CN1580752A - Method and device for synchronized determining hydrogen storage alloy structure and tissue change during charging-discharing circle - Google Patents
Method and device for synchronized determining hydrogen storage alloy structure and tissue change during charging-discharing circle Download PDFInfo
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- CN1580752A CN1580752A CN 200410027217 CN200410027217A CN1580752A CN 1580752 A CN1580752 A CN 1580752A CN 200410027217 CN200410027217 CN 200410027217 CN 200410027217 A CN200410027217 A CN 200410027217A CN 1580752 A CN1580752 A CN 1580752A
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Abstract
The present invention provides a method for determining hydrogen storage alloy structure and tissue change in charge-discharge circulation process. Said method includes the following steps : in the charge-discharge circulation testing process for determining analog nickel-hydrogen secondary cell making X ray irradiate the analog cell negative electrode plate made of hydrogen storage alloy according to a certain diffraction angle, receiving diffraction signal and making real-time analysis. said invention also provides an equipment for implementing the said method. said equipment includes hydrogen storage characteristics tester, analog nickel-hydrogen secondary all whose negative electrode plate is hydrogen storage alloy and X-ray diffractometer. Said invention also provides the connection method of the said all the components.
Description
Technical field
The present invention relates to a kind of battery material device for detecting performance, particularly a kind of hydrogen bearing alloy structure and method and device thereof of organizing variation in simulating nickel-hydrogen secondary cell charge and discharge cycles test process, measured synchronously.
Background technology
Face global range more and more serious environmental pollution and energy crisis; it is one of urgent task of facing of the mankind that little and new forms of energy that can regenerate are polluted in exploitation; the practicability and the commercialization of the discovery of hydrogen bearing alloy and utilization and the Ni-MH secondary cell developed on this basis are the important breakthroughs that obtains as the development and use aspect of raw-material Hydrogen Energy with water.At present, the Ni-MH battery of making the negative pole making of hydrogen storage material obtains to use very widely in production, various fields in life, becomes one of necessity of the daily productive life of people.Continuous development and progress along with science and technology, more and more to the secondary cell demand, requirement to product quality is also more and more higher, capacity and life-span to secondary cell constantly propose higher requirement, therefore need further develop and have more high performance hydrogen bearing alloy, thereby obtain high capacity, long-life battery as cell negative electrode material.The electric automobile that with the Hydrogen Energy is power resources is to develop one of very fast industry in recent years, wherein the technical bottleneck of most critical is the manufacturing of the secondary cell of high specific energy (50Wh/kg), high specific power (150W/kg), and the hydrogen storage material how to obtain to be suitable for is the emphasis of current research work.The periodic duty life-span of hydrogen bearing alloy is whether the decision material has one of the factor of the most critical of practical value, in continuous charge and discharge cycles process, unit cell volume expands bigger behind the absorption hydrogen, easily efflorescence, specific surface increases thereupon, thereby increases the chance of alloy oxidation, because the oxidized corrosion of hydrogen storage electrode material, cause electrode capacity to reduce gradually, make alloy lose suction too early and put Hydrogen Energy power, thereby cause battery failure.Cycle index when the periodic duty life-span of electrode is reduced to a certain particular value with the capacity of electrode is usually measured.At present, people are in the periodic duty of analyzing hydrogen bearing alloy during the life-span, normally drop to certain numerical value according to the cycle life curve top electrode capacity of battery after, hydrogen storage material is taken out, by structured testing and structure observation, judge and cause material to inhale the reason of putting the decay of Hydrogen Energy power.This indirect conclusion that analytical approach drew, often can't reflect the variation of hydrogen storage electrode material tissue, structure and surface state in continuous charge and discharge cycles process truly, for example is (1) hydrogen storage material inhaled hydrogen and is put how lattice dimensions and stress change in the hydrogen process at each round-robin? this is a key of explaining material efflorescence reason; Beginning to occur tangible oxidation corrosion when (2) hydrogen storage electrode material is experience how many times charge and discharge cycles, how are the degree of generation oxidation corrosion and the corresponding relation of electrode capacity at that time? and this analyzes most critical and the most important foundation that causes the battery failure reason just.But also be not specifically designed to analog detection method and the device that in the cyclic process of test simulation charging/discharging of secondary cell, carries out structured testing and fabric analysis at present.
