• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    Measuring device, or electrochemical cell, for obtaining electrochemical measurements on a sample (1) comprising at least one body (2) with a housing (22) to house said sample (1), wherein said housing (22) comprises an opening (23) to a watertight cavity (3) configured to house a working solution (32), characterized in that said cavity (3) comprises at least one opening (23) sealed in a sealed manner with a movable element (4) It can be used at an angle other than 0º on the horizontal, thus allowing the measurement of electrochemical or other processes, without the loss of liquid due to the inclination suffered by the electrochemical cell. In addition, it would allow the study of any material, including those that produce gases in their electrochemical reactions, without the risk of registering interferences in the acquisition of measurements. (Machine-translation by Google Translate, not legally binding)
    公开号:ES2802295A1
    申请号:ES201900103
    申请日:2019-07-09
    公开日:2021-01-18
    发明作者:Suarez Ricardo Manuel Souto；Gonzalez Vicente Fernando Mena；La Nuez Pestana Ignacio Agustin De；Rodriguez Juan Jose Santana
    申请人:Universidad de La Laguna；Universidad de las Palmas de Gran Canaria；
    IPC主号:
    专利说明:

    [0002] MEASURING DEVICE FOR OBTAINING ELECTROCHEMICAL MEASUREMENTS
    [0004] OBJECT OF THE INVENTION
    [0006] The object of the present patent application is a measurement device for obtaining electrochemical measurements on a sample, according to claim 1, incorporating notable innovations and advantages over the technical solutions used up to now.
    [0008] BACKGROUND OF THE INVENTION
    [0010] The field of application of the present invention is framed within the technical sector of devices for electrochemical measurements of a sample.
    [0012] It has been detected that the Industry currently requires more and more knowledge of the processes involved in the interaction of an electrolyte with various material surfaces, both on a micrometric scale and on a nanometric scale. Measurements are usually carried out in an electrochemical cell, in the presence of a quantity of liquid called electrolyte, which presents the difficulty of containing this liquid when it comes to measurements with inclination above the horizontal.
    [0014] At an introductory level, it should be noted that an electrochemical cell is a device capable of either generating electrical energy through the energy of chemical reactions or facilitating chemical reactions through the introduction of electrical energy. A common example of an electrochemical cell is a standard 1.5 volt cell (AA battery) made for consumer use. This type of device is known as a single galvanic cell. A battery consists of two or more cells, connected, either in parallel or in a series pattern.
    [0015] Various measuring devices are known in the current state of the art for obtaining electrochemical measurements on a sample.
    [0017] Specifically, it is known from the state of the art, according to what is disclosed in document JP2006220597, a scanning probe microscope, sample surface roughness meter, electrochemical microscope for measuring surface information of various samples, such as hard disk and semiconductor wafers . The surface information measurement device, the scanning probe microscope, has a micromotion and angle adjustment mechanism that adjusts the angle between the sample movement stage and the sample surface.
    [0019] It is also known from the state of the art, according to what is disclosed in document CN102183678, a multifunctional electrolytic tank for a scanning electrochemical microscope, comprising an upper cover, a lower cover and a double-layer cylinder, in which the upper cover and the lower one are concave The inner side of the upper cover and the inner side of the lower cover are respectively provided with an internal thread, two ends of the double-layer cylinder are respectively provided with an external thread The multi-functional electrolytic tank can complete the experiments of a three-electrode system, a four-electrode system and a complex electrode system through different structures of the lower cover.
    [0021] In view of this and other background already known in the state of the art, it is seen that there is still a need to find a design of an electrochemical cell for use at an angle other than 0o on the horizontal. This design would allow the measurement of electrochemical or other processes, without the loss of liquid due to the inclination suffered by the measurement cell. In addition, it would allow the study of any material, even those that produce gases in their electrochemical reactions, without the risk of registering interferences in the acquisition of measurements.
    [0023] DESCRIPTION OF THE INVENTION
    [0025] The present invention consists of an electrochemical work cell to carry out measurements of an electrochemical or other nature of materials subjected to the action of an electrolyte exposed with different inclinations with respect to the horizontal. Thus, the invention allows to observe, measure and analyze samples that are not necessarily in the horizontal position, but inclined with various slopes or angles, even variables in space, that is, curves, not flat, macroscopically speaking.
    [0027] Thus, and more specifically, the measuring device for obtaining electrochemical measurements on a sample comprises at least one body with a housing to house said sample, wherein said housing comprises an opening to a watertight cavity configured to house a working solution, and said cavity comprises at least one opening sealed in a sealed manner with a movable element. Thus, the measurement of electrochemical or other processes is possible, without the loss of liquid due to the inclination suffered by the measurement cell. The danger of recording interferences in the acquisition of measurements in the study of any material, even those that produce gases in their electrochemical reactions, is further minimized.
