Sample holder for in-situ x-ray diffractometer

Abstract

A sample holder for an in-situ X-ray diffractometer, according to one embodiment, comprises: a mount connected to a main body of the in-situ X-ray diffractometer; a connector which is supported by the mount and which receives a current from the outside; and a cell accommodated in the connector and irradiated with X-rays, wherein the cell can include: a case; a cap coupled to the case; an energy storage element disposed between the case and the cap; a case hole penetrating the case; and a polyimide film which covers the case hole and through which the X-rays can pass.

Description

Sample holder for in situ X-ray diffraction apparatus

[0001] The present invention relates to a sample holder for an in-situ X-Ray Diffractometer.

[0002] An in-situ X-ray diffraction device is a device that can obtain information on real-time structural changes in a sample, such as component analysis of organic and inorganic substances, crystal structure analysis, and crystal size, using X-ray diffraction. X-ray diffraction is a technique that determines the crystal structure of a material by irradiating X-rays on the angles and spacing of the crystal lattice of a sample and measuring the peaks diffracted at specific angles.

[0003] There is a need for a sample holder that can be compatible with a conventional in-situ X-ray diffraction device and obtain clear X-ray diffraction peaks of a sample by reducing the influence of X-ray peak intensity from a window.

[0004] In one embodiment, a sample holder for an in-situ X-ray diffractometer comprises: a mount connected to a main body of the in-situ X-ray diffractometer; a connector supported by the mount and supplied with current from the outside; and a cell accommodated in the connector and irradiated with X-rays, wherein the cell may include a case, a cap coupled to the case, an energy storage element disposed between the case and the cap, a case hole formed through the case, and a polyimide film covering the case hole and allowing the X-rays to pass therethrough.

[0005] In one embodiment, the mount may include a support plate supported by the body of the in-situ X-ray diffraction device, a base extending from the support plate, a connector receiving groove formed in the base and receiving the connector, and a first mount hole and a second mount hole formed through the base.

[0006] In one embodiment, the connector may include a connector body supported by the base, a cell receiving groove formed in the connector body and configured to receive the cell, a first terminal connected to the connector body and passing through the first mount hole, and a second terminal connected to the connector body and passing through the second mount hole and having a different polarity from the first terminal.

[0007] In one embodiment, the cell can contact the first terminal and the second terminal while being accommodated within the connector body.

[0008] In one embodiment, when diffraction occurs in the X-rays irradiated to the cell, twice the angle between the X-rays irradiated to the cell and the surface of the cell through which the X-rays are transmitted may be between 4° and 4.1°.

[0009] In one embodiment, when diffraction occurs in the X-rays irradiated to the cell, twice the angle between the X-rays irradiated to the cell and the surface of the cell through which the X-rays are transmitted may be between 5.8° and 6°.

[0010] In one embodiment, when diffraction occurs in the X-rays irradiated to the cell, twice the angle between the X-rays irradiated to the cell and the surface of the cell through which the X-rays are transmitted may be between 14.1° and 14.3°.

[0011] In one embodiment, when diffraction occurs in the X-rays irradiated to the cell, twice the angle between the X-rays irradiated to the cell and the surface of the cell through which the X-rays are transmitted may be between 29.4° and 29.6°.

[0012] In one embodiment, the energy storage element may include an anode, a cathode disposed opposite the cap with respect to the anode, a separator disposed between the anode and the cathode, and an electrolyte contained between the case and the cap.

[0013] In one embodiment, the energy storage element may include a cathode, an anode disposed opposite the cap with respect to the cathode, a separator disposed between the cathode and the anode, and an electrolyte contained between the case and the cap.

[0014] FIG. 1 is a perspective view illustrating an X-ray diffraction apparatus with a sample holder connected according to one embodiment.

[0015] FIG. 2 is a perspective view illustrating an X-ray diffraction apparatus with a sample holder connected according to one embodiment.

[0016] FIG. 3 is a perspective view illustrating a mount according to one embodiment.

[0017] Figure 4 is a perspective view illustrating a connector according to one embodiment.

[0018] Figure 5 is a perspective view illustrating a cell according to one embodiment.

[0019] Figure 6 is a cross-sectional view illustrating a cell according to one embodiment.

[0020] FIG. 7 is a graph showing X-ray peaks according to X-ray incidence angle in a cell including a beryllium film according to one embodiment.

