Structure for battery analysis

Abstract

Provided is a structure for battery analysis in which an all-solid-state battery is used as a sample battery, wherein even higher airtightness is achieved in order to shield the sample battery S accommodated within a hollow part of a battery accommodation unit 20 from the atmosphere. Specifically, a route indicated by arrows leading from an X-ray window 11 to the sample battery S via a space between a partition member 12 and the inner wall of the battery accommodation unit 20 around the X-ray window 11 is shielded (second airtight structure) by providing an O-ring 51a (airtight member) to a discretionary location on the route.

Description

Structure for battery analysis

[0001] The present invention relates to a structure for battery analysis used when evaluating an all-solid-state battery by X-ray diffraction measurement.

[0002] All-solid-state batteries have a structure in which electrode active material layers are placed on both ends of the electrolyte layer, which causes capacity degradation and resistance increase during charge-discharge cycles. For example, in all-solid-state lithium-ion batteries, the crystal structure is prone to change as lithium ions (Li) are inserted and extracted, so in order to elucidate the degradation mechanism, the changes in the crystal structure that occur during charge and discharge are evaluated using X-ray diffraction measurements.

[0003] In all-solid-state batteries, a solid electrolyte is used in the electrolyte layer. Inside the all-solid-state battery, the various components, such as the electrode active material layer, solid electrolyte layer, and conductive material, expand and contract during charging and discharging, which can easily lead to voids between particles, peeling at the interface between the solid electrolyte layer and the electrode active material layer, or internal cracks. If these phenomena occur, the battery will no longer function properly. Therefore, when analyzing and evaluating this type of all-solid-state battery as a sample battery, it is necessary to maintain the sample battery under pressure to ensure a conductive path and suppress expansion and contraction during charging and discharging.

[0004] Therefore, the present applicant has already proposed a structure for battery analysis that can suppress the expansion and contraction of a sample battery by applying pressure to the battery (see Patent Document 1).

[0005] International Publication No. 2021 / 038943

[0006] The sample battery is housed in the hollow portion of the battery housing unit in a state where it is shielded from the atmosphere, in order to prevent the components that make up the sample battery from chemically reacting with the atmosphere and changing.

[0007] The battery analysis structure disclosed in Patent Document 1 has an X-ray window (11) formed by a cutout hole in a battery accommodating unit, and a partition member (12) is disposed between the X-ray window (11) and an insulating member (21) to form an airtight structure (see Figure 2 in Patent Document 1).

[0008] The inventors recognize that when a liquid battery such as a currently widely used lithium ion battery is used as the sample battery, liquid components leaking from the sample battery due to pressure will enter between the insulating member (21) and the partition member (12), forming a double airtight structure.

[0009] However, such a phenomenon cannot be expected in all-solid-state batteries, and therefore the present inventors have conducted extensive research to achieve even higher airtightness performance in the battery analysis structure according to the present invention, which is intended for all-solid-state batteries, and have come to create the present invention.

[0010] The present invention aims to achieve even higher airtightness in a battery analysis structure using an all-solid-state battery as a sample battery, in order to isolate the sample battery housed in the hollow portion of a battery housing unit from the atmosphere.

[0011] The present invention relates to a battery analysis structure in which a sample battery is an all-solid-state battery in which electrode active material layers are disposed on both end sides of an electrolyte layer and current collector layers are disposed on the outer side of each electrode active material layer, and the structure includes: a battery accommodating unit having a hollow portion for accommodating the sample battery, and an X-ray window formed by a notch that penetrates from the inner wall of the hollow portion to the outside, which irradiates X-rays onto the sample battery accommodated in the hollow portion and allows diffracted X-rays reflected from the sample battery to exit; an insulating member that is fitted into the hollow portion of the battery accommodating unit and is interposed between the sample battery and the inner wall of the hollow portion of the battery accommodating unit so as to surround the outer peripheral surface of the sample battery accommodated in the hollow portion, thereby insulating the outer peripheral surface of the sample battery; and a pressure unit that applies pressure to the sample battery accommodated in the hollow portion of the battery accommodating unit.

[0012] The first invention is characterized in that a thin-plate partition member is disposed between the inner wall around the X-ray window in the battery accommodating unit and the end face of the insulating member surrounding the outer peripheral surface of the sample battery, and an airtight member is disposed between the partition member and the end face of the insulating member, and the insulating member is fixed to the battery accommodating unit while being pressed against the inner wall around the X-ray window, thereby forming a first airtight structure by tightly contacting the end face of the insulating member, the airtight member, the partition member, and the inner wall around the X-ray window, and further forming a second airtight structure by providing another airtight member at any point on a path from the X-ray window to the sample battery, via the inner wall around the X-ray window in the battery accommodating unit and the partition member.

[0013] The second airtight structure may be configured such that the separate airtight member is provided outside the area where the partition member is disposed, between the inner wall of the battery accommodating unit and the insulating member.