    [0029] Advantageously, the movable element of the measuring device is a flexible membrane. Said flexible membrane preferably has a tight anchoring system of the working electrode that allows it to be deformed, in such a way that the working electrode can move without resistance over the entire surface of the sample exposed to the electrolyte and / or working solution.
    [0031] According to another aspect of the invention, the body with the housing comprises a cover that closes said housing, with a first sealing element between the body and the cover, so that said connection of the cell cover to the body thereof results watertight.
    [0033] It is worth mentioning that the cover is fixed to the body by means of at least one first fastening element, said joint presenting sufficient robustness, preventing uncontrolled openings of the cell from occurring.
    [0035] On the other hand, the measuring device comprises a second sealing element between the sample and the opening to a cavity also presenting the corresponding and necessary sealing.
    [0037] Specify that the second sealing element is located on the opposite side of the body cover, so that the force exerted on the closure of the measuring device increases the sealing performance of this second element.
    [0038] Further note that the sample is secured in the housing by a second clamping element that presses the sample against the second sealing element. In this way, a watertight installation of the sample is achieved.
    [0040] In a preferred embodiment of the invention, the measuring device comprises a first electrode in connection with the sample, in order to be able to take the corresponding electrochemical measurements.
    [0042] Advantageously, the measuring device comprises a second electrode in connection with the working solution, said second electrode being positioned in the opening of the housing to the cavity. In this way and through this second electrode, also called counter electrode, it is possible to set the working potential. Additionally, the measuring device may comprise a third reference electrode for the values to be measured.
    [0044] According to another preferred embodiment of the invention, the measuring device comprises an expansion tank for the working solution, so that it is possible to absorb variations in volume and inertia as a result of the movement of the working solution.
    [0046] Additionally, the measuring device comprises a fourth electrode for taking measurements, offering greater versatility in the measurement task. Said fourth electrode can also be called a working electrode or an ultramicroelectrode.
    [0048] According to another aspect of the invention, said fourth electrode is coupled to the movable element by means of a joint adaptable to the perimeter of said fourth electrode. This results in a tight anchoring system of the working electrode in its central part, and that allows a certain degree of deformation. Note that the movable element is fixed to the cavity on the opposite side to the lid, by means of a third sealing element. Preferably the third sealing element is a screw and an O-ring which guarantees the tightness of the system. And in addition to sealing, the coupling by means of a joint adaptable to the diameter of the electrode allows it to move in the x and z directions due to the flexibility of the flexible membrane, the cavity remaining airtight at all times.
    [0049] According to a preferred embodiment of the invention, the fourth electrode is oriented in space by at least one orientation motor, which allows the orientation of said fourth electrode in at least one of the three coordinate directions of the x-y-z space. In a preferred embodiment, the fourth electrode is oriented in space by an orientation motor for each axis, which allows the orientation of said fourth electrode in the three coordinate directions of space, defined as (Nx, Ny, Nz).
    [0051] More in particular, the measuring device comprises a motor for rotating the measuring device itself with respect to the vertical, so that the measurement of electrochemical or other processes is made possible, without loss of liquid due to the inclination suffered by the measurement cell.
    [0053] According to another aspect of the invention, the cavity of the measuring device comprises an orifice in its upper part, in order to establish a pressure balance. Said hole represents an opening in the cell that allows working at atmospheric pressure, as well as the evacuation of possible gases produced during the measurement. This would allow the study of any material, even those that produce gases in their electrochemical reactions, without the danger of registering interferences in the acquisition of measurements. Preferably, the orifice must be close to the movable element. Specifically, it must be located in the upper part of the cell, as close as possible to the flexible membrane.
    [0055] The attached drawings show, by way of non-limiting example, a measuring device for obtaining electrochemical measurements on a sample, constituted according to the invention. Other characteristics and advantages of said measuring device for obtaining electrochemical measurements in A sample, object of the present invention, will be evident from the description of a preferred, but not exclusive, embodiment, which is illustrated by way of non-limiting example in the accompanying drawings, in which:
    [0057] BRIEF DESCRIPTION OF THE DRAWINGS
    [0058] Figure 1.- Is a sectional view of the measuring device for obtaining electrochemical measurements on a sample, according to the present invention.
