CN116626140A - Material tolerance test device and use method thereof - Google Patents
Material tolerance test device and use method thereof Download PDFInfo
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- CN116626140A CN116626140A CN202310633723.4A CN202310633723A CN116626140A CN 116626140 A CN116626140 A CN 116626140A CN 202310633723 A CN202310633723 A CN 202310633723A CN 116626140 A CN116626140 A CN 116626140A
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- 238000012360 testing method Methods 0.000 title claims abstract description 80
- 239000000463 material Substances 0.000 title claims abstract description 60
- 238000000034 method Methods 0.000 title claims abstract description 38
- 239000003792 electrolyte Substances 0.000 claims abstract description 59
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 41
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000002253 acid Substances 0.000 claims abstract description 14
- 210000005056 cell body Anatomy 0.000 claims description 44
- 210000004027 cell Anatomy 0.000 claims description 33
- 238000005868 electrolysis reaction Methods 0.000 claims description 26
- 239000007788 liquid Substances 0.000 claims description 25
- 239000012528 membrane Substances 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 238000007789 sealing Methods 0.000 claims description 10
- 230000001590 oxidative effect Effects 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 229910001456 vanadium ion Inorganic materials 0.000 claims description 6
- UQSQSQZYBQSBJZ-UHFFFAOYSA-N fluorosulfonic acid Chemical group OS(F)(=O)=O UQSQSQZYBQSBJZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000012544 monitoring process Methods 0.000 claims description 2
- 230000001502 supplementing effect Effects 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 abstract description 9
- 238000007254 oxidation reaction Methods 0.000 abstract description 9
- 230000009467 reduction Effects 0.000 abstract description 6
- 239000000243 solution Substances 0.000 description 17
- 210000003339 pole cell Anatomy 0.000 description 6
- 239000007789 gas Substances 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 238000013022 venting Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
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- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
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- 239000007800 oxidant agent Substances 0.000 description 1
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- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
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- 230000004044 response Effects 0.000 description 1
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- 238000003860 storage Methods 0.000 description 1
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- 239000000725 suspension Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 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
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
- G01N17/02—Electrochemical measuring systems for weathering, corrosion or corrosion-protection measurement
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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Abstract
The application provides a material tolerance testing device and a using method thereof, wherein the testing device comprises a tank body, a diaphragm and a sample placing piece for placing a sample to be tested, the tank body comprises an anode tank body and a cathode tank body, an anode plate is arranged in the anode tank body, and a cathode plate is arranged in the cathode tank body; the anode plate and the cathode plate are used for switching on a power supply to electrolyze electrolyte in the anode tank body and the cathode tank body; the diaphragm is arranged between the anode tank body and the cathode tank body; the sample placing piece is arranged in the anode tank body and/or the cathode tank body. The application can simultaneously meet the test requirements of materials, especially vanadium battery materials, on the acid resistance, the oxidation resistance and the reduction resistance of electrolyte.
Description
Technical Field
The application mainly relates to the technical field of vanadium batteries, in particular to a material tolerance testing device and a using method thereof.
Background
The all-vanadium redox flow battery (VFB, vanadium battery or vanadium battery system) is a high-efficiency energy storage battery, is a redox battery taking vanadium as an active material and in a circulating flowing liquid state, and has the outstanding advantages of mutually independent and adjustable system capacity and power, quick response, safety, reliability, environmental friendliness, long cycle life, easiness in maintenance, reproducibility and the like. All-vanadium redox flow batteries become one of the most promising technologies in renewable energy power generation, peak clipping and valley filling of power grids, large-scale energy storage of emergency and standby power stations and the like.
The all-vanadium redox flow battery mainly comprises a capacity unit, a power unit, a control unit, a conveying unit and the like. In a vanadium battery system, there are a wide variety of parts and devices that are in direct contact with the vanadium electrolyte and do not provide a circuit path (electrode, plate, separator), such as: electrolyte storage tank in capacity unit, flow frame, sealing member (such as runner apron, O circle, rubber pad etc.) in the power unit, pipeline, pump, valve and heat exchanger etc. in the delivery unit. The degree of the tolerance (acid corrosion resistance, oxidation resistance, reduction resistance and the like) of the materials of the parts and the equipment to the electrolyte directly influences the composition components of the vanadium electrolyte and the service lives of the parts and the equipment, so that the overall electrical performance and the service life of the vanadium battery are further influenced.