[0014] The second airtight structure may be configured such that the separate airtight member is provided between the partition member and an inner wall surrounding the X-ray window in the battery accommodating unit.

[0015] In a second aspect of the present invention, an atmosphere blocking unit is provided outside the battery housing unit so as to surround and seal the X-ray window. Here, it is preferable that the atmosphere blocking unit has a portion facing the X-ray window formed of a material that is transparent to X-rays and blocks the atmosphere.

[0016] As explained above, the first invention is provided with the first and second airtight structures, thereby realizing even higher airtightness. In addition, the second invention is provided with an atmosphere blocking unit outside the battery accommodating unit, thereby realizing even higher airtightness.

[0017] FIG. 1 is a perspective view showing the appearance of a battery analysis structure according to a first embodiment of the present invention. FIG. 2 is a plan view of the battery analysis structure according to the first embodiment of the present invention. FIG. 3 is a cross-sectional view taken along line A-A in FIG. 2. FIG. 4 is an exploded perspective view of the battery analysis structure according to the first embodiment of the present invention. FIG. 5 is an exploded perspective view showing the internal structure of a battery accommodating unit in the battery analysis structure. FIG. 6 is a longitudinal cross-sectional view showing a path from an X-ray window in a battery accommodating unit to a sample battery, the path being blocked by a second airtight structure in the battery analysis structure. FIG. 7 is an exploded perspective view of a pressurizing unit in the battery analysis structure. FIG. 8 is an exploded perspective view of the pressurizing unit and airtight case unit in the battery analysis structure, following FIG. 7. FIG. 9 is a flowchart illustrating a method for analyzing and evaluating a sample battery using the battery analysis structure according to the first embodiment of the present invention. FIG. 10 is a perspective view showing the appearance of a battery analysis structure according to a second embodiment of the present invention. FIG. 11 is a longitudinal cross-sectional view of the battery analysis structure according to the second embodiment of the present invention, taken along the same plane as FIG. 3. FIG. 12 is an exploded perspective view of an air-blocking unit in the battery analysis structure. FIG. 13 is a vertical cross-sectional view showing a modified example of the present invention.

[0018] S: sample battery, 10: pressure receiving portion, 11: X-ray window, 12: partition member, 13: first airtight structure, 14: second airtight structure, 15: first electrode terminal, 20: battery accommodating unit, 21: insulating member, 21a: flange portion, 22: pressing member, 23: female thread portion, 30: pressure unit, 30A: outer body portion, 30B: inner body portion, 31: nut portion, 32: bolt member, 33: pressure transmitting member, 34: load cell, 34a: hermetic connector, 35: male thread portion, 36a: first metal ring, 36b: second metal ring, 37: male thread portion, 40: airtight case unit, 41: female thread portion, 42: second electrode terminal, 43: conductive member, 50: fastener, 51, 51a, 51b: O-ring (airtight member), 52: operating rod 60: Atmospheric isolation unit, 61: Unit body, 61a: Notched space, 61b, 61c: Outer edges of side walls, 62: X-ray transparent belt, 63: Legs

[0019] An embodiment of the present invention will be described in detail below with reference to the drawings. The sample battery to be analyzed and evaluated has an all-solid-state battery configuration, with electrode active material layers disposed on both ends of an electrolyte layer and current collector layers disposed on the outer surfaces of each electrode active material layer. Conventional batteries, such as lithium-ion batteries, use liquid or gel electrolytes for their electrolyte layers. However, all-solid-state batteries, which have been developed in recent years, use solid electrolytes for their electrolyte layers. Inside all-solid-state batteries, expansion and contraction associated with charging and discharging can easily cause voids between particles, peeling at the interface between the solid electrolyte layer and the electrode active material layer, or internal cracks. These phenomena can lead to malfunction of the battery. Therefore, when analyzing and evaluating this type of all-solid-state battery as a sample battery, it is necessary to maintain the sample battery under pressure to ensure a conductive path and suppress expansion and contraction associated with charging and discharging.

[0020] As mentioned above, each element constituting an all-solid-state battery is made of a material that reacts with moisture and air. Therefore, the assembly of a battery analysis structure is generally performed in a space such as a glove box (GB) under an inert atmosphere of high-purity argon gas. Then, the sample battery sealed inside the battery analysis structure is analyzed and evaluated in the atmosphere using an X-ray diffraction device. Here, it is preferable that the X-ray diffraction device be a highly versatile reflection X-ray diffraction device capable of performing the analysis and evaluation. The battery analysis structure according to each embodiment of the present invention described below is configured to satisfy all of the above-mentioned conditions.

[0021] First Embodiment First, a structure for battery analysis according to a first embodiment of the present invention will be described in detail with reference to Figures 1 to 9. Figure 1 is a perspective view showing the appearance of the structure for battery analysis according to this embodiment, Figure 2 is a plan view of the same structure for battery analysis, and Figure 3 is a cross-sectional view taken along line A-A in Figure 2. Furthermore, Figure 4 is an exploded perspective view of the structure for battery analysis according to this embodiment.