    [0060] DESCRIPTION OF A PREFERRED EMBODIMENT
    [0062] In view of the aforementioned figure and, according to the numbering adopted, it can be seen in them an example of a preferred embodiment of the measuring device, or electrochemical cell, for obtaining electrochemical measurements on a sample, which comprises of the following following items:
    [0063] - a body 2 of the electrochemical cell, with a cover 21 that is screwed to the body 2 by means of clamping screws, called first clamping element 26;
    [0064] - an O-ring, called the first sealing element 24, which serves as a seal for the attachment of the cover 21 of the cell to the body 2 thereof;
    [0065] - sample 1 tested. The sample 1 is fixed to the cell by using a screw, called the second clamping element 27, which presses it against an O-ring, or second sealing element 25, located on the face opposite the cover 21 of the cell. Sample 1 is placed in housing 22, which comprises opening 23 on the side opposite to cover 21;
    [0066] - an electrical connection of the device for measuring or measuring the sample 1 by means of a first electrode 51;
    [0067] - a second electrode 52, or counter electrode for connection to the measurement or measurement device, said second electrode 52 preferably being an electrode of noble metal or inert conductive material (stainless steel, gold, platinum, carbon, etc ...) surrounding the measurement area;
    [0068] - a reservoir or cavity 3 where the electrolyte or working solution 32 is located;
    [0069] - an expansion tank 6 for the electrolyte or working solution;
    [0070] - a reference electrode or third electrode 53 with connection to the measuring device; - a fourth electrode 54, or working electrode or ultramicroelectrode or measuring probe, connected to a flexible membrane or movable element 4 in a hermetic way by means of a joint 54a adaptable to the diameter of the fourth electrode 54 that allows it to move in the XYZ directions, keeping the sealing properties;
    [0071] - a movable element 4 or flexible membrane, which allows it to be deformed, in such a way that the working electrode or fourth electrode 54 can move without resistance over the entire surface of the sample 1 exposed to the electrolyte or working solution 32. Said element movable 4 is anchored in the area opposite the cover 2 by means of fastening or anchoring screws, thus generating the watertight area. Between the work area and the anchoring system, there is an O-ring that guarantees the tightness of the system; - at least one orientation motor 7 that moves the working electrode, or fourth electrode 54, in the three coordinate directions (Nx, Ny, Nz).
    [0072] - a turning system of the electrochemical cell or measuring device in the Y axis. It is understood that the Y axis is the one that comes out perpendicularly from the plane of the section of figure 1.
    [0073] - at least one opening, or hole 31, in the electrochemical cell or measuring device located in the upper part of the cell, as close as possible to the flexible membrane or movable element 4;
    [0075] Thus, and more specifically, as seen in figure 1, the measuring device for obtaining electrochemical measurements on a sample 1 comprises at least one body 2 with a housing 22 to house said sample 1, wherein said housing 22 comprises an opening 23 to a watertight cavity 3 configured to house a working solution 32, and said cavity 3 comprises at least one opening 23 sealed in a sealed manner with a movable element 4. Said movable element 4 is anchored in the area opposite to cover 2 by means of fastening or anchoring screws, thus generating the watertight area. Between the work area and the anchoring system there is an O-ring that guarantees the tightness of the system. Specify that the working solution 32 can be an electrolyte or an ionic liquid.
    [0077] Preferably, as can be seen in FIG. 1, the movable element 4 is a flexible membrane.
    [0079] According to another aspect of the invention, as seen in figure 1, the body 2 with the housing 22 comprises a cover 21 that closes said housing 22, with a first sealing element 24 between the body 2 and the cover 21.
    [0081] More specifically, as seen in figure 1, the cover 21 is fixed to the body 2 by means of at least one first fastening element 26, which can be a fastening screw, or a fastening clip.
    [0082] According to a particular embodiment of the invention, as seen in Figure 1, the measuring device comprises a second sealing element 25 between the sample 1 and the opening 23 to a cavity 3. Specify that, according to a preferred embodiment of In the invention, the first sealing element 24 and / or the second sealing element 25 are at least one O-ring.
    [0084] More specifically, as seen in figure 1, the second sealing element 25 is located on the opposite side of the cover 21 from the body 2.
    [0086] On the other hand, as seen in figure 1, the sample 1 is fixed in the housing 22 by means of a second clamping element 27 that presses the sample 1 against the second sealing element 25. Specify that the second clamping element Fastener 27 may be a threaded screw through cap 21.
    [0088] According to another aspect of the invention, as can be seen in figure 1, the measuring device comprises a first electrode 51 in connection with sample 1. Said connection can be made through the part of the rear cover, through a cable electrical welded to the specimen and a hole in the back cover.
