CN111830071A - Sample stage for in-situ electrochemical X-ray diffraction analysis - Google Patents
Sample stage for in-situ electrochemical X-ray diffraction analysis Download PDFInfo
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- CN111830071A CN111830071A CN201910276088.2A CN201910276088A CN111830071A CN 111830071 A CN111830071 A CN 111830071A CN 201910276088 A CN201910276088 A CN 201910276088A CN 111830071 A CN111830071 A CN 111830071A
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- 238000002441 X-ray diffraction Methods 0.000 title claims abstract description 20
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 9
- 239000007772 electrode material Substances 0.000 claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 17
- 238000013461 design Methods 0.000 claims abstract description 7
- 238000007789 sealing Methods 0.000 claims description 12
- 238000002474 experimental method Methods 0.000 claims description 6
- 238000003487 electrochemical reaction Methods 0.000 claims description 5
- 241000270722 Crocodylidae Species 0.000 claims description 4
- LNNWVNGFPYWNQE-GMIGKAJZSA-N desomorphine Chemical compound C1C2=CC=C(O)C3=C2[C@]24CCN(C)[C@H]1[C@@H]2CCC[C@@H]4O3 LNNWVNGFPYWNQE-GMIGKAJZSA-N 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 2
- 230000035945 sensitivity Effects 0.000 claims description 2
- 238000004458 analytical method Methods 0.000 abstract description 7
- 238000000155 in situ X-ray diffraction Methods 0.000 abstract description 7
- 238000000034 method Methods 0.000 abstract description 6
- 238000011160 research Methods 0.000 abstract description 3
- 239000013078 crystal Substances 0.000 abstract description 2
- 229910021645 metal ion Inorganic materials 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 238000010325 electrochemical charging Methods 0.000 abstract 1
- 238000010326 electrochemical discharging Methods 0.000 abstract 1
- 238000004154 testing of material Methods 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 13
- 238000007599 discharging Methods 0.000 description 4
- 241000270728 Alligator Species 0.000 description 2
- 239000004697 Polyetherimide Substances 0.000 description 2
- 238000000840 electrochemical analysis Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000005192 partition Methods 0.000 description 2
- 229920001601 polyetherimide Polymers 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000004696 Poly ether ether ketone Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- JUPQTSLXMOCDHR-UHFFFAOYSA-N benzene-1,4-diol;bis(4-fluorophenyl)methanone Chemical compound OC1=CC=C(O)C=C1.C1=CC(F)=CC=C1C(=O)C1=CC=C(F)C=C1 JUPQTSLXMOCDHR-UHFFFAOYSA-N 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 238000011066 ex-situ storage Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920002530 polyetherether ketone Polymers 0.000 description 1
- 229920006254 polymer film Polymers 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 239000012780 transparent material Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
- G01N23/20025—Sample holders or supports therefor
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- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The invention discloses a sample stage for in-situ electrochemical X-ray diffraction analysis, which belongs to the field of material testing and research, can perform in-situ X-ray diffraction analysis on a metal ion battery electrode material in the two-electrode and three-electrode electrochemical charging and discharging processes, performs tracking analysis on the crystal structure, chemical change and stress of the material, is suitable for the X-ray diffraction analysis instrument commonly used at present, and realizes the X-ray diffraction analysis at any angle through the design of an anode fixing piece and a semicircular window.
Description
Technical Field
The invention relates to the field of experimental equipment capable of carrying out in-situ X-ray diffraction analysis on a material under an electrochemical condition, in particular to experimental equipment for carrying out in-situ X-ray diffraction analysis on a metal ion battery electrode material under a charging and discharging condition.