[0021] FIG. 8 is a graph showing X-ray peaks according to X-ray incidence angle in a cell including a polyimide film according to one embodiment.

[0022] Specific structural or functional descriptions of the embodiments are disclosed for illustrative purposes only and may be modified and implemented in various forms. Therefore, the actual implementation is not limited to the specific embodiments disclosed, and the scope of this specification includes modifications, equivalents, or alternatives within the technical concepts described in the embodiments.

[0023] Although terms such as "first" or "second" may be used to describe various components, these terms should be interpreted only to distinguish one component from another. For example, a first component may be referred to as a second component, and similarly, a second component may also be referred to as a first component.

[0024] When it is said that a component is "connected" to another component, it should be understood that it may be directly connected or connected to that other component, but there may also be other components in between.

[0025] Singular expressions include plural expressions unless the context clearly dictates otherwise. In this specification, the terms "comprises" or "has" should be understood to indicate the presence of a described feature, number, step, operation, component, part, or combination thereof, but not to exclude the possibility of the presence or addition of one or more other features, numbers, steps, operations, components, parts, or combinations thereof.

[0026] Components included in one embodiment and components that share common functions will be described using the same designations in other embodiments. Unless otherwise stated, descriptions given in one embodiment apply to other embodiments, and detailed descriptions will be omitted to the extent of overlap.

[0027] Unless otherwise defined, all terms used herein, including technical or scientific terms, have the same meaning as commonly understood by a person of ordinary skill in the art. Terms defined in commonly used dictionaries should be interpreted to have a meaning consistent with their meaning in the context of the relevant technology, and will not be interpreted in an idealized or overly formal sense unless explicitly defined herein.

[0028] Hereinafter, embodiments will be described in detail with reference to the attached drawings. In the description with reference to the attached drawings, identical components are assigned the same reference numerals regardless of the drawing numbers, and redundant descriptions thereof will be omitted.

[0029] FIGS. 1 and 2 are perspective views illustrating an X-ray diffraction apparatus with a sample holder connected thereto according to one embodiment.

[0030] Referring to FIGS. 1 and 2, a sample holder (11) according to one embodiment can be used in an in-situ X-ray diffraction device (1). The sample holder (11) can support a sample while being fixed to the main body (12) of the in-situ X-ray diffraction device (1). In one embodiment, the sample may be lithium included in a lithium battery. While X-rays are irradiated to the sample, the sample holder (11) may not move with respect to the main body (12) of the X-ray diffraction device (1). Meanwhile, it should be noted in advance that FIGS. 1 and 2 schematically illustrate only the main body (12) to which the sample holder (11) is connected among the parts of the in-situ X-ray diffraction device (1), and the components such as a chamber accommodating the main body (12), an X-ray generator, etc. are omitted. The sample holder (11) may include a mount (111), a connector (112), and a cell (113).

[0031] A mount (111) is connected to a body (12) of an in-situ X-ray diffraction device (1) and can support a connector (112). The mount (111) can be connected to a fixing element (14) provided on the body (12) of the X-ray diffraction device. In one embodiment, the fixing element (14) can be formed of an elastic material. As the fixing element (14) presses the mount (111), the mount (111) can be supported by a support (13) extending from the body (12) of the in-situ X-ray diffraction device (1). From this structure, a process of detaching or connecting the mount (111) from the in-situ X-ray diffraction device (1) can be simplified. Meanwhile, it should be noted that the connecting means between the in-situ X-ray diffraction device (1) and the mount (111) is not necessarily limited thereto.

[0032] The connector (112) can support the cell (113) while connected to the mount (111). The connector (112) can receive current from the outside and transmit the received current to the cell (113).

[0033] The cell (113) is accommodated in the connector (112) and can contain a sample therein. The cell (113) can be charged and discharged by receiving current from the connector (112).

[0034] The in-situ X-ray diffraction device (1) can irradiate X-rays to the cell (113). The X-rays irradiated toward the cell (113) can pass through the cell (113), irradiate to the sample, and then be diffracted. Formula 2d, also referred to as Bragg's law Depending on the wavelength of the X-ray being investigated ( ) and the angle of incidence of X-rays ( ) can be used to determine the spacing (d) between the grid planes of the sample. Hereinafter, the structures of each of the mount (111), connector (112), and cell (113) will be described in detail.