[0022] 3 and 4, the battery analysis structure includes, as its components, a battery accommodating unit 20, a pressurizing unit 30, and an airtight case unit 40. Each of these units has one end (upper end in the figure) of the pressurizing unit 30 attached to the open end (lower end in the figure) of the battery accommodating unit 20, and the open end (upper end in the figure) of the airtight case unit 40 attached to the other end (lower end in the figure) of the pressurizing unit 30.

[0023] Fig. 5 is an exploded perspective view showing the internal structure of the battery housing unit. As shown in Figs. 3 and 5, the battery housing unit 20 is formed in a cylindrical shape with one end (the upper end in the figure) closed, and the sample battery S is housed in a hollow space formed inside. The battery housing unit 20 is made of a conductive metal material such as stainless steel.

[0024] If the battery housing unit 20 were made of a metal material, the sample battery S housed within the hollow portion would be electrically short-circuited. Therefore, a cylindrical insulating member 21 is fitted into the hollow portion of the battery housing unit 20, and the sample battery S is housed within the hollow portion of this insulating member 21, thereby insulating the outer surface of the sample battery S with the insulating member 21. The insulating member 21 is formed from an insulating synthetic resin material. It is preferable to prepare insulating members 21 of various dimensions in advance so that the inner diameter of the hollow portion matches the diameter of the various sample batteries S to be analyzed and evaluated, and to replace them depending on the sample battery S.

[0025] The closed end of the battery accommodating unit 20 constitutes a pressure receiving portion 10, and a radially extending elongated X-ray window 11 is formed in the center of this pressure receiving portion by a notch that penetrates the inner wall of the hollow portion and the outside. The shape of the X-ray window 11 is not limited to an elongated hole, and it may be formed in other shapes such as a circle or a rectangle as necessary.

[0026] A thin plate-shaped partition member 12 is arranged between the inner wall surrounding the X-ray window 11 in the battery accommodating unit 20 and the end face of the insulating member 21 surrounding the outer surface of the sample battery S, forming a first airtight structure 13 described below, which prevents air from entering the hollow portion of the battery accommodating unit 20 through the X-ray window 11.

[0027] The partition member 12 is formed from a material that transmits X-rays but does not transmit air or moisture. In this embodiment, the partition member 12 is configured from one of the current collector layers disposed as electrodes on both sides of the sample battery S. The current collector layer is made of conductive metal foil such as aluminum foil or copper foil. This metal foil has the property of transmitting X-rays but not transmitting air or moisture, and therefore can be used as the partition member 12. Therefore, in this embodiment, one of the current collector layers of the sample battery S is separated and disposed opposite the inner wall (inner wall of the pressure receiving portion 10) surrounding the X-ray window 11 in the battery accommodating unit 20.

[0028] In this embodiment, the insulating member 21 also functions as a pressing means for pressing the partition member 12 against the inner wall of the pressure-receiving portion 10. That is, the partition member 12 is disposed opposite the inner wall surrounding the X-ray window 11 formed in the pressure-receiving portion 10, and is pressed against the inner wall of the pressure-receiving portion 10 by the insulating member 21.

[0029] The sample battery S, housed in the hollow portion of the battery housing unit 20 with its outer periphery surrounded by the insulating member 21, is positioned across the partition member 12, facing the X-ray window formed in the pressure receiving portion 10 and the surrounding inner wall. The sample battery S is then pressed against the inner wall of the pressure receiving portion 10 with a given pressure, as will be described later. The pressure receiving portion 10 has the function of receiving the pressure acting on the sample battery S. The X-ray window 11 also has the function of irradiating X-rays onto the end face of the sample battery S housed in the hollow portion of the battery housing unit 20 and emitting diffracted X-rays reflected from the sample battery S to the outside.

[0030] Here, the width of the X-ray window 11 is set to be at least smaller than the width of the sample battery S in order to ensure that the inner wall of the pressure-receiving portion 10 has a sufficient area to receive the pressure from the sample battery S. In addition, the length of the X-ray window 11 and the thickness of the inner wall are preferably determined taking into consideration the measurement range of the X-ray diffraction measurement (X-ray incident angle θ and detected diffraction angle 2θ) required by the analyzer / evaluator of the sample battery S, the pressurization conditions of the sample battery S, etc.

[0031] As described above, a thin plate-like partition member 12 is disposed between the inner wall surrounding the X-ray window 11 in the battery accommodating unit 20 and the end face of the insulating member 21 that surrounds the outer periphery of the sample battery S. Furthermore, an O-ring (airtight member) 51 is disposed between the partition member 12 and the end face of the insulating member 21. Specifically, a groove for disposing the O-ring 51 is formed in the end face of the insulating member, and the O-ring is disposed in this groove. Then, by fixing the insulating member 21 to the battery accommodating unit 20 while pressing it against the inner wall surrounding the X-ray window 11, the end face of the insulating member 21, the O-ring 51, the partition member 12, and the inner wall surrounding the X-ray window 11 are brought into close contact with each other, forming a first airtight structure 13.