Summary of the invention
The objective of the invention is to overcome the shortcoming of prior art, provide a kind of simple to operate, use and in simulation nickel-hydrogen secondary cell charge and discharge cycles test process, to measure the method that hydrogen bearing alloy structure and tissue change easily synchronously.
Another object of the present invention is to provide a kind of device of realizing said method.
Purpose of the present invention is achieved through the following technical solutions: measure the hydrogen bearing alloy structure in this charge and discharge cycles process synchronously and comprise the steps: simulation nickel-hydrogen secondary cell is being carried out in the charge and discharge cycles test process with the method that tissue changes, X ray is shone the cell negative electrode plate that hydrogen bearing alloy is made with certain angle of diffraction, and the reception diffracted signal, thereby the tissue and the structure of hydrogen bearing alloy are tested also real-time analysis.
Described angle of diffraction is 20 °～150 °.
Described real-time analysis is meant when simulation nickel-hydrogen secondary cell is carried out the charge and discharge cycles test, hydrogen bearing alloy is carried out X-ray diffraction analysis, obtain tissue, crystallite dimension, the variation of stress state and the information such as formation of oxide of hydrogen bearing alloy, thereby set up direct quantitative relationship between the chemical property of hydrogen bearing alloy changes in microstructure and simulation nickel-hydrogen secondary cell changes in the charge and discharge cycles process.
Measure the hydrogen bearing alloy structure in the charge and discharge cycles process of realization said method synchronously and comprise that with the device of organizing variation hydrogen storage property tester, negative plate are the simulation nickel-hydrogen secondary cell of hydrogen bearing alloy, described simulation nickel-hydrogen secondary cell is connected with the hydrogen storage property tester, it is characterized in that: comprise X-ray diffractometer, described X-ray diffractometer and described simulation nickel-hydrogen secondary cell are oppositely arranged.
Described simulation nickel-hydrogen secondary cell is arranged in the seal box, described seal box is provided with the X ray test window, the seal box that simulation nickel-hydrogen secondary cell is housed is placed on the sample stage of X-ray diffractometer, X ray transmitted X-rays test window is radiated on the hydrogen storage alloy negative sheet of simulation nickel-hydrogen secondary cell.
Described seal box comprises lid and box body, and lid links together with thread connecting mode and box body, and described lid is provided with the X ray test window, beryllium glass thin slice or wheat is installed on the X ray test window draws (miller) film; One cavity is arranged in the described box body, be provided with sample support plate, location adjustment means in cavity, described sample support plate is connected with box body by the location adjustment means.
Described location adjustment means comprises banking stop, elasticity adjusting part, and described elasticity adjusting part apical grafting is in sample support plate bottom, and banking stop is arranged between sample support plate and the lid; Described elasticity adjusting part cooperates with banking stop and is fixed the sample support plate, and the depth of parallelism of scalable sample support plate and X ray test window, because the upper end of sample support plate forms sample chamber, described negative plate is that the simulation nickel-hydrogen secondary cell of hydrogen bearing alloy is positioned in the sample chamber, the depth of parallelism of tested negative plate of essence scalable (hydrogen bearing alloy) and X ray test window so the elasticity adjusting part matches with banking stop.
Described elasticity adjusting part is socketed on the positioning screw by retainer spring and constitutes.
Described lid and box body surface of contact are provided with O-ring seal, so that lid and box body are tightly connected.
Described box body is provided with positive terminal, negative terminal A, positive terminal and box body short circuit, the insulation of negative terminal A and box body, described sample support plate is provided with negative terminal B, is connected with conductive material between negative terminal A and the negative terminal B; The simulation electrode that described simulated battery is made up of negative plate (hydrogen bearing alloy), diaphragm paper and positive plate places the sample chamber that fills an amount of electrolytic solution to constitute, its negative plate is connected with negative terminal A, negative terminal B, positive plate is connected with positive terminal, and described positive terminal is connected with negative pole with the positive pole of hydrogen storage property tester respectively with negative terminal A.