[0035] FIG. 3 is a perspective view illustrating a mount according to one embodiment, and FIG. 4 is a perspective view illustrating a connector according to one embodiment. FIG. 5 is a perspective view illustrating a cell according to one embodiment, and FIG. 6 is a cross-sectional view illustrating a cell according to one embodiment.

[0036] Referring to FIGS. 3 to 6, a sample holder according to one embodiment may have a structure in which a mount (111), a connector (112), and a cell (113) are assembled. The mount (111) may include a support plate (1111), a base (1112), a connector receiving groove (1113), a first mount hole (1114), and a second mount hole (1115).

[0037] The support plate (1111) can be supported by the main body of the in-situ X-ray diffraction apparatus. The support plate (1111) can be pressed by a fixing element. For example, the support plate (1111) can have a flat structure so as to be stably supported by the main body of the X-ray diffraction apparatus.

[0038] The base (1112) may be formed to extend from the support plate (1111). A connector receiving groove (1113) for receiving the connector (112) may be formed recessed in the base (1112). The base (1112) may support the bottom and side surfaces of the connector (112). Here, the bottom is a surface facing the -z direction.

[0039] Each of the first mount hole (1114) and the second mount hole (1115) may be formed through the base (1112). For example, the first mount hole (1114) and the second mount hole (1115) may be formed through the bottom surface of the base (1112). At least a portion of the bottom surface and the side surface of the connector (112) may be exposed to the outside of the sample holder through the first mount hole (1114) and the second mount hole (1115).

[0040] The connector (112) may have a shape corresponding to the connector receiving groove (1113). The side surface of the connector (112) may contact the base (1112), and the lateral movement of the connector (112) with respect to the base (1112) may be limited. Here, the lateral movement means the movement in the xy plane. Meanwhile, it should be noted in advance that an additional connecting means may be provided between the connector (112) and the base (1112) in order to increase the connection strength between the connector (112) and the base (1112). The connector (112) may include a connector body (1121), a cell receiving groove (1122), a first terminal (1123), and a second terminal (1124).

[0041] The connector body (1121) may be supported by the base (1112). A cell receiving groove (1122) for receiving a cell (113) may be formed in a recessed manner in the connector body (1121). The connector body (1121) may support the bottom and side surfaces of the cell (113).

[0042] A first terminal (1123) and a second terminal (1124) may be connected to a connector body (1121). The first terminal (1123) and the second terminal (1124) may have different polarities. For example, the first terminal (1123) may be a positive pole, and the second terminal (1124) may be a negative pole. Each of one end of the first terminal (1123) and the second terminal (1124) may extend from the bottom of the connector body (1121). One end of the first terminal (1123) may pass through a first mount hole (1114) of the mount (111), and one end of the second terminal (1124) may pass through a second mount hole (1115) of the mount (111). Each end of the first terminal (1123) and the second terminal (1124) can receive current from the outside.

[0043] Meanwhile, in the drawings of this specification, the first terminal (1123) and the second terminal (1124) are illustrated as being arranged along a direction parallel to the y-axis, but it should be noted that the arrangement direction of the first terminal (1123) and the second terminal (1124) is not limited thereto. For example, the first terminal (1123) and the second terminal (1124) may also be arranged along a direction parallel to the x-axis. In such a case, the first mount hole (1114) and the second mount hole (1115) can also be understood to be arranged along a direction parallel to the x-axis.

[0044] The cell (113) may have a shape corresponding to the cell receiving groove (1122). The side surface of the cell (113) may contact the connector (112), and the lateral movement of the cell (113) with respect to the connector (112) may be restricted. From this structure, the bottom and the side surface of the cell (113) may be supported by the connector (112), and the bottom and the side surface of the connector (112) may be supported by the mount (111). Meanwhile, it should be noted in advance that an additional connecting means may be provided between the cell (113) and the connector (112) in order to increase the connection strength between the cell (113) and the connector (112). The cell (113) may include a case (1131), a case hole (1132), a cap (1133), an energy storage element (1134), and a polyimide film (1135).