[0032] As shown in Fig. 5, insulating member 21 has flange portion 21a formed thereon, which expands radially outward from the outer peripheral surface, and flange portion 21a is fastened to the inner wall of battery housing unit 20 with fasteners 50 such as bolts and screws. The fastening force (pressing force) applied at this time presses partition member 12 against the inner wall of pressure-receiving portion 10 via O-ring 51 (see Fig. 3). As a result, partition member 12 comes into close contact with the periphery of X-ray window 11, closing it.

[0033] Now, let us focus on the path indicated by the arrow in Figure 6. That is, this path runs from the X-ray window 11 through the gap between the inner wall surrounding the X-ray window 11 in the battery housing unit 20 and the partition member 12 (specifically, between the inner wall of the pressure-receiving portion 10 and the upper surface of the partition member 12, which is in close contact with this inner wall), to the sample battery S. This path is airtight because the partition member 12 and the insulating member 21 are in close contact with the inner wall of the battery housing unit 20. To further enhance airtightness, however, it is preferable to install an airtight member at any point along this path to block this path (to block the flow of air along this path). (Note that Figure 6 shows the path already blocked by the O-ring 51a.)

[0034] Therefore, in the present invention, an airtight member is provided at any location on the above-mentioned path to form a second airtight structure 14 that blocks the path. For example, the second airtight structure 14 can be formed by providing an airtight member between the inner wall of the battery accommodating unit 20 and the insulating member 21 at any location where the inner wall of the battery accommodating unit 20 and the insulating member 21 contact each other outside the area where the partition member 12 is arranged.

[0035] 3 and 4, an O-ring 51a (airtight member) is provided between the upper surface of the flange portion 21a of the insulating member 21 and the opposing inner wall of the battery accommodating unit 20, thereby forming the second airtight structure 14. Specifically, a groove is formed in the upper surface of the flange portion 21a of the insulating member 21, and the O-ring 51a is disposed in the groove. When the insulating member 21 is fastened and fixed to the inner wall of the battery accommodating unit 20 with a fastener 50, the O-ring 51a is compressed by the tightening force (pressure force), and the second airtight structure 14 is formed between the insulating member 21 and the inner wall of the battery accommodating unit 20.

[0036] By forming the second airtight structure 14, the path indicated by the arrow in FIG. 6 is blocked by the O-ring 51a (airtight member), and the airtightness inside the hollow portion of the battery accommodating unit 20 can be further improved.

[0037] The above-described attachment of the partition member 12, insulating member 21, and O-rings 51, 51a to the battery accommodating unit 20 is performed before the sample battery S is housed in the hollow portion of the battery accommodating unit 20. Therefore, this work can be performed in the atmosphere, and the fastening of the insulating member 21 with the fastener 50 can also be performed easily and without cumbersome work.

[0038] 7 and 8 are exploded perspective views of the pressurizing unit and airtight case unit, with Fig. 8 continuing below Fig. 7. Note that some components are depicted overlappingly in each of these figures. The pressurizing unit 30 has the function of applying pressure to the sample battery S housed within the hollow portion of the battery housing unit 20 (specifically, within the hollow portion of the insulating member 21) (see Fig. 3).

[0039] The pressurizing unit 30 has a cylindrical body portion. The body portion is composed of an outer body portion 30A and an inner body portion 30B, and the inner body portion 30B, which is also cylindrical, is fitted into the interior (hollow portion) of the outer body portion 30A and fixed together with fasteners 50 such as bolts and screws (see FIGS. 8, 3, and 4).

[0040] The outer body portion 30A is made of a synthetic resin material (e.g., polyvinyl chloride (PVC), polyvinylidene chloride (PVdC), polystyrene (PS), acrylonitrile-styrene copolymer (AS resin), acrylonitrile-butadiene-styrene copolymer (ABS resin), polyethylene styrene (HDPE), polypropylene (PP), polyacetal (POM), polymethyl methacrylate (PMMA), methacrylate-styrene copolymer (MS), polycarbonate (PC), polychlorotrifluoroethylene (PCTFE), tetrafluoroethylene (PTFE), or the like) that has electrical insulation, strength, and airtightness sufficient to withstand the reaction of the pressurizing force. On the other hand, the inner body portion 30B is made of a metal material that has strength sufficient to withstand the reaction of the pressurizing force.