The relative prior art of the present invention has following advantage and effect: the inventive method and device are by utilizing x-ray bombardment to be in the hydrogen bearing alloy of charge and discharge cycles test mode and receiving diffracted signal, directly measuring lattice dimensions and stress state changes, and electrode surface degree of oxidation, by of the contrast of above-mentioned parameter with the electrode electrical property parameter that utilizes the hydrogen storage property tester to measure, can set up the corresponding relation curve between alloy pulverization-anodizing-electrode capacity three, provide directly full and accurate experimental basis for analyzing the factor cause hydrogen storage electrode material to inhale to put the reason of Hydrogen Energy power decay and influence cycle life all-sidedly and accurately, can to exploitation have more the high electrode capacity and more the hydrogen storage electrode material of long circulation life the important techniques assurance is provided.
Description of drawings
Fig. 1 is the principle of work synoptic diagram of apparatus of the present invention.
Fig. 2 is the structural representation that the seal box of simulation secondary cell is housed.
Embodiment
The present invention is described in further detail below in conjunction with embodiment and accompanying drawing, but embodiments of the present invention are not limited thereto.
Embodiment
Fig. 1 and Fig. 2 show the specific embodiment of the present invention, as seen from Figure 1, apparatus of the present invention comprise hydrogen storage property tester 20, the seal box of simulation nickel-hydrogen secondary cell are housed, X-ray diffractometer 16, hydrogen storage property tester 20 is connected with the seal box that simulation nickel-hydrogen secondary cell is housed, and described seal box places on the horizontal sample platform 19 of X-ray diffractometer 16; Wherein hydrogen storage property tester 20 can adopt the CPI type hydrogen storage property tester that United States advanced Materials Co., Ltd (Advanced Materials Corporation) produces; X-ray diffractometer 16 can adopt Philips X ' Pert Pro type X-ray diffractometer.
The described seal box that simulation nickel-hydrogen secondary cell is housed comprises lid 4 and box body 1, and lid 4 links together with thread connecting mode and box body 1, is provided with O-ring seal 10 at lid 4 and box body 1 surface of contact, and lid 4 and box body 1 are tightly connected; Described lid 4 is provided with X ray test window 7, and the beryllium glass thin slice is installed on X ray test window 7; In the described box body 1 cavity is arranged, in cavity, be provided with sample support plate 3, location adjustment means, described sample support plate 3 is connected with box body 1 by the location adjustment means, described location adjustment means comprises banking stop 5, elasticity adjusting part, described elasticity adjusting part apical grafting is in sample support plate 3 bottoms, and banking stop 5 is arranged between sample support plate 3 and the lid 4; Described elasticity adjusting part cooperates with banking stop 5 and is fixed sample support plate 3, and the depth of parallelism of scalable sample support plate 3 and X ray test window 7, because the upper end of sample support plate 3 forms sample chamber 8, described negative plate 15 is positioned in the sample chamber 8 for the positive and negative plate of the simulation nickel-hydrogen secondary cell of hydrogen bearing alloy, the tested negative plate 15 (hydrogen bearing alloy) of essence scalable and the depth of parallelism of X ray test window 7 so the elasticity adjusting part matches with banking stop 5; Described elasticity adjusting part is socketed on the positioning screw 2 by retainer spring 14 and constitutes; Described box body 1 is provided with positive terminal 12, negative terminal 13, positive terminal 12 and box body 1 short circuit, negative terminal 13 and box body insulation, described sample support plate 3 is provided with negative terminal 11, is connected with conductive material between negative terminal 11 and the negative terminal 13; The simulation electrode that described simulation nickel-hydrogen secondary cell is made up of negative plate (hydrogen bearing alloy) 15, diaphragm paper and positive plate places the sample chamber 8 that fills an amount of electrolytic solution to constitute, its negative plate 15 is connected with negative terminal 11, negative terminal 13, positive plate is connected with positive terminal 12, and described positive terminal 12 is connected with negative pole with the positive pole of hydrogen storage property tester 20 respectively with negative terminal 13.