The electrode material used as the all-vanadium redox flow battery has the advantages of strong oxidation resistance, strong acidity, low resistance, good conductivity, high mechanical strength, good electrochemical activity and the like, so the electrode material is particularly important for the material tolerance test of the all-vanadium redox flow battery.
At present, in the all-vanadium redox flow battery industry, a soaking method is mainly adopted as a method for testing material tolerance, namely, a material sample is soaked in vanadium electrolyte for a period of time, and then the material performance is evaluated through a weighing method and an observation method. However, the method only has a certain evaluation effect on acid corrosion resistance, and in the use process of the vanadium battery, a solution system facing the material has not only acidity, but also oxidability and reducibility according to different charge and discharge states, but also does not have a tolerance test device capable of simultaneously meeting the acid resistance, the oxidation resistance and the reducibility of the vanadium battery material to vanadium electrolyte.
Disclosure of Invention
The application aims to solve the technical problem of providing a material tolerance testing device and a using method thereof, which can simultaneously meet the testing requirements of materials, particularly vanadium battery materials, on acid resistance, oxidation resistance and reduction resistance of electrolyte.
To solve the above technical problem, in a first aspect, the present application provides a material tolerance testing device, including: the cell body comprises an anode cell body and a cathode cell body; wherein an anode plate is arranged in the anode tank body, and a cathode plate is arranged in the cathode tank body; the anode plate and the cathode plate are used for being powered on to electrolyze electrolyte in the anode tank body and the cathode tank body; a separator disposed between the anode cell body and the cathode cell body; the sample placing piece is used for placing a sample to be tested and is arranged in the anode tank body and/or the cathode tank body.
Optionally, the anode tank body and/or the cathode tank body are/is provided with a cover plate, and the cover plate is matched with the anode tank body and/or the cathode tank body and is used for sealing the opening of the anode tank body and/or the opening of the cathode tank body.
Optionally, one side of the cover plate is movably connected with one side of the anode tank body and/or one side of the cathode tank body, or the cover plate is of an independent structure separated from the anode tank body and the cathode tank body.
Optionally, a breather valve is further provided, and the breather valve is provided on the cover plate.
Optionally, a liquid inlet valve is further provided, and the liquid inlet valve is arranged on the cover plate.
Optionally, the membrane is a perfluorosulfonic acid proton membrane.
Optionally, the sample placing piece comprises a tank network and at least one sample cage, wherein the tank network is arranged inside the anode tank body and/or the cathode tank body, and the tank network is connected with the sample cage.
Optionally, the sample cage has a hanger that is hung from the trough net.
Optionally, the anode tank body and the cathode tank body are respectively provided with a drain valve.
Optionally, liquid level pipes are respectively arranged on the anode tank body and the cathode tank body.
In a second aspect, the present application also provides a method of using a material tolerance test apparatus, suitable for use in a material tolerance test apparatus according to the first aspect, comprising: electrolyte is respectively injected into the anode tank body and the cathode tank body, wherein acid electrolyte is injected into the anode tank body and the cathode tank body; connecting the anode plate and the cathode plate with an electrolysis power supply, and introducing electrolysis current; stopping electrifying after the electrolysis process is completed, and placing the material to be tested in the electrolyte of the anode tank body and/or the cathode tank body, wherein the cathode tank body provides a reducing environment, and the anode tank body provides an oxidizing environment; and introducing a test current to perform a tolerance test on the material to be tested.
Optionally, the cathode tank body is filled with vanadium electrolyte, and the anode tank body is filled with 25-30wt% sulfuric acid solution.
Optionally, the electrolysis current has a current density of 100-300mA/cm 2 The electrolysis time t is calculated by the following formula:wherein: t is electrolysis time, and the unit is s; c is the concentration of vanadium electrolyte, and the unit mol/L; v is the volume of the injected vanadium electrolyte and is in unit L; ā is the average valence state of the initial vanadium ion of the vanadium electrolyte and is in unit mol/L; f is Faraday constant, and 96485.3C/mol is taken; i is electrolysis current, and the unit is A.