[0041] The inner circumferential surface of the inner body portion 30B is formed in a stepped shape as shown in FIG. 3 , and a nut portion 31 is formed on the inner circumferential surface of the portion with a smaller inner diameter (the lower half of the figure). A single bolt member 32 is threadedly engaged with this nut portion 31. The bolt member 32 constitutes a pressure mechanism for applying pressure to the sample battery S housed within the hollow portion of the battery housing unit 20. Furthermore, as will be described later, this bolt member 32 forms a conductive path for charging and discharging the sample battery S. For this reason, the bolt member 32 is made of a metallic material that is strong enough to apply high pressure to the sample battery S and has electrical conductivity.

[0042] A pressure transmission member 33 is slidably fitted into the inner circumferential surface of the large-diameter portion of the inner body 30B (the upper half of FIG. 3 ), and a load cell 34 is incorporated into this pressure transmission member 33 as a pressure measurement means. The load cell 34 measures the pressure generated by the screwing of the bolt member 32 and outputs an electrical signal indicating the measurement value. This output is sent to a pressure indicator (not shown). Measuring the pressure in this manner makes it possible to analyze and evaluate the correlation between the pressure acting on the sample battery S and changes in the crystal structure of the sample battery S that accompany charging and discharging.

[0043] In this embodiment, a hermetic connector 34a is provided on the outer body 30A of the pressurizing unit 30 as an interface for outputting an electrical signal from the load cell 34. The hermetic connector 34a ensures airtightness while exposing its terminals to the outer peripheral surface of the pressurizing unit 30. This eliminates the risk of air entering the interior of the pressurizing unit 30 from the signal output portion of the load cell 34.

[0044] As will be described later, the pressure transmitting member 33 and the load cell 34 also form a conductive path for charging and discharging the sample battery S. For this reason, they are made of a conductive metal material. Note that the pressure measuring means is not limited to a load cell; for example, a torque wrench can be used instead of the load cell to determine the pressure from the torque acting on the bolt member 32.

[0045] As shown in Figures 1, 3, and 4, the pressurizing unit 30 is attached to the open end (bottom end in the figure) of the battery housing unit 20. A cylindrical pressing member 22 is inserted into the hollow portion of the battery housing unit 20 (specifically, the hollow portion of the insulating member 21). This pressing member 22 is interposed between the load cell 34 and the sample battery S and functions to press the sample battery S toward the pressure-receiving portion 10 of the battery housing unit 20 with the pressing force from the bolt member 32. That is, as the bolt member 32 is screwed in, a pressing force is applied to the sample battery S via the pressure transmission member 33, the load cell 34, and the pressing member 22, pressing the sample battery S against the pressure-receiving portion 10 of the battery housing unit 20. This allows the sample battery S to be pressurized. The amount of pressure applied can be set as desired by adjusting the amount of screwing of the bolt member 32 while referring to the display on the pressure indicator (not shown).

[0046] As will be described later, the pressing member 22 also forms a conductive path for charging and discharging the sample battery S. For this reason, the pressing member 22 is made of a conductive metal material.

[0047] 3, 4, and 8, the airtight case unit 40 is formed in a cylindrical shape with a bottom, and its open end (upper end in the figure) is attached to the end (lower end in the figure) of the pressurizing unit 30 on the side where the head of the bolt member 32 is exposed. The bottom of the airtight case unit 40 is closed.

[0048] The airtight case unit 40 has the function of sealing the area around the exposed head of the bolt member 32 of the pressurizing unit 30, thereby isolating the surrounding space from the atmosphere. This makes it possible to prevent air from entering the battery accommodating unit 20 through a small gap at the portion where the bolt member 32 and the nut portion 31 are engaged.

[0049] The airtight case unit 40 is formed from an electrically insulating synthetic resin material (for example, polyvinyl chloride (PVC), polyvinylidene chloride (PVdC), polystyrene (PS), acrylonitrile-styrene copolymer (AS resin), acrylonitrile-butadiene-styrene copolymer (ABS resin), polyethylene styrene (HDPE), polypropylene (PP), polyacetal (POM), polymethyl methacrylate (PMMA), methacrylate-styrene copolymer (MS), polycarbonate (PC), trifluorochloroethylene (PCTFE), tetrafluoroethylene (PTFE), or the like.

[0050] 4, the pressurizing unit 30 is formed with a male thread 35, while the inner wall of the open end of the battery accommodating unit 20 is formed with a female thread 23 (see FIG. 3) that screws into the male thread 35. The pressurizing unit 30 is attached to the open end of the battery accommodating unit 20 by screwing the male thread 35 into the female thread 23.

[0051] 7 , the male thread portion 35 of the pressure unit 30 is formed on the outer peripheral surface of a first metal ring 36a. This first metal ring 36a is supported by a second metal ring 36b. That is, the second metal ring 36b is first fastened to one end of the outer body portion 30A with fasteners 50 such as bolts and screws, and then the first metal ring 36a is fastened to the second metal ring 36b with fasteners 50 such as bolts and screws. The second metal ring 36b functions as a reinforcing member for the outer body portion 30A, which is made of a synthetic resin material as described above. By providing this second metal ring 36b, damage to the outer body portion 30A can be avoided even when the male thread portion 35 is screwed into the female thread portion 23 with a large tightening force.