The aforementioned seal box that simulation nickel-hydrogen secondary cell is housed is lain in a horizontal plane on the horizontal sample platform 19 of X-ray diffractometer 16, suitably adjust by horizontal sample platform 19 X-ray diffractometer 16, make X ray that x ray generator 17 sends with certain angle of diffraction by the beryllium glass thin slice on the X ray test window 7 on the lid 4 of seal box, be radiated at the surface of cell negative electrode plate 15, and utilize angular instrument 18 to receive diffracted signal, thereby the tissue and the structure of anticathode sheet (hydrogen bearing alloy) 15 are tested, lattice dimensions to hydrogen bearing alloy, the variation of stress state, and the oxidation situation is carried out real-time analysis, set up the corresponding relation curve between alloy pulverization-anodizing-electrode capacity three, cause the reason that the decay of Hydrogen Energy power is put in the hydrogen storage electrode material suction to provide directly full and accurate experimental basis with the factor that influences cycle life for analyzing all-sidedly and accurately.
Claims (10)
1, a kind of hydrogen bearing alloy structure and method of organizing variation in the charge and discharge cycles process, measured synchronously, it is characterized in that comprising the steps: simulation nickel-hydrogen secondary cell is being carried out in the charge and discharge cycles test process, X ray is shone the cell negative electrode plate that hydrogen bearing alloy is made with certain angle of diffraction, and the reception diffracted signal, the tissue and the structure of hydrogen bearing alloy are tested also real-time analysis.
2, hydrogen bearing alloy structure and the method for organizing variation in the charge and discharge cycles process, measured synchronously according to claim 1, it is characterized in that: described real-time analysis is meant when simulation nickel-hydrogen secondary cell is carried out the charge and discharge cycles test, hydrogen bearing alloy is carried out X-ray diffraction analysis, obtain tissue, crystallite dimension, the variation of stress state and the information of oxidation situation of hydrogen bearing alloy, thereby set up direct quantitative relationship between the chemical property of hydrogen bearing alloy changes in microstructure and simulation nickel-hydrogen secondary cell changes in the charge and discharge cycles process.
3, hydrogen bearing alloy structure and the method for organizing variation measured synchronously in the charge and discharge cycles process according to claim 1, it is characterized in that: described x-ray diffraction angle is 20 °～150 °.
4, a kind of hydrogen bearing alloy structure and device of organizing variation in the charge and discharge cycles process, measured synchronously, comprise that hydrogen storage property tester, negative plate are the simulation nickel-hydrogen secondary cell of hydrogen bearing alloy, described simulation nickel-hydrogen secondary cell is connected with the hydrogen storage property tester, it is characterized in that: comprise X-ray diffractometer, described X-ray diffractometer and described simulation nickel-hydrogen secondary cell are oppositely arranged.
5, hydrogen bearing alloy structure and the device of organizing variation in the charge and discharge cycles process, measured synchronously according to claim 4, it is characterized in that: described simulation nickel-hydrogen secondary cell is arranged in the seal box, described seal box is provided with the X ray test window, described seal box places on the sample stage of X-ray diffractometer, and X ray transmitted X-rays test window is radiated on the hydrogen storage alloy negative sheet of simulation nickel-hydrogen secondary cell.
6, hydrogen bearing alloy structure and the device of organizing variation in the charge and discharge cycles process, measured synchronously according to claim 5, it is characterized in that: described seal box comprises lid and box body, lid links together with thread connecting mode and box body, described lid is provided with the X ray test window, and beryllium glass thin slice or miller film are installed on the X ray test window; One cavity is arranged in the described box body, be provided with sample support plate, location adjustment means in cavity, described sample support plate is connected with box body by the location adjustment means.
7, hydrogen bearing alloy structure and the device of organizing variation in the charge and discharge cycles process, measured synchronously according to claim 6, it is characterized in that: described location adjustment means comprises banking stop, elasticity adjusting part, described elasticity adjusting part apical grafting is in sample support plate bottom, and banking stop is arranged between sample support plate and the lid; Described elasticity adjusting part cooperates with banking stop and is fixed the sample support plate.
8, hydrogen bearing alloy structure and the device of organizing variation measured synchronously in the charge and discharge cycles process according to claim 7, it is characterized in that: described elasticity adjusting part is socketed on the positioning screw by retainer spring and constitutes.