    [0090] It should be mentioned that, as can be seen in Figure 1, the measuring device comprises a second electrode 52 in connection with the working solution 32, said second electrode 52 being positioned in the opening 23 of the housing 22 to the cavity 3. Point out that the opening 23 to the cavity 3 is the measurement zone, and that the second electrode 52, or counter electrode, is an electrode of noble metal or inert conductive material (stainless steel, gold, platinum, carbon, etc ...)
    [0092] Additionally, as can be seen in figure 1, the measuring device comprises an expansion tank 6 for the working solution 32.
    [0094] More particularly, as seen in figure 1, the measuring device comprises a fourth electrode 54 for taking measurements.
    [0096] It should be mentioned that, as seen in figure 1, the fourth electrode 54 is coupled to the movable element 4 by means of an adaptable joint 54a to the perimeter of said fourth electrode 54.
    [0097] According to a preferred embodiment of the invention, as seen in figure 1, the fourth electrode 54 is oriented in space by at least one orientation motor 7.
    [0099] According to a particular embodiment of the invention, as seen in figure 1, the measuring device comprises a rotation motor 8 of the measuring device itself with respect to the vertical.
    [0101] Additionally, as seen in figure 1, cavity 3 comprises a hole 31 in its upper part.
    [0103] The details, shapes, dimensions and other accessory elements, as well as the components used in the measuring device to obtain electrochemical measurements on a sample, may be conveniently replaced by others that are technically equivalent, and do not depart from the essentiality of the invention or of the scope defined by the claims that follow the following list.
    [0105] Numeric references list:
    [0107] 1 sample
    [0108] 2 body
    [0109] 21 cap
    [0110] 22 accommodation
    [0111] 23 aperture
    [0112] 24 first sealing element
    [0113] 25 second sealing element
    [0114] 26 first clamping element
    [0115] 27 second clamping element
    [0116] 3 cavity
    [0117] 31 hole
    [0118] 32 dissolution of work
    [0119] 4 movable element
    [0120] 51 first electrode
    [0121] 52 second electrode
    [0122] third electrode fourth electrode
    [0123] to adaptable joint expansion tank orientation motor rotation motor
    权利要求:
    Claims (1)
    [0001]
    1- Measuring device for obtaining electrochemical measurements in a sample (1) that comprises at least one body (2) with a housing (22) to house said sample (1), wherein said housing (22) comprises an opening (23) to a sealed cavity (3) configured to house a working solution (32), characterized in that said cavity (3) comprises at least one opening (23) sealed in a sealed manner with a movable element (4).
    2- Measuring device according to claim 1, characterized in that the movable element (4) is a flexible membrane.
    3- Measuring device according to any of the preceding claims, characterized in that the body (2) with the housing (22) comprises a cover (21) that closes said housing (22), with a first sealing element (24) between the body (2) and cover (21).
    4- Measuring device according to claim 3, characterized in that the cover (21) is fixed to the body (2) by at least one first clamping element (26).
    5- Measuring device according to claim 3, characterized in that it comprises a second sealing element (25) between the sample (1) and the opening (23) to a cavity (3).
    6.Measuring device according to claim 3, characterized in that the second sealing element (25) is located on the opposite side of the cover (21) from the body (2).
    7- Measuring device according to one of claims 5 or 6, characterized in that the sample (1) is fixed in the housing (22) by means of a second clamping element (27) that presses the sample (1) against the second element sealing (25).
    8. Measuring device according to any of the preceding claims, characterized in that it comprises a first electrode (51) in connection with the sample (1).
    9.Measuring device according to any of the preceding claims, characterized in that it comprises a second electrode (52) in connection with the working solution (32), said second electrode (52) being positioned in the opening (23) of the housing (22) to the cavity (3).
    10. Measuring device according to any of the preceding claims, characterized in that it comprises an expansion tank (6) for the working solution (32).
    11. Measuring device according to any of the preceding claims, characterized in that it comprises a fourth electrode (54) for taking measurements.
    12. Measuring device according to claim 3, characterized in that the fourth electrode (54) is coupled to the movable element (4) by means of an adaptable joint (54a) to the perimeter of said fourth electrode (54).
    13. Measuring device according to any of claims 11 or 12, characterized in that the fourth electrode (54) is oriented in space by at least one orientation motor (7).
    14. Measuring device according to any of the preceding claims, characterized in that it comprises a rotation motor (8) of the measuring device itself with respect to the vertical.
    15. Measuring device according to any of the preceding claims, characterized in that the cavity (3) comprises a hole (31) in its upper part.
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    同族专利:
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    引用文献:
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