[0052] 4, the pressurizing unit 30 is formed with a male thread 37, while the inner wall of the open end of the airtight case unit 40 is formed with a female thread 41 that screws onto the male thread 37 (see FIG. 3). The airtight case unit 40 is attached to the pressurizing unit 30 by screwing the male thread 37 into the female thread 41.

[0053] In this way, the pressurizing unit 30 can be attached to the battery accommodating unit 20 by simply screwing in a pair of male and female threaded portions, thereby sealing the space between the battery accommodating unit 20 accommodating the sample battery S and the pressurizing unit 30. Similarly, the airtight case unit 40 can be attached to the pressurizing unit 30 by simply screwing in a pair of male and female threaded portions, thereby sealing the periphery of the other end face of the pressurizing unit 30 where the bolt member 32 (pressurizing mechanism) is exposed. Therefore, even if the worker is performing the assembly work from outside the glove box while wearing gloves, the worker can easily perform the work.

[0054] These screwing operations do not require special tools; for example, one unit to be screwed can be fixed in place, and the other unit can be grasped and easily screwed in manually. In this embodiment, as shown in Fig. 1, a control rod 52 for screwing operations is provided on the outer peripheral surface of the battery accommodating unit 20, protruding radially. The worker can perform the above-mentioned screwing operations even more easily by simply turning this control rod 52 by hand.

[0055] Since the female thread portion 23 is formed in the metal battery accommodating unit 20, the male thread portion 35 that screws into the female thread portion 23 is also formed on the outer circumferential surface of the first metal ring 36a. This allows the male thread portion 35 to have the same wear resistance, strength, etc. as the female thread portion 23.

[0056] Also, an O-ring 51 serving as a sealing member is provided on the end faces where the battery accommodating unit 20 and the pressurizing unit 30 come into close contact with each other. Furthermore, an O-ring 51 serving as a sealing member is also provided on the end faces where the pressurizing unit 30 and the airtight case unit 40 come into close contact with each other. By using these O-rings 51, it is possible to easily seal the units together simply by manually screwing them together.

[0057] As shown in FIG. 1, the structure for battery analysis of this embodiment has a first electrode terminal 15 and a second electrode terminal 42 on the outside.

[0058] The first electrode terminal 15 is fixed to the outer surface of the battery accommodating unit 20 by fasteners 50 such as bolts and screws. The battery accommodating unit 20 is formed of a conductive metal material. Therefore, the first electrode terminal 15 is electrically connected to one of the electrode active material layers of the sample battery S via the battery accommodating unit 20 and the conductive partition member 12 (current collector layer) (see FIGS. 3 and 5 ).

[0059] The second electrode terminal 42 is fixed to the outer circumferential surface of the airtight case unit 40 by fasteners 50 such as bolts and screws. A conductive member 43 that is electrically connected to the second electrode terminal 42 is disposed inside the airtight case unit 40 (see FIG. 3 ). The conductive member 43 is formed from a metal plate having spring properties, and is positioned so that the head of the bolt member 32 abuts against the conductive member 43 when the airtight case unit 40 is attached to the pressurizing unit 30.

[0060] Therefore, the second electrode terminal 42 is electrically connected to the other electrode active material layer of the sample battery S via the conductive path formed by the conductive member 43, the bolt member 32, the pressure transmission member 33, the load cell 34, and the pressing member 22.

[0061] Therefore, by passing electricity between these first electrode terminal 15 and second electrode terminal 42, the sample battery S contained inside the battery accommodating unit 20 can be charged, and by establishing electrical conduction between these electrode terminals via a resistor, the sample battery S can be discharged.

[0062] The first electrode terminal 15 and the second electrode terminal 42 are insulated from each other by an outer body portion 30A made of synthetic resin in the pressurizing unit 30 and an airtight case unit 40 also made of synthetic resin.

[0063] Next, an example of a method for analyzing and evaluating a sample battery using the battery analysis structure according to this embodiment will be described with reference to Fig. 9. First, a partition member 12 (current collector layer) is placed on the pressure receiving portion 10 of the battery accommodating unit 20, and an insulating member 21 is attached to the battery accommodating unit 20 (step S1). This presses the partition member 12 (current collector layer) against the pressure receiving portion 10 of the battery accommodating unit 20, sealing the X-ray window 11. The steps up to this point can be performed outside the glove box.

[0064] Next, the necessary components, battery materials, pressure indicator, etc. are stored inside a glove box filled with an inert gas (for example, argon gas) (step S2).

[0065] The worker puts on the gloves provided in the glove box and first molds the sample battery S inside the glove box (step S3). Next, the molded sample battery S is housed in the hollow portion of the insulating member 21 attached to the battery housing unit 20, and the pressing member 22 is also inserted into the hollow portion of the insulating member (step S4).