[0045] The case (1131) and the cap (1133) may be connected to each other to form an internal space. For example, the case (1131) may have a structure including a circular upper surface and a side surface extending in a vertical direction along an edge of the upper surface. An energy storage element (1134) may be arranged in the space surrounded by the case (1131) and the cap (1133). In one embodiment, the case (1131) contacts a first terminal (1123) of the connector (112), wherein the first terminal (1123) may be a positive electrode. The cap (1133) contacts a second terminal (1124) of the connector (112), wherein the second terminal (1124) may be a negative electrode. When current flows through the first terminal (1123) and the second terminal (1124), charging and discharging of energy can occur in the energy storage element (1134).

[0046] A case hole (1132) may be formed through the case (1131). In one embodiment, the case hole (1132) may be covered by a polyimide film (1135). The polyimide film (1135) may function as a window of the cell (113). X-rays may pass through the polyimide film (1135) to reach the energy storage element (1134).

[0047] In one embodiment, the polyimide film (1135) covers the case hole (1132), and the edge of the polyimide film (1135) can be attached to the case (1131). With this structure, the interior of the cell (113) can be sealed from the outside. Meanwhile, it should be noted that, depending on the size of the case (1131) and the cap (1133), a spacer, an elastic body, etc. can be additionally placed in the interior space of the cell (113).

[0048] When a polyimide film (1135) is used as the window of the cell (113), compared to when a beryllium film is used, an X-ray peak generated from the window may be reduced, or an X-ray peak may be generated from the window at an X-ray incidence angle different from the X-ray incidence angle at which the X-ray peak is generated from the sample. The X-ray peak generated from the sample is distinguished from the X-ray peak intensity generated from the window, and the accuracy of the sample analysis may be increased.

[0049] Polyimide films (1135) are cheaper than beryllium films, can be reused repeatedly, and are safe, which can increase cost-effectiveness. The energy storage element (1134) may include an anode (1134a), a cathode (1134b), a separator (1134c), and an electrolyte (1134d).

[0050] The anode (1134a) may be composed of a negative electrode material or a negative electrode active material. In one embodiment, the anode (1134a) may be formed of a lithium layer. In this case, it can be understood that the sample to be analyzed through an X-ray diffraction device is lithium. Meanwhile, it should be noted that the material constituting the anode (1134a) is not necessarily limited to lithium. For example, the anode (1134a) may include silicon (Si), oxide, lithium titanium oxide (LTO), or the like.

[0051] The cathode (1134b) may be composed of a positive electrode material or a positive electrode active material. For example, the cathode (1134b) may include lithium cobalt oxide (LiCoO2), lithium iron phosphate (LiFePO4), lithium nickel manganese cobalt oxide (LiNiMnCoO2), etc. The cathode (1134b) may be arranged on the opposite side of the cap (1133) with respect to the anode (1134a). To prevent direct contact between the anode (1134a) and the cathode (1134b), a separator (1134c) may be arranged between the anode (1134a) and the cathode (1134b). An electrolyte (1134d) can be accommodated inside a cell (113) sealed by a case (1131), a cap (1133), and a polyimide film (1135). Through the electrolyte (1134d), ions move between the anode (1134a) and the cathode (1134b), and through a chemical reaction process, the cell (113) can be charged and discharged. As described above, by using the polyimide film (1135) as a window of the cell (113), the structural change of the lithium layer constituting the anode (1134a) can be clearly analyzed during charging and discharging of the cell (113).

[0052] Meanwhile, it should be noted that the positions where the anode (1134a) and the cathode (1134b) are arranged may be interchanged. For example, the anode (1134a) may face the polyimide film (1135), and the cathode (1134b) may face the cap (1133). In this case, it can be understood that the object to be analyzed through the X-ray diffraction device is the cathode (1134b).

[0053] Fig. 7 is a graph showing X-ray peaks according to X-ray incidence angle in a cell including a beryllium film according to one embodiment. Fig. 8 is a graph showing X-ray peaks according to X-ray incidence angle in a cell including a polyimide film according to one embodiment.

[0054] Referring to FIGS. 7 and 8, in a cell including a polyimide film according to one embodiment, the X-ray peak of the sample can be clearly analyzed compared to a cell including a beryllium film.

[0055] In FIGS. 7 and 8, the x-axis of the graphs is twice the angle (2θ) between the X-rays irradiated on the cell and the surface of the cell through which the X-rays are transmitted, which may be equal to twice the incident angle of the X-rays (e.g., θ in FIG. 5). Hereinafter, for convenience of explanation, twice the angle between the X-rays irradiated on the cell and the surface of the cell through which the X-rays are transmitted is referred to as 2θ.