Optionally, the test current has a current density of 10-20mA/cm 2 。
Optionally, the method further comprises: and monitoring the electrolyte liquid level in the anode tank body and/or the cathode tank body in the test process of the sample to be tested, and supplementing pure water to maintain the electrolyte volume.
Compared with the prior art, the application has the following advantages: the device comprises a tank body, a diaphragm and a sample placing piece for placing a sample to be tested, wherein the tank body comprises an anode tank body and a cathode tank body, an anode plate is arranged in the anode tank body, and a cathode plate is arranged in the cathode tank body; the anode plate and the cathode plate are used for switching on a power supply to electrolyze electrolyte in the anode tank body and the cathode tank body; the diaphragm is arranged between the anode tank body and the cathode tank body; the sample placing piece is arranged in the anode tank body and/or the cathode tank body, so that the test requirements of materials, especially vanadium battery materials, on the acid resistance, the oxidation resistance and the reduction resistance of electrolyte can be met simultaneously.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this specification, illustrate embodiments of the application and together with the description serve to explain the principles of the application. In the accompanying drawings:
FIG. 1 is a schematic diagram of a material tolerance test apparatus according to an embodiment of the present application;
FIG. 2 is a schematic diagram of a cell network in accordance with one embodiment of the present application;
FIG. 3 is a schematic view of the structure of a sample cage according to an embodiment of the present application;
FIG. 4 is a flow chart of a method of using a material tolerance test apparatus according to an embodiment of the application.
The marks in the figure are respectively expressed as:
10-cell body, 101-anode cell body, 102-cathode cell body;
11-anode plate;
12-a cathode plate;
13-a membrane;
14-sample placing pieces, 141-groove net, 142-sample cage and 143-hanging lugs;
15-cover plate;
16-a respiratory valve;
17-a liquid inlet valve;
18-a drain valve;
19-level tube.
Detailed Description
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are used in the description of the embodiments will be briefly described below. It is apparent that the drawings in the following description are only some examples or embodiments of the present application, and it is apparent to those of ordinary skill in the art that the present application may be applied to other similar situations according to the drawings without inventive effort. Unless otherwise apparent from the context of the language or otherwise specified, like reference numerals in the figures refer to like structures or operations.
As used in the specification and in the claims, the terms "a," "an," "the," and/or "the" are not specific to a singular, but may include a plurality, unless the context clearly dictates otherwise. In general, the terms "comprises" and "comprising" merely indicate that the steps and elements are explicitly identified, and they do not constitute an exclusive list, as other steps or elements may be included in a method or apparatus.
The relative arrangement of the components and steps, numerical expressions and numerical values set forth in these embodiments do not limit the scope of the present application unless it is specifically stated otherwise. Meanwhile, it should be understood that the sizes of the respective parts shown in the drawings are not drawn in actual scale for convenience of description. Techniques, methods, and apparatus known to one of ordinary skill in the relevant art may not be discussed in detail, but should be considered part of the specification where appropriate. In all examples shown and discussed herein, any specific values should be construed as merely illustrative, and not a limitation. Thus, other examples of the exemplary embodiments may have different values. It should be noted that: like reference numerals and letters denote like items in the following figures, and thus once an item is defined in one figure, no further discussion thereof is necessary in subsequent figures.
In the description of the present application, it should be understood that the azimuth or positional relationships indicated by the azimuth terms such as "front, rear, upper, lower, left, right", "lateral, vertical, horizontal", and "top, bottom", etc., are generally based on the azimuth or positional relationships shown in the drawings, merely to facilitate description of the present application and simplify the description, and these azimuth terms do not indicate and imply that the apparatus or elements referred to must have a specific azimuth or be constructed and operated in a specific azimuth, and thus should not be construed as limiting the scope of protection of the present application; the orientation word "inner and outer" refers to inner and outer relative to the contour of the respective component itself.