[0066] Next, the pressurizing unit 30 is attached to the battery accommodating unit 20 (step S5), and further, a pressure indicator is connected to the load cell 34 (step S6).

[0067] After completing the above steps, the bolt members 32 are screwed in while watching the pressure indicator, applying pressure to the sample battery S inside the battery housing unit 20 (Step S7). The bolt members 32 are screwed in using a tool such as a wrench. When the pressure acting on the sample battery S reaches the target value, the screwing of the bolt members 32 is terminated (Step S8).

[0068] Next, the airtight case unit 40 is attached to the pressurizing unit 30 (step S9), and the pressure indicator is removed from the load cell 34 (step S10). The assembly of the battery analysis structure is completed by attaching the airtight case unit 40. Thereafter, the battery analysis structure is removed from the glove box (step S11).

[0069] Next, the battery analysis structure is mounted on the X-ray diffraction device (step S12), and a charge / discharge device is connected to the first and second electrode terminals 15, 42 (step S13). Then, X-ray diffraction measurement is performed on the sample battery S while charging and discharging the sample battery S (step S14), and the characteristics of the sample battery S are analyzed and evaluated based on the measurement data. A pressure indicator can be connected to the hermetic connector 34a during or after the X-ray diffraction measurement to measure the pressure acting on the sample battery S. This allows the measurement results from the X-ray diffraction measurement to be analyzed and evaluated in relation to the pressure of the sample battery S. Note that X-ray diffraction measurement can also be performed on the sample battery S after charging and discharging the sample battery S.

[0070] Second Embodiment Next, a battery analytical structure according to a second embodiment of the present invention will be described with reference to Figures 10 to 12. Note that parts that are the same as or correspond to those in the first embodiment described above are given the same reference numerals, and detailed descriptions thereof will be omitted.

[0071] The battery analysis structure according to this embodiment is configured such that an atmosphere blocking unit 60 is provided on the outside of the battery accommodating unit 20 so as to surround and seal the X-ray window 11. As shown in Fig. 12, the atmosphere blocking unit 60 includes a unit main body 61 and an X-ray transparent belt 62. The unit main body 61 is made of a conductive metal material, and is fastened and fixed to the outer end surface of the battery accommodating unit 20 on which the X-ray window 11 is formed, using fasteners 50 such as bolts and screws.

[0072] An O-ring 51 is provided as a sealing member on the end surface where the battery accommodating unit 20 and the atmosphere blocking unit 60 come into close contact with each other. By providing the O-ring 51, the units 20, 60 can be easily sealed from each other simply by manually screwing in the fastener 50.

[0073] 11 and 12, the unit main body 61 is formed with a cutout space 61a that opens radially around the X-ray window 11 formed in the battery housing unit 20, and both side walls of the cutout space 61a are formed in a semicircular arc shape. X-ray transparent belts 62 are provided in close contact with outer edges 61b, 61c of these semicircular arc-shaped both side walls. As a result, the space outside the X-ray window 11 formed in the battery housing unit 20, i.e., the cutout space 61a, is sealed by the X-ray transparent belts 62, preventing the intrusion of air.

[0074] The X-ray transparent belt 62 may be made of a material that is transparent to X-rays and shields the atmosphere, such as the following: For example, metal materials such as beryllium and aluminum are suitable for the X-ray transparent belt 62. Furthermore, artificial minerals such as graphite, glassy carbon, diamond, SiN, quartz, and sapphire are suitable for the X-ray transparent belt 62. Furthermore, polymer materials such as polyethylene film (PE film), polyvinyl chloride film (PVC film), polyvinylidene chloride film (PVDC film), polyvinyl alcohol film (PVA film), polypropylene film (PP film), polycarbonate film (PC film), polystyrene film (PS film), polyacrylonitrile film (PAN film), ethylene-vinyl acetate copolymer film (EVA film), ethylene-vinyl alcohol copolymer film (EVOH film), polyetherimide (PEI), and aromatic polyether ketone (PEEK) are suitable for the X-ray transparent belt 62. Polymer materials are basically thermoplastic resins, and also include fluororesins, in which hydrogen is replaced with fluorine. Additionally, a multilayer processed belt such as one obtained by coextrusion, a single vapor deposition or composite vapor deposition of aluminum, alumina, or silica, or a surface-treated belt thereof are also suitable for the X-ray transparent belt 62. The X-ray transparent belt 62 is attached to the outer edges 61b, 61c of the semicircular arc-shaped side walls of the unit body 61 with an adhesive or joined by brazing.