Background
In order to improve the performance and service life of the battery, researchers need to perform detailed analysis and research on the changes of the electrode material in the charging and discharging processes, and through X-ray diffraction analysis, the information such as the crystal form change of the electrode material, the generation of new substances, the particle size change of the material, the stress change involved in the charging and discharging processes and the like can be obtained, so that the method is an effective and practical research means. At present, for the X-ray diffraction analysis of an electrode material, an ex-situ method is mainly adopted, namely, a battery material is charged and discharged to a certain degree, then the charging and discharging control is cut off, after the battery is opened, the electrode material is taken out, and the X-ray diffraction analysis is carried out on the electrode material directly or after cleaning and drying. The device that can carry out the normal position experiment can improve above-mentioned non-normal position test often can not accurately reflect the problem of electrode material actual conditions, though the device that can be used for carrying out the normal position experiment has aroused extensive concern, but still there are some inadequacies, chinese utility model patent that the grant official publication is CN 207541001U discloses "a lithium air battery normal position X ray diffraction testing arrangement", the utility model relates to a device is because gas feed and export are located the testing arrangement both sides, the integrated device is not applicable to and puts in the X ray diffractometer of present comparatively commonly used, and because positive grade mainboard and negative pole mainboard do not leave the interface of external electrochemistry workstation, bring a great deal of difficulty for the test of reality. The invention patent with the grant publication number of CN 102435625B discloses an X-ray diffraction in-situ test method and a sample holder, wherein a part of the device is composed of a polymer film, the sealing mode of the device is used for preventing the device from being reused, only two-electrode tests can be carried out, and the device is greatly influenced by the environment during measurement. In conclusion, the device which can accurately regulate and control the electrochemical reaction by the three-electrode method and perform the in-situ electrochemical X-ray diffraction analysis on the basis is still absent. In order to make up for the defects of the existing testing method and enable the in-situ X-ray diffraction analysis means to become a favorable tool for researching electrochemical reaction and new energy batteries, the patent provides a sample table device capable of carrying out two-electrode and three-electrode electrochemical tests, and the device can be used for carrying out in-situ X-ray diffraction experiments under electrochemical conditions (the incident angle is between 0 and 45 degrees). The design of the sample table has universality, the appearance of the sample table can be conveniently changed so as to be suitable for different X-ray diffraction instruments, and meanwhile, the sample table is simple and convenient to assemble, good in repeated measurement stability and capable of being repeatedly used for a long time.
Disclosure of Invention
As described above, aiming at the problem that the current in-situ electrochemical X-ray diffraction analysis lacks a proper sample stage, the present invention provides a sample stage for in-situ electrochemical X-ray diffraction analysis, which can perform an in-situ X-ray diffraction analysis experiment in a two-electrode or three-electrode electrochemical reaction without modifying a diffractometer, wherein the incident angle can be any angle interval between 0 and 45 degrees, and in order to achieve the above purpose, the present invention adopts the following technical scheme: the sample table can be directly placed in a diffractometer by matching the design of parameters such as the size, the thickness and the like of the appearance of the sample table main body (01) with a sample rod of a commercial X-ray diffractometer; the main external structure of the sample table is formed by a sample table main body (01), a semicircular window (02), an anode connecting port (03), a cathode connecting port (04) and a reference electrode connecting port (05), and is sealed by an O-shaped sealing ring and a sealing gasket, X-rays penetrate through the semicircular window (02) to enter a material to be tested below two small semicircular anode fixing pieces (06), then the X-rays are diffracted out of the semicircular window (02) and received by a detector of a diffractometer, and the low-angle X-rays can be blocked by an X-ray baffle plate (08) to improve the sensitivity of the detector; the semicircular window (02) is made of glass or PET, and the two materials have high X-ray transmittance and are stable to common organic solvents; the positive plate fixing screw (07) fixes the positive fixing plate (06) and the X-ray baffle plate (08) at the same time, the positive plate fixing screw (07), the positive fixing plate (06) and the X-ray baffle plate (08) are made of stainless steel materials, and the X-ray baffle plate (08) simultaneously plays a role in connecting the two positive fixing plates; an electrode material placing platform with adjustable height is arranged in the sample table main body (01) to place a negative electrode and a reference electrode, a semicircular window (02) is internally provided with a closed space, so that electrochemical reaction can be carried out in a specific atmosphere environment, and all parts of the sample table are sealed by a sealing ring or a sealing gasket.
The negative pole post (9) is contained in the sample platform main body (01), the partition plate (10) and the electrode material placing platform integrated with the reference electrode post (11), the negative pole material and the reference electrode can be placed on the negative pole post (9) and the reference electrode post (11) respectively, the diaphragm and the positive pole material are placed on the negative pole material and the reference electrode in sequence, the height of the electrode material placing platform can be adjusted through the rotation of the negative pole post fixing nut (13), the outer surface height of the electrode material to be researched is flush with the outer edge of the sample platform main body (01), and the X-ray diffraction experiment with the angle larger than 0 degree and smaller than 45 degrees can be carried out.