Spatially relative terms, such as "above … …," "above … …," "upper surface at … …," "above," and the like, may be used herein for ease of description to describe one device or feature's spatial location relative to another device or feature as illustrated in the figures. It will be understood that the spatially relative terms are intended to encompass different orientations in use or operation in addition to the orientation depicted in the figures. For example, if the device in the figures is turned over, elements described as "above" or "over" other devices or structures would then be oriented "below" or "beneath" the other devices or structures. Thus, the exemplary term "above … …" may include both orientations of "above … …" and "below … …". The device may also be positioned in other different ways (rotated 90 degrees or at other orientations) and the spatially relative descriptors used herein interpreted accordingly.
A flowchart is used in the present application to describe the operations performed by a system according to embodiments of the present application. It should be understood that the preceding or following operations are not necessarily performed in order precisely. Rather, the various steps may be processed in reverse order or simultaneously. At the same time, other operations are added to or removed from these processes.
Example 1
Fig. 1 is a schematic structural diagram of a material tolerance testing apparatus according to an embodiment of the present application, and referring to fig. 1, the material tolerance testing apparatus according to the embodiment mainly includes: the cell body 10, the cell body 10 includes an anode cell body 101 and a cathode cell body 102, wherein the anode cell body 101 is internally provided with an anode plate 11, and the cathode cell body 102 is internally provided with a cathode plate 12. The anode plate 11 and the cathode plate 12 are used for being powered on to electrolyze the electrolyte in the anode tank body 101 and the cathode tank body 102; also included is a diaphragm 13, the diaphragm 13 being disposed between the anode cell 101 and the cathode cell 102, and a sample placement member 14 for placing a sample to be tested, the sample placement member 14 being disposed within the anode cell 101 and/or the cathode cell 102.
In this embodiment, as shown in fig. 1, an anode tank 101 may be provided at the left side, and an acidic electrolyte such as a vanadium electrolyte may be added thereto, and a cathode tank 102 may be provided at the right side, and another acidic electrolyte such as a sulfuric acid solution may be added thereto. Because anode plate 11 and negative plate 12 are used for switching on in order to electrolyze the electrolyte in positive pole cell body 101 and the negative pole cell body 102, consequently can provide the reductive environment in the negative pole cell body 102 after the electrolyte is electrolyzed, positive pole cell body 101 provides the oxidizing environment, and the electrolyte in positive pole cell body 102 and the positive pole cell body 101 is the acidic electrolyte by oneself, consequently, this embodiment testing arrangement can provide the test environment of acidity, reducibility and oxidizing simultaneously, make things convenient for the material that awaits measuring to carry out above-mentioned various tolerance test smoothly in same device, the comparatively single defect of test environment of current testing arrangement has been solved.
In one example, the illustrated apparatus may further include a cover plate 15, the cover plate 15 cooperating with the anode and/or cathode cell bodies 101, 102 for sealing the anode and/or cathode cell body 101, 102 openings. After the anode tank body 101 and/or the cathode tank body 102 are sealed, on one hand, the testing environment in the tank body 10 is isolated from other external environments, so that the testing result is more accurate; on the other hand, the cover plate 15 is arranged, so that the safety of testers can be ensured in the testing process.
Illustratively, the cover plate 15 in this embodiment may be a monolithic plate having an area substantially corresponding to the opening area of the cell body 10 (the total opening area of the anode cell body 101 and the cathode cell body 102), and capable of sealing the anode cell body 101 and the cathode cell body 102 at the same time; in addition, the cover plate 15 may be divided into two parts, one part is used for sealing the anode tank body 101 and the other part is used for sealing the cathode tank body 102, and the sealing of the two areas is independent and is not affected.
In one example, one side of the cover plate 15 is movably connected to one side of the anode and/or cathode cell bodies 101, 102, or the cover plate 15 is a separate structure from the anode and cathode cell bodies 101, 102.
For example, when one side of the cover 15 is movably connected to one side of the anode tank 101 and/or the cathode tank 102, referring to fig. 1, the connecting edge E1 of the cover 15 is movably connected to the tank 10, such as by a hinge, a shaft, or the like, which is not particularly limited herein, and the other side of the cover 15, i.e., the moving edge E2, can rotate about the connecting edge E1 of the cover 15, thereby realizing the sealing and opening functions of the opening of the tank 10.
