticking tank of powdered alloy and slimeball; from for the second time operation; every interval 10 hours alloy powder under argon shield is processed, and be 400 hours working time altogether.Secondly minute different time periods (at 50 hours, 100 hours, 200 hours, respectively getting one time sample in 400 hours) collected specimens, each sample that gathers is about 3g, and is constant for guaranteeing ratio of grinding media to material, accordingly abrading-ball taken out simultaneously when taking out sample each.Sample after the collection is crossed 200 mesh sieves through after grinding, and the magnesium-titanium-based hydrogen storage alloy after will sieving at last carries out XRD, PCT and DTA/TG test.The XRD test result as shown in Figure 4, Mg
38Ti
44Ni
12Mn
6Alloy is in 50 hour stage of ball milling, and phase structure is mainly by having HCP and the FCC structure forms in the mixture; When Ball-milling Time was 100 hours, the corresponding diffraction peak of Mn and Ni disappeared; After Ball-milling Time is increased to 200 hours, near 2 θ=43.1 °, 63.1 ° and 70.7 °, BCC structure phase appears; After Ball-milling Time was increased to 400 hours, the diffraction peak with HCP structure almost all disappeared, and simple substance is solid-solubilized in together mutually basically fully in the alloy, only occurs FCC and BCC structure in the alloy.DTA test result such as Fig. 5, among Fig. 5 through Mg behind 200 hours ball millings
38Ti
44Ni
12Mn
6The hydride of (corresponding x=32) alloy two endotherm(ic)peaks all occur in heat-processed, and these two endotherm(ic)peak positions are respectively 389 ℃ and 543 ℃.
Claims (5)
1. a BCC structure magnesium titanium base composite hydrogen storage alloy is characterised in that the chemical constitution of magnesium titanium base composite hydrogen storage alloy is Mg
70-xTi
12+xNi
12Mn
6, x=8 in the formula, 16,24,32.
2. a kind of preparation method of BCC structure magnesium titanium base composite hydrogen storage alloy as claimed in claim 1 is characterized in that preparation process is as follows:
1) under protection of inert gas, with purity all at the Mg more than 99.9%, Ti, Ni, Mn metal-powder according to Mg:Ti:Ni:Mn=(70-x): (12+x): the atomic ratio of 12:6, x=8 in the formula, 16,24,32, place ball grinder;
2) place ball grinder take ball material mass ratio as 20: 1 Stainless Steel Ball, wherein large ball is 4, and diameter is 8mm, and all the other diameters are respectively middle ball and the bead of 4mm and 2mm, and the number ratio of middle ball and bead is 1:1;
3) for the first time begin ball milling before, ball grinder is vacuumized, took out in advance 4 minutes first, then be filled with the 3atm argon gas, 3 times so repeatedly, carry out ball milling after being filled with at last the 3atm argon gas, Ball-milling Time is 30 hours for the first time;
4) since the ball milling second time, ball grinder was opened in 10 hours in every interval, and ball grinder is processed, and avoided powdered alloy to glue tank, was to carry out in vacuum glove box when opening ball grinder, and adding 1atm purity is 99.9% argon gas in the vacuum glove box;
5) rotating speed of planetary ball mill is 300 rev/mins in mechanical milling process, and every operation 30 minutes stops to reverse after 10 minutes again, and Ball-milling Time is 400 hours altogether, obtains BCC structure magnesium titanium base composite hydrogen storage alloy.