The positive electrode fixing piece (06) is composed of two small semi-circles, is placed in parallel, has a gap in the middle, and the distance of the gap is determined by the size of the positive electrode piece.
The X-ray baffle plate (08) can connect two positive fixing pieces (06) together, the lower end of the X-ray baffle plate is in a knife edge shape, the height of the X-ray baffle plate can be infinitely close to a sample to be detected, diffracted X-rays can be allowed to pass through the X-ray baffle plate, and the X-rays which may directly hit a detector can be blocked.
The sample table main body (01) is prepared from engineering plastics PEEK or PPS; the size and shape of the external profile are adjusted according to the X-ray powder diffractometer used so as to be suitable for different models of instruments.
The negative pole column fixing nut (13) adopts an internal thread design, is used for fixing the negative pole connecting port (04) and the negative pole column (09) by screwing threads, and simultaneously exerts pressure on the positive pole, the negative pole and the diaphragm assembled in the sample stage to play a role in compressing the positive pole, the negative pole and the diaphragm.
The positive electrode connecting port (03), the negative electrode connecting port (04) and the reference electrode connecting port (05) are respectively provided with a groove which is specially designed, and the groove can be directly connected with the crocodile clip to prevent the crocodile clip from falling off.
The contact part of the negative pole connecting port (04) and the negative pole column (09) is provided with a semicircular bulge design for reducing friction, and when the negative pole column fixing nut (13) is screwed, the negative pole column (09) does not rotate along with the negative pole connecting port (04).
The invention has the beneficial effects that the sample stage for X-ray diffraction test is provided, the sample stage can be used for carrying out two-electrode or three-electrode electrochemical regulation and control test on a material to be researched in a closed space and simultaneously collecting X-ray diffraction signals, the electrode material is arranged at the position which is parallel to the outer edge of the sample stage, the diffractometer detector can be allowed to collect the signals with the incident angle of 0-45 degrees, and the sample stage is simple to assemble and maintain and can be repeatedly used.
Drawings
The invention is further described with reference to the following figures and examples.
FIG. 1 is a front view of the overall appearance of a sample stage.
FIG. 2 is a front view of the main body of the sample stage.
Fig. 3 is a schematic perspective view (top view) of the sample stage body.
Fig. 4 is a perspective view (bottom view) of the main body of the sample stage.
FIG. 5 is a front view of the internal structure of the sample stage.
FIG. 6 is a perspective view of the internal structure of the sample stage.
FIG. 7 is a schematic top view of the internal structure of the sample stage.
FIG. 8 is a schematic perspective view of the internal reference electrode and negative electrode structure of the sample stage.
FIG. 9 is a front view of the structure of the reference electrode and the negative electrode inside the sample stage.
FIG. 10 is a perspective view of an X-ray baffle.
FIG. 11 is a perspective view of a semicircular window and a window key.
In the figure, 01, a sample table main body, 02, a semicircular window, 03, a positive electrode connecting port, 04, a negative electrode connecting port, 05, a reference electrode connecting port, 06, a positive electrode fixing piece, 07, a positive electrode piece fixing screw, 08. X-ray baffle plates, 09, a negative electrode column, 10, a separation plate, 11, a reference electrode column, 12, a reference electrode connecting column, 13, a negative electrode column fixing nut, 14, a sealing ring groove, 15, a window spoon, 16, a negative electrode column sealing ring groove and 17 are test material placing spaces.
Detailed Description
[ example 1 ]
As shown in fig. 1, the external main body of the sample stage according to the present invention is composed of a main body 01 of the sample stage and a semicircular window 02, wherein a positive electrode connection port 03, a negative electrode connection port 04 and a reference electrode connection port 05 are provided below the main body 01 (fig. 2, 3 and 4) of the sample stage for connecting with an additionally equipped alligator clip, and the alligator clip is connected with an external electrochemical workstation for precisely controlling current and voltage. The middle platform of the sample stage main body 01 (figure 2) is provided with threads (not shown in the figure) which are matched with the threads in the semicircular window 02, and the semicircular window 02 is sealed by the sealing ring sample stage main body 01 arranged in the sealing ring groove 14. The semicircular window 02 is made of transparent materials such as glass or PEI (polyetherimide) and the like so as to facilitate the entrance and exit of X-rays.