[0056] In Fig. 7, it can be confirmed that when 2θ is in the range of 22° to 25°, 25° to 27°, 35° to 37°, etc., X-ray peaks having relatively small intensities are generated. These X-ray peaks are X-ray peaks generated from the sample. On the other hand, it can be confirmed that when 2θ is in the range of 28° to 30°, 45° to 47°, 50° to 55°, etc., X-ray peaks having relatively large intensities are generated. These X-ray peaks are X-ray peaks generated from the beryllium film, which is a window. Since the intensity of the X-ray peak generated from the sample is smaller than the X-ray peak generated from the beryllium film, the accuracy of the sample analysis may be low.

[0057] In Fig. 8, it can be confirmed that when 2θ is in the range of 17° to 20°, 35° to 37°, 43° to 47°, etc., X-ray peaks with relatively large intensities are generated. These X-ray peaks are X-ray peaks generated from the sample. Meanwhile, although the values ​​are relatively small and not clearly shown on the graph, when 2θ is in the range of 4° to 4.1°, 5.8° to 6.0°, 14.1° to 14.3°, 29.4° to 29.6°, X-ray peaks may be generated from the polyimide film. Since the intensity of the X-ray peak generated from the sample is greater than the X-ray peak generated from the polyimide film, the accuracy of the sample analysis can be high.

[0058] Although the embodiments described above have been described with limited drawings, those skilled in the art will appreciate that various technical modifications and variations can be applied based on the above. For example, appropriate results can still be achieved even if the described techniques are performed in a different order than described, and / or components of the described systems, structures, devices, circuits, etc. are combined or combined in a different manner than described, or are replaced or substituted with other components or equivalents.

[0059] Therefore, other implementations, other embodiments, and equivalents to the claims also fall within the scope of the claims described below.

Claims

1. In a sample holder for an in-situ X-ray diffractometer, the sample holder comprises: A mount connected to the body of the above in-situ X-ray diffraction device; A connector supported by the above mount and supplied with current from the outside; and A cell is included in the connector and is X-ray irradiated, The above cell is, case; A cap coupled to the above case; An energy storage element disposed between the case and the cap; a case hole formed through the case; and A sample holder covering the case hole and including a polyimide film that is transparent to X-rays.

2. In paragraph 1, The above mount is, A support plate supported by the main body of the above in-situ X-ray diffraction device; A base formed by extending from the above support plate; a connector receiving groove formed in the base and receiving the connector; and A sample holder comprising a first mount hole and a second mount hole formed through the base.

3. In paragraph 2, The above connector, A connector body supported by the above base; A cell receiving groove formed in the above connector body and accommodating the cell; A first terminal connected to the connector body and passing through the first mount hole; and A sample holder comprising a second terminal connected to the connector body, passing through the second mount hole, and having a different polarity from the first terminal.

4. In paragraph 3, The above cell is, A sample holder that contacts the first terminal and the second terminal while being accommodated within the connector body.

5. In paragraph 1, A sample holder in which, when diffraction occurs in the X-rays irradiated to the cell, twice the angle between the X-rays irradiated to the cell and the surface of the cell through which the X-rays are transmitted is between 4° and 4.1°.

6. In paragraph 1, A sample holder in which, when diffraction occurs in the X-rays irradiated to the cell, twice the angle between the X-rays irradiated to the cell and the surface of the cell through which the X-rays are transmitted is between 5.8° and 6°.

7. In paragraph 1, A sample holder in which, when diffraction occurs in the X-rays irradiated to the cell, twice the angle between the X-rays irradiated to the cell and the surface of the cell through which the X-rays are transmitted is between 14.1° and 14.3°.

8. In paragraph 1, A sample holder in which, when diffraction occurs in the X-rays irradiated to the cell, twice the angle between the X-rays irradiated to the cell and the surface of the cell through which the X-rays are transmitted is between 29.4° and 29.6°.

9. In paragraph 1, The above energy storage element is, anode; A cathode positioned on the opposite side of the cap relative to the anode; a separator disposed between the anode and the cathode; and A sample holder comprising an electrolyte contained between the case and the cap.

10. In paragraph 1, The above energy storage element is, cathode; An anode positioned on the opposite side of the cap relative to the cathode; A separator disposed between the cathode and the anode; and A sample holder comprising an electrolyte contained between the case and the cap.

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