[0075] By providing the atmosphere blocking unit 60 configured as described above on the outside of the battery housing unit 20 so as to surround and seal the X-ray window 11, it is possible to prevent the intrusion of atmosphere into the interior of the battery housing unit 20 through the X-ray window 11. Moreover, since the periphery of the X-ray window 11 is open in the radial direction and an X-ray transparent belt 62 is provided opposite the X-ray window 11, X-rays (Xa) can be irradiated onto the sample battery S inside the battery housing unit 20 through the X-ray window 11 from a low angle, as shown in Figure 11. Furthermore, diffracted X-rays (Xb) reflected at a low angle from the sample battery S can be extracted through the X-ray transparent belt 62.

[0076] 10, the atmosphere cutoff unit 60 has four protruding legs 63. Before assembling the atmosphere cutoff unit 60 to the battery accommodating unit 20 or after removing it from the battery accommodating unit 20, the atmosphere cutoff unit 60 can be placed on a work table using these legs 63, thereby protecting the surface of the X-ray transparent belt 62 and preventing it from being scratched.

[0077] [Modifications or Applications] The present invention is not limited to the above-described embodiment, and various modifications and applications are possible. The components, such as the battery accommodating unit, pressurizing unit, airtight case unit, insulating member, and atmosphere blocking unit, are not limited to the structures of the above-described embodiment. For example, the design of which parts of each component are made of conductive or insulating materials can be changed as appropriate depending on the installation locations of each electrode terminal, etc.

[0078] Furthermore, as a modification of the first embodiment, as shown in FIG. 13 , an O-ring 51 b (airtight member) can be provided between the inner wall around the X-ray window 11 in the battery accommodating unit 20 and the partition member 12, and the O-ring 51 can be compressed by the end face of the insulating member 21 to form a second airtight structure 14.

[0079] In the above-described embodiments, an O-ring is used as the airtight member, but various sealing parts other than an O-ring may be used as the airtight member as needed. For example, a second airtight structure may be formed by applying vacuum grease as an airtight member between the inner wall around the X-ray window 11 and the partition member 12 in the battery housing unit 20 shown in FIG. 13 instead of the O-ring 51a.

Claims

1. A battery analysis structure using an all-solid-state battery as a sample battery, in which electrode active material layers are disposed on both ends of an electrolyte layer and current collector layers are disposed on the outer sides of each electrode active material layer, comprising: a battery housing unit having a hollow portion for accommodating the sample battery, and an X-ray window formed by a cutout hole penetrating from the inner wall of the hollow portion for irradiating X-rays onto the sample battery accommodated in the hollow portion and for emitting diffracted X-rays reflected from the sample battery to the outside; an insulating member fitted into the hollow portion of the battery housing unit and interposed between the sample battery and the inner wall of the hollow portion of the battery housing unit so as to surround the outer peripheral surface of the sample battery accommodated in the hollow portion, thereby insulating the outer peripheral surface of the sample battery; and a pressure unit for applying pressure to the sample battery accommodated in the hollow portion of the battery housing unit. a thin-plate partition member is disposed between the inner wall around the X-ray window in the battery accommodating unit and the end face of the insulating member surrounding the outer peripheral surface of the sample battery, and an airtight member is disposed between the partition member and the end face of the insulating member, and the insulating member is fixed to the battery accommodating unit while being pressed against the inner wall around the X-ray window, thereby bringing the end face of the insulating member, the airtight member, the partition member, and the inner wall around the X-ray window into close contact with each other, thereby forming a first airtight structure; and a second airtight structure is formed by providing another airtight member at any point on a path from the X-ray window to the sample battery, via the inner wall around the X-ray window in the battery accommodating unit and the partition member, to block the path.

2. The battery analysis structure described in claim 1, characterized in that the second airtight structure is configured such that another airtight member is provided outside the area in which the partition member is arranged, between the inner wall of the battery accommodating unit and the insulating member.

3. The battery analysis structure described in claim 1, characterized in that the second airtight structure is configured such that the other airtight member is provided between the inner wall surrounding the X-ray window in the battery accommodating unit and the partition member.

4. A battery analysis structure using an all-solid-state battery as a sample battery, in which electrode active material layers are disposed on both ends of an electrolyte layer and current collector layers are disposed on the outside of each electrode active material layer, comprising: a battery accommodating unit having a hollow portion for accommodating the sample battery, and an X-ray window formed by a cutout hole penetrating from the inner wall of the hollow portion for irradiating X-rays onto the sample battery accommodated in the hollow portion and for emitting diffracted X-rays reflected from the sample battery to the outside; an insulating member fitted into the hollow portion of the battery accommodating unit and interposed between the sample battery and the inner wall of the hollow portion of the battery accommodating unit so as to surround the outer surface of the sample battery accommodated in the hollow portion and insulate the outer surface of the sample battery; and a pressure unit for applying pressure to the sample battery accommodated in the hollow portion of the battery accommodating unit; and further comprising an air-blocking unit provided outside the battery accommodating unit so as to surround and seal the X-ray window.

5. A battery analysis structure as described in claim 4, characterized in that the portion of the atmosphere-blocking unit facing the X-ray window is formed from a material that is transparent to X-rays and blocks the atmosphere.

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