As shown in fig. 5 and 6, which are schematic views of the inside of the sample stage, the positive electrode fixing pieces 06 are fixed to the sample stage main body 01 by positive electrode piece fixing screws 07 and an X-ray blocking plate 08 (fig. 10), and a space is provided between the two positive electrode fixing pieces (fig. 7) for allowing X-rays to pass (arrows in fig. 6 indicate the incident and diffraction directions of the X-rays, respectively). Between the electrode material platform (fig. 8) composed of the negative pole column 09, the separator 10, and the reference pole column 11 and the positive pole fixing piece 06 is a test material placing space 17 for placing the positive pole, the negative pole, and the diaphragm. The negative electrode column 09 and the reference electrode column 11 are separated by a separator 10 and are usually assembled together as a single body. The reference electrode column 11 is connected with an external circuit through a reference electrode connecting column 12 and a reference electrode connecting port 05. The negative pole 09 is provided with a negative pole seal ring groove 16 (figure 9) for placing a seal ring to play a role in sealing.
When the electrode material storage platform is used, the electrode material storage platform consisting of the negative pole column 09, the partition plate 10 and the reference electrode column 11 is placed into the sample platform main body 01 in the glove box according to the connection mode, then the negative pole connecting port 04 and the negative pole column fixing nut 13 are installed, and the negative pole connecting port 04 is fixed through the negative pole column fixing nut 13 without being screwed down. And sequentially placing a negative electrode on the electrode material placing platform, and placing a reference electrode, a diaphragm and a positive electrode if a three-electrode test is carried out. Then, the positive electrode fixing piece 06 and the X-ray shield 08 are mounted and fixed by the positive electrode fixing screw 07. The positive electrode connection port 03 and the reference electrode connection port 05 are installed and the negative electrode post fixing screws 13 are tightened, at which time the negative electrode, the separator and the positive electrode should be tightly pressed against the positive electrode fixing piece 06. Finally, the semicircular window 02 is mounted (fig. 11) using a window key 15. And after the testing device is removed from the glove box, connecting the sample table to an external circuit to realize the in-situ X-ray diffraction spectrum test of the battery electrode material in an electrochemical test state.
Claims (8)
1. A sample stage for in situ electrochemical X-ray diffraction analysis, comprising: the sample table main body (01) is matched with a sample rod of a commercial X-ray diffractometer, a main external structure of the sample table is formed by a semicircular window (02), an anode connecting port (03), a cathode connecting port (04) and a reference electrode connecting port (05), X-rays penetrate through the semicircular window (02) to enter materials to be tested below two small semicircular anode fixing pieces (06) and then are diffracted out of the semicircular window (02), low-angle X-rays can be blocked by an X-ray baffle plate (08) to improve the sensitivity of a detector, the anode fixing piece (06) and the X-ray baffle plate (08) are simultaneously fixed by an anode piece fixing screw (07), an electrode material placing platform with adjustable height is arranged in the sample table main body (01) to place a cathode and a reference electrode, and all parts of the sample table are sealed by a sealing ring or a sealing gasket, the semicircular window (02) is provided with a closed space, so that the electrochemical reaction can be carried out in a specific atmosphere environment.
2. The sample stage of claim 1, wherein: the negative pole post (9), division board (10), reference electrode post (11) three electrode material place the platform as an organic whole are contained in foretell sample platform main part (01), negative pole material and reference electrode can be placed respectively on negative pole post (9) and reference electrode post (11), place diaphragm and anodal material on negative pole material and the reference electrode, electrode material place the platform highly can adjust through the rotation of negative pole post fixation nut (13), the surface height of the electrode material studied flushes with sample platform main part (01) outer edge, can carry out the X-ray diffraction experiment that is greater than 0 degree and is less than 45 degrees angles.
3. The sample stage of claim 1, wherein: the positive electrode fixing piece (06) is composed of two small semi-circles, is placed in parallel with a gap in the middle, the distance of the gap is determined by the size of the positive electrode slice, and at least allows X-rays to pass through, and the structure can allow X-rays with any angle to enter to study the electrode material.