When the cover plate 15 is in a structure separated from the anode tank body 101 and the cathode tank body 102, that is, the cover plate 15 and the tank body 10 are structurally independent, there is no physical connection relationship between them, and the cover plate 15 is used as an independent accessory of the testing device, and when the cover plate 15 is required in the use process of the device, the cover plate 15 is placed on the opening of the tank body 10 in a proper mode. Compared with the movable connection mode, the independent structure has the advantages that whether the cover plate 15 is needed or not can be determined according to the situation, and when the cover plate 15 is not needed, the testing device is simpler; the cover 15 in the form of an articulated connection is already one of the components connected to the test device, whether or not it is used. The disadvantage of the independent construction is that the sealing effect of the independent cover plate 15 is not as good as the former.
In an example, the testing device may also be provided with a breather valve 16, the breather valve 16 being provided on the cover plate 15. When the testing device is provided with the cover plate 15, the groove body 10 forms a sealed structure, and the testing device can generate some gases in the testing process, which is unfavorable for the discharge of the gases, so that a corresponding breather valve 16 is required to be arranged. For example, the breather valve 16 may be provided on the cover plate 15 on the cathode tank 102 side, the breather valve 16 may be provided on the cover plate 15 on the anode tank 101 side, or the breather valve 16 may be provided on both the cover plates 15 on the cathode tank 102 side and the anode tank 101 side. It will be appreciated that the breather valve 16 may be used in the present embodiment for gas venting during the endurance test, or other devices with similar gas venting functions may be used, which are not shown here.
In an example, the present test device may further be provided with a liquid inlet valve 17, and the liquid inlet valve 17 is disposed on the cover plate 15. In the case of the cover plate 15, the cover plate 15 is generally used to cover the tank 10, and then the electrolyte is added to reduce the splashing of the electrolyte or the influence of the external environment. When the present test device has a cover plate 15, the tank body 10 forms a sealed structure, and it is necessary to provide a suitable liquid inlet for adding electrolyte, so that it is necessary to provide a corresponding liquid inlet valve 17, and electrolyte is added into the tank body 10 through the liquid inlet valve 17. For example, the liquid inlet valve 17 may be disposed on the cover plate 15 on the cathode tank 102 side, the liquid inlet valve 17 may be disposed on the cover plate 15 on the anode tank 101 side, or the liquid inlet valve 17 may be disposed on both the cover plates 15 on the cathode tank 102 side and the anode tank 101 side. It will be appreciated that in this embodiment, the electrolyte is added to the tank 10 by using the inlet valve 17, and other devices having the same or similar functions may be used, which are not shown here.
In one example, the membrane 13 is a perfluorosulfonic acid proton membrane. The perfluorosulfonic acid proton membrane has excellent heat resistance, mechanical property, electrochemical property and chemical stability, can be used under harsh conditions such as strong acid, strong alkali, strong oxidant medium and the like, is not only used as a key component of a proton exchange membrane fuel cell, but also widely applied to the fields such as vanadium cells, water electrolysis hydrogen production, electrochemical synthesis, gas separation, electrochemical sensors and the like, and is used as a solid electrolyte membrane in various electrochemical cells relying on cation selective conduction. In this embodiment, the membrane 13 separates the cell body 10 into a cathode cell body 102 and an anode cell body 101, and a perfluorosulfonic acid proton membrane is used, so that the testing device can be applied to more severe testing conditions such as strong acid, strong oxidation and the like.
In one example, the sample placement member 14 comprises a cell network 141 and at least one sample cage 142, wherein the cell network 141 is disposed within the anode cell body 101 and/or the cathode cell body 102, and the sample cage 142 is coupled to the cell network 141.