9, hydrogen bearing alloy structure and the device of organizing variation measured synchronously in the charge and discharge cycles process according to claim 6, it is characterized in that: described lid and box body surface of contact are provided with O-ring seal.
10, hydrogen bearing alloy structure and the device of organizing variation in the charge and discharge cycles process, measured synchronously according to claim 6, it is characterized in that: described box body is provided with positive terminal, negative terminal A, positive terminal and box body short circuit, negative terminal A and box body insulation, described sample support plate is provided with negative terminal B, is connected with conductive material between negative terminal A and the negative terminal B; The simulation electrode that described simulated battery is made up of negative plate, diaphragm paper and positive plate places the sample chamber that fills an amount of electrolytic solution to constitute, its negative plate is connected with negative terminal A, negative terminal B, positive plate is connected with positive terminal, and described positive terminal is connected with negative pole with the positive pole of hydrogen storage property tester respectively with negative terminal A.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410027217 CN1580752A (en) | 2004-05-17 | 2004-05-17 | Method and device for synchronized determining hydrogen storage alloy structure and tissue change during charging-discharing circle |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410027217 CN1580752A (en) | 2004-05-17 | 2004-05-17 | Method and device for synchronized determining hydrogen storage alloy structure and tissue change during charging-discharing circle |
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| CN1580752A true CN1580752A (en) | 2005-02-16 |
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| CN 200410027217 Pending CN1580752A (en) | 2004-05-17 | 2004-05-17 | Method and device for synchronized determining hydrogen storage alloy structure and tissue change during charging-discharing circle |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100371711C (en) * | 2005-04-27 | 2008-02-27 | 中国科学院金属研究所 | Method for accurate testing performance of pressure concentration-temperature of hydrogen storage material |
| CN102435625A (en) * | 2011-12-27 | 2012-05-02 | 东莞新能源科技有限公司 | Method and sample shelf for X-ray diffraction in-situ test |
| CN104597064A (en) * | 2014-12-30 | 2015-05-06 | 北大先行科技产业有限公司 | Electrochemical analysis in-situ cell for X-ray diffraction and testing method |
| CN105319230A (en) * | 2015-12-10 | 2016-02-10 | 黄冈师范学院 | In-situ XRD battery test sealing box |
| CN107910582A (en) * | 2017-11-23 | 2018-04-13 | 福建师范大学 | X-ray diffractometer original position cell apparatus and its assemble method |
| CN108427049A (en) * | 2018-03-09 | 2018-08-21 | 合肥国轩高科动力能源有限公司 | A method of lithium ion battery material performance is judged based on crystallite dimension |
| CN109696403A (en) * | 2017-10-23 | 2019-04-30 | 中国科学院重庆绿色智能技术研究院 | A kind of sample room for immersion micro-imaging |
-
2004
- 2004-05-17 CN CN 200410027217 patent/CN1580752A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100371711C (en) * | 2005-04-27 | 2008-02-27 | 中国科学院金属研究所 | Method for accurate testing performance of pressure concentration-temperature of hydrogen storage material |
| CN102435625A (en) * | 2011-12-27 | 2012-05-02 | 东莞新能源科技有限公司 | Method and sample shelf for X-ray diffraction in-situ test |
| CN104597064A (en) * | 2014-12-30 | 2015-05-06 | 北大先行科技产业有限公司 | Electrochemical analysis in-situ cell for X-ray diffraction and testing method |
| CN105319230A (en) * | 2015-12-10 | 2016-02-10 | 黄冈师范学院 | In-situ XRD battery test sealing box |
| CN109696403A (en) * | 2017-10-23 | 2019-04-30 | 中国科学院重庆绿色智能技术研究院 | A kind of sample room for immersion micro-imaging |
| CN109696403B (en) * | 2017-10-23 | 2021-08-13 | 中国科学院重庆绿色智能技术研究院 | Sample chamber for immersed microscopic imaging |
| CN107910582A (en) * | 2017-11-23 | 2018-04-13 | 福建师范大学 | X-ray diffractometer original position cell apparatus and its assemble method |
| CN108427049A (en) * | 2018-03-09 | 2018-08-21 | 合肥国轩高科动力能源有限公司 | A method of lithium ion battery material performance is judged based on crystallite dimension |
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