4. The sample stage of claim 1, wherein: the X-ray baffle plate (08) can connect two positive fixing pieces (06) together, the lower end of the X-ray baffle plate is in a knife edge shape, the height of the X-ray baffle plate can be infinitely close to a tested sample, and simultaneously diffracted X-rays can be allowed to pass through and can be blocked from X-rays which may directly hit a detector.
5. A sample stage for in situ electrochemical X-ray diffraction analysis according to claims 1 and 4, wherein: the size and shape of the external outline of the sample stage main body (01) are adjusted according to the X-ray powder diffractometer used, so that the sample stage main body is suitable for instruments of different models.
6. The sample stage of claim 1, wherein: the negative pole column fixing nut (13) adopts an internal thread design, is used for fixing the negative pole connecting port (04) and the negative pole column (09) by screwing threads, and simultaneously exerts pressure on the positive pole, the negative pole and the diaphragm assembled in the sample stage to play a role in compressing the positive pole, the negative pole and the diaphragm.
7. The sample stage of claim 1, wherein: the positive electrode connecting port (03), the negative electrode connecting port (04) and the reference electrode connecting port (05) are respectively provided with a groove which is specially designed, and the groove can be directly connected with the crocodile clip to prevent the crocodile clip from falling off.
8. The sample stage of claim 1, wherein: the contact part of the negative pole connecting port (04) and the negative pole column (09) is provided with a semicircular bulge design for reducing friction, and when the negative pole column fixing nut (13) is screwed, the negative pole column (09) does not rotate along with the negative pole connecting port (04).
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910276088.2A CN111830071B (en) | 2019-04-14 | 2019-04-14 | Sample stage for in-situ electrochemical X-ray diffraction analysis |
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| CN201910276088.2A CN111830071B (en) | 2019-04-14 | 2019-04-14 | Sample stage for in-situ electrochemical X-ray diffraction analysis |
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| CN111830071B CN111830071B (en) | 2024-07-05 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112394096A (en) * | 2020-12-10 | 2021-02-23 | 南杰智汇(深圳)科技有限公司 | Novel three-electrode electrochemical testing device |
| CN112697863A (en) * | 2020-12-10 | 2021-04-23 | 南杰智汇(深圳)科技有限公司 | Electrochemical optical synchronous test sample table |
| CN114235621A (en) * | 2021-12-21 | 2022-03-25 | 吉林大学 | Energy storage material cycle life testing device and testing method |
| IT202200009386A1 (en) * | 2022-05-06 | 2023-11-06 | Univ Degli Studi Di Sassari | POLARIZATION AND MEASUREMENT CELL FOR PIEZOELECTRIC CERAMIC MATERIALS |
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| JP2015014569A (en) * | 2013-07-08 | 2015-01-22 | 国立大学法人京都大学 | X-ray diffractometer built-in atmosphere control glove box device and method for manufacturing the same |
| CN109406593A (en) * | 2018-09-28 | 2019-03-01 | 吉林大学 | Electrochemical in-situ reacts X ray test device |
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| CN103033474A (en) * | 2012-12-10 | 2013-04-10 | 中南大学 | Electrochemical-optical combined in-situ study spectral cell |
| JP2015014569A (en) * | 2013-07-08 | 2015-01-22 | 国立大学法人京都大学 | X-ray diffractometer built-in atmosphere control glove box device and method for manufacturing the same |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112394096A (en) * | 2020-12-10 | 2021-02-23 | 南杰智汇(深圳)科技有限公司 | Novel three-electrode electrochemical testing device |
| CN112697863A (en) * | 2020-12-10 | 2021-04-23 | 南杰智汇(深圳)科技有限公司 | Electrochemical optical synchronous test sample table |
| CN114235621A (en) * | 2021-12-21 | 2022-03-25 | 吉林大学 | Energy storage material cycle life testing device and testing method |
| CN114235621B (en) * | 2021-12-21 | 2024-04-16 | 吉林大学 | Device and method for testing cycle life of energy storage material |
| IT202200009386A1 (en) * | 2022-05-06 | 2023-11-06 | Univ Degli Studi Di Sassari | POLARIZATION AND MEASUREMENT CELL FOR PIEZOELECTRIC CERAMIC MATERIALS |
| WO2023214441A1 (en) * | 2022-05-06 | 2023-11-09 | Università Degli Studi Di Sassari | Polarisation and measurement cell for piezoelectric ceramic materials |
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| CN111830071B (en) | 2024-07-05 |
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