In this embodiment, the sample placing member 14 is a place where the sample to be tested is placed, so that the testing device can flexibly test one or more samples to be tested, as shown in fig. 2, the device may adopt a combination mode of a tank net 141 and a sample cage 142, where the tank net 141 is tightly attached to the anode plate 11 or the cathode plate 12 for conducting electricity, and one or more sample cages 142 are provided in the tank net 141 for placing the tolerance test samples, so that the number of the sample cages 142 is determined according to the number of the samples to be tested. Further, the material of the tank net 141 may be titanium, preferably iridium-plated tantalum, and the material of the sample cage 142 may be identical to that of the tank net 141. The titanium material sample cage 142 is in conductive communication with the anode plate 11, so that a strong oxidizing environment for continuous oxygen evolution can be maintained in the sample cage 142.
In this embodiment, the mesh 141 is generally equal in size to the inside of the anode cell 101 or the cathode cell 102, and is also identical in shape to the inside of the anode cell 101 or the cathode cell 102. If the inside of the anode cell 101 or the cathode cell 102 is in the shape of a square column, the shape of the cell 141 is also a square column, and if the inside of the anode cell 101 or the cathode cell 102 is in the shape of a cylinder, the shape of the cell 141 is also a cylinder.
In an example, the sample cage 142 has a hanging lug 143, the hanging lug 143 is hung on the groove net 141, and the sample cage 142 is hung on the groove net 141 through the hanging lug 143, so that the method is simple and flexible. As shown in fig. 3, a hanger 143 may be provided at one place of the sample cage 143, or a plurality of hangers 143 may be provided at a plurality of places of the sample cage 143. The design of the movable suspension loop type sample cage 143 can meet the requirement of simultaneously testing a plurality of samples to be tested.
In one example, the anode cell 101 and the cathode cell 102 may be provided with a drain valve 18, respectively, for draining the solution. Of course, other similar devices capable of achieving the tapping function may be used in this embodiment, which is not shown here.
In one example, the anode tank 101 and the cathode tank 102 are each provided with a liquid level pipe 19. In the testing process, the volume of the solution in the tank body 10 will change, and the liquid level tubes 19 are respectively disposed in the anode tank body 101 and the cathode tank body 102, so that the volume change of the solution in the tank body can be observed, that is, the liquid level in the tank body 10 is effectively monitored, and the volume change of the solution is known through the liquid level change of the solution. For example, when the solution volume of the tank 10 is observed to decrease through the level pipe 19, pure water may be timely replenished to maintain the solution volume.
In this embodiment, the cover 15, the tank body 10, the tank net 141, the pipe valve, and the like may be made of a corrosion-resistant polymer material such as PP, PVDF, PTFE.
According to the material tolerance testing device provided by the embodiment, a tank body, a diaphragm and a sample placing piece for placing a sample to be tested are arranged, wherein the tank body comprises an anode tank body and a cathode tank body, an anode plate is arranged in the anode tank body, and a cathode plate is arranged in the cathode tank body; the anode plate and the cathode plate are used for switching on a power supply to electrolyze electrolyte in the anode tank body and the cathode tank body; the diaphragm is arranged between the anode tank body and the cathode tank body; the sample placing piece is arranged in the anode tank body and/or the cathode tank body, so that the test requirements of materials, especially vanadium battery materials, on the acid resistance, the oxidation resistance and the reduction resistance of electrolyte can be met simultaneously.
Example two
Fig. 4 is a flow chart illustrating a method of using a material tolerance test apparatus according to an embodiment of the present application, and referring to fig. 4, a method 400 can be applied to the material tolerance test apparatus according to the first embodiment, which includes:
410. electrolyte is respectively injected into the anode tank body and the cathode tank body, wherein acid electrolyte is injected into the anode tank body and the cathode tank body.
For example, using the test apparatus described above, the cover plate 15 is closed, and then the electrolyte is injected into the cathode tank 102 and the anode tank 101 through the liquid inlet valve 17.
In one example, a vanadium electrolyte is injected into the cathode cell body 102, and 25-30wt% sulfuric acid solution is injected into the anode cell body 101 for testing the durability of the vanadium cell material.
420. And connecting the anode plate and the cathode plate with an electrolysis power supply, and introducing electrolysis current.
In one example, the electrolysis current may have a current density of 100-300mA/cm 2 The electrolysis time t is calculated by the following formula:
wherein: t is electrolysis time, and the unit is s; c is the concentration of vanadium electrolyte, and the unit mol/L; v is the volume of the injected vanadium electrolyte and is in unit L; ā is the average valence state of the initial vanadium ion of the vanadium electrolyte and is in unit mol/L; f is Faraday constant, and 96485.3C/mol is taken; i is electrolysis current, and the unit is A. .