3. a kind of preparation method of BCC structure magnesium titanium base composite hydrogen storage alloy as claimed in claim 1, preparation process is as follows:
1) under protection of inert gas, with purity all at the Mg more than 99.9%, Ti, Ni, Mn metal-powder according to Mg:Ti:Ni:Mn=(70-24): (12+24): 12: 6 atomic ratio places ball grinder;
2) place ball grinder take ball material mass ratio as 20: 1 Stainless Steel Ball, wherein large ball is 4, and diameter is 8mm, and all the other diameters are respectively middle ball and the bead of 4mm and 2mm, and the number ratio of middle ball and bead is 1: 1;
3) for the first time begin ball milling before, ball grinder is vacuumized, took out in advance 4 minutes first, then be filled with the 3atm argon gas, 3 times so repeatedly, carry out ball milling after being filled with at last the 3atm argon gas, Ball-milling Time is 30 hours for the first time;
4) since the ball milling second time, ball grinder was opened in 10 hours in every interval, and ball grinder is processed, and avoided powdered alloy to glue tank, was to carry out in vacuum glove box when opening ball grinder, and adding 1atm purity is 99.9% argon gas in the vacuum glove box;
5) rotating speed of planetary ball mill is 300 rev/mins in mechanical milling process, and every operation 30 minutes stops to reverse after 10 minutes again, and Ball-milling Time is 200 hours altogether, obtains BCC structure magnesium titanium base composite hydrogen storage alloy.
4. a kind of preparation method of BCC structure magnesium titanium base composite hydrogen storage alloy as claimed in claim 1, preparation process is as follows:
1) under protection of inert gas, with purity all at the Mg more than 99.9%, Ti, Ni, Mn metal-powder according to Mg:Ti:Ni:Mn=(70-24): (12+24): 12: 6 atomic ratio places ball grinder;
2) place ball grinder take ball material mass ratio as 20: 1 Stainless Steel Ball, wherein large ball is 4, and diameter is 8mm, and all the other diameters are respectively middle ball and the bead of 4mm and 2mm, and the number ratio of middle ball and bead is 1:1;
3) for the first time begin ball milling before, ball grinder is vacuumized, took out in advance 4 minutes first, then be filled with the 3atm argon gas, 3 times so repeatedly, carry out ball milling after being filled with at last the 3atm argon gas, Ball-milling Time is 30 hours for the first time;
4) since the ball milling second time, ball grinder was opened in 10 hours in every interval, and ball grinder is processed, and avoided powdered alloy to glue tank, was to carry out in vacuum glove box when opening ball grinder, and adding 1atm purity is 99.9% argon gas in the vacuum glove box;
5) rotating speed of planetary ball mill is 300 rev/mins in mechanical milling process, and every operation 30 minutes stops to reverse after 10 minutes again, and Ball-milling Time is 200 hours altogether, obtains BCC structure magnesium titanium base composite hydrogen storage alloy.
5. require the purposes of 1 described a kind of BCC structure magnesium titanium base composite hydrogen storage alloy such as letter of authorization, it is characterized in that, be prepared into fuel cell with described magnesium titanium base composite hydrogen storage alloy, be mainly used in the Hydrogen Energy storage system.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103421996A (en) * | 2013-08-23 | 2013-12-04 | 苏州长盛机电有限公司 | Titanium-magnesium alloy material |
CN105132838A (en) * | 2015-09-25 | 2015-12-09 | 广西大学 | Regulation method of Mg17Al12 hydrogenation |
CN105603230A (en) * | 2016-03-22 | 2016-05-25 | 南京工程学院 | Method for preparing dispersed reinforced phase light Mg-Ti solid solution |
-
2012
- 2012-11-05 CN CN2012104346033A patent/CN102925773A/en active Pending
Non-Patent Citations (1)
Title |
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栏志强等: "Mg-Ti基bcc结构固溶体的制备与性能研究", 《功能材料》 * |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103421996A (en) * | 2013-08-23 | 2013-12-04 | 苏州长盛机电有限公司 | Titanium-magnesium alloy material |
CN103421996B (en) * | 2013-08-23 | 2015-07-15 | 苏州长盛机电有限公司 | Titanium-magnesium alloy material |
CN105132838A (en) * | 2015-09-25 | 2015-12-09 | 广西大学 | Regulation method of Mg17Al12 hydrogenation |
CN105603230A (en) * | 2016-03-22 | 2016-05-25 | 南京工程学院 | Method for preparing dispersed reinforced phase light Mg-Ti solid solution |
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Application publication date: 20130213 |