430. And stopping electrifying after the electrolysis process is finished, and placing a material to be tested (a sample to be tested) into the electrolyte of the anode tank body and/or the cathode tank body, wherein a reducing environment is provided in the cathode tank body, and an oxidizing environment is provided in the anode tank body.
For example, the material to be tested is cut or sliced into samples of suitable size, placed in the sample cages 142 of the cathode cell body 102 and the anode cell body 101, respectively, and the sample cages 142 are fixed to the cell nets 141 of the cathode cell body 102 and the anode cell body 101 by the lugs 143, so that the sample to be tested is completely immersed in the solution, the cover plate 15 is closed, and the material tolerance test is started.
440. And introducing a test current to perform a tolerance test on the material to be tested.
In one example, the test current has a current density of 10-20mA/cm 2 Electrolysis was continued until the material resistance test ended. Illustratively, the cathode is maintained continuously near +2-valent by microcurrent electrolysis, maintaining high reducibility.
Further, during testing of the sample to be tested, the electrolyte level in the anode cell 101 and/or in the cathode cell 102 may also be monitored in order to supplement pure water to maintain the electrolyte volume.
For example, the liquid level in the tank 10 is monitored by the liquid level pipe 19 using the testing device as described above, and the pure water is supplied to the liquid inlet valve 17 to maintain the solution volume.
In the embodiment, the cathode adopts a vanadium electrolyte solution, the anode adopts a sulfuric acid solution, the average valence state of vanadium ions of the vanadium electrolyte in the cathode tank 102 reaches about +2 in a short time through preliminary high-current electrolysis, a reducing environment is provided for the material tolerance test, and the solution system maintains the reducibility through continuous microcurrent electrolysis; the sample cage 142 in the anode tank body 101 is hung on the tank net 141 and is in contact with the anode plate 11 to conduct electricity, so that the sample cage 142 becomes a reaction place of anode electrolyzed water, and the surface is enriched with oxygen free radicals with strong oxidability, thereby providing an oxidability environment for material tolerance test; meanwhile, the vanadium electrolyte and the anodic acid solution are both acidic solutions, and an acidic environment is provided for material tolerance test. Therefore, the application method provided by the embodiment can simultaneously meet the test requirements of the materials, especially the vanadium battery materials, on the acid resistance, the oxidation resistance and the reduction resistance of the electrolyte.
While the basic concepts have been described above, it will be apparent to those skilled in the art that the foregoing disclosure is by way of example only and is not intended to be limiting. Although not explicitly described herein, various modifications, improvements and adaptations of the application may occur to one skilled in the art. Such modifications, improvements, and modifications are intended to be suggested within the present disclosure, and therefore, such modifications, improvements, and adaptations are intended to be within the spirit and scope of the exemplary embodiments of the present disclosure.
Meanwhile, the present application uses specific words to describe embodiments of the present application. Reference to "one embodiment," "an embodiment," and/or "some embodiments" means that a particular feature, structure, or characteristic is associated with at least one embodiment of the application. Thus, it should be emphasized and should be appreciated that two or more references to "an embodiment" or "one embodiment" or "an alternative embodiment" in various positions in this specification are not necessarily referring to the same embodiment. Furthermore, certain features, structures, or characteristics of one or more embodiments of the application may be combined as suitable.
Similarly, it should be noted that in order to simplify the description of the present disclosure and thereby aid in understanding one or more inventive embodiments, various features are sometimes grouped together in a single embodiment, figure, or description thereof. This method of disclosure, however, is not intended to imply that more features than are required by the subject application. Indeed, less than all of the features of a single embodiment disclosed above.
In some embodiments, numbers describing the components, number of attributes are used, it being understood that such numbers being used in the description of embodiments are modified in some examples by the modifier "about," approximately, "or" substantially. Unless otherwise indicated, "about," "approximately," or "substantially" indicate that the number allows for a 20% variation. Accordingly, in some embodiments, numerical parameters set forth in the specification and claims are approximations that may vary depending upon the desired properties sought to be obtained by the individual embodiments. In some embodiments, the numerical parameters should take into account the specified significant digits and employ a method for preserving the general number of digits. Although the numerical ranges and parameters set forth herein are approximations in some embodiments for use in determining the breadth of the range, in particular embodiments, the numerical values set forth herein are as precisely as possible.
While the application has been described with reference to the specific embodiments presently, it will be appreciated by those skilled in the art that the foregoing embodiments are merely illustrative of the application, and various equivalent changes and substitutions may be made without departing from the spirit of the application, and therefore, all changes and modifications to the embodiments are intended to be within the scope of the appended claims.
Claims (15)
1. A material resistance testing apparatus, comprising:
the cell body comprises an anode cell body and a cathode cell body; wherein an anode plate is arranged in the anode tank body, and a cathode plate is arranged in the cathode tank body;
the anode plate and the cathode plate are used for being powered on to electrolyze electrolyte in the anode tank body and the cathode tank body;
a separator disposed between the anode cell body and the cathode cell body;
the sample placing piece is used for placing a sample to be tested and is arranged in the anode tank body and/or the cathode tank body.
2. The material tolerance test device according to claim 1, further comprising a cover plate cooperating with the anode cell body and/or the cathode cell body for sealing the anode cell body and/or the cathode cell body opening.
3. The material tolerance test device according to claim 2, wherein one side of the cover plate is movably connected to one side of the anode tank body and/or the cathode tank body, or the cover plate is a separate structure from the anode tank body and the cathode tank body.
4. The material resistance testing device according to claim 2, further provided with a breather valve provided on the cover plate.
5. The material tolerance testing device of claim 2, further comprising a liquid inlet valve disposed on the cover plate.
6. The material tolerance test device according to claim 1, wherein the membrane is a perfluorosulfonic acid proton membrane.
7. The material tolerance test device according to claim 1, wherein the sample placement member comprises a mesh of cells and at least one sample cage, wherein the mesh of cells is disposed inside the anode cell body and/or the cathode cell body, the mesh of cells being connected to the sample cage.
8. The material tolerance testing device of claim 7, wherein the sample cage has a hanger that is hung from the cell wire.
9. The material tolerance test device according to claim 1, wherein a drain valve is provided on each of the anode tank body and the cathode tank body.
10. The material tolerance test device according to claim 1, wherein liquid level pipes are provided on the anode tank body and the cathode tank body, respectively.
11. A method of using a material resistance testing device according to any one of claims 1 to 10, comprising:
electrolyte is respectively injected into the anode tank body and the cathode tank body, wherein acid electrolyte is injected into the anode tank body and the cathode tank body;
connecting the anode plate and the cathode plate with an electrolysis power supply, and introducing electrolysis current;
stopping electrifying after the electrolysis process is completed, and placing the material to be tested in the electrolyte of the anode tank body and/or the cathode tank body, wherein the cathode tank body provides a reducing environment, and the anode tank body provides an oxidizing environment;
and introducing a test current to perform a tolerance test on the material to be tested.
12. The method of claim 11, wherein the cathode cell is filled with vanadium electrolyte and the anode cell is filled with 25-30wt% sulfuric acid solution.
13. The method of claim 11, wherein the electrolysis current has a current density of 100-300mA/cm 2 The electrolysis time t is calculated by the following formula:
wherein: t is electrolysis time, and the unit is s; c is the concentration of vanadium electrolyte, and the unit mol/L; v is the volume of the injected vanadium electrolyte and is in unit L;the average valence state of vanadium ions is the initial average valence state of vanadium ions of the vanadium electrolyte, and the unit mol/L is the initial average valence state of vanadium ions; f is Faraday constant, and 96485.3C/mol is taken; i is electrolysis current, and the unit is A.
14. The method of claim 11, wherein the test current has a current density of 10-20mA/cm 2 。
15. The method of use of claim 11, further comprising: and monitoring the electrolyte liquid level in the anode tank body and/or the cathode tank body in the test process of the sample to be tested, and supplementing pure water to maintain the electrolyte volume.
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