JP2013205077A - Sample holding device, and sample analysis method - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a sample holding device for performing the measurement by beam irradiation with an environment with which front and rear faces of a sample contact separated.SOLUTION: A sample holding device 1 includes a holder holding a sample 99. The holder includes: a front-side environmental chamber 18 formed in a manner to contact with a front face of the sample 99; a back-side environmental chamber 28 formed in a manner to contact with a rear face of the sample 99; a beam incidence port 16 for letting a beam enter the sample 99; and a beam outgoing port 26 for letting the beam go out of the sample 99.

Description

  The present invention relates to a sample holding device and a sample analysis method, and more particularly to a sample holding device for holding a sample for beam irradiation and a sample analysis method for analyzing a sample by irradiating a beam.

  Conventionally, a sample analysis method for analyzing a sample by irradiating the sample with a beam such as an electromagnetic wave or a particle beam is known. In order to perform measurement with high accuracy, it is necessary to hold the sample so that the position irradiated with the beam is constant.

  In measurement by beam irradiation, there are cases where it is desired to perform measurement while changing the environment of the sample (medium, temperature, humidity, pressure, electric field, magnetic field, etc.). For example, there is a case where it is desired to distribute the solution in the sample chamber in order to cause the solution to act on the sample. In this case, the sample holding device is required to have a structure capable of allowing the solution to flow through the sample chamber and fixing the sample so as not to move.

  In Japanese Patent Application Laid-Open No. 2008-64463 (Patent Document 1), a sample of a soft material to be irradiated with a beam can be easily fixed so as not to move to a measuring apparatus, and the solution can be more uniformly applied to the sample. A structure analysis method and a soft material holding device of a soft material by beam irradiation for performing measurement while maintaining a simple state are described.

JP 2008-64463 A

  By the way, in the case of a plate-like or film-like sample, it may be desired to separate the environment where the front and back surfaces of the sample are in contact. For example, there is a case where it is desired to measure the solution permeability of a sample by applying a solution from one side of the sample. At this time, if measurement by beam irradiation is also performed, the correlation between the crystal structure of the sample obtained from beam irradiation and the solution permeability can be examined.

  In the case of a sample having a large solid difference or site difference, such as biological skin, it is preferable to perform these two measurements simultaneously on the same sample. That is, it is preferable to perform measurement by beam irradiation by separating the environment where the front and back surfaces of the sample are in contact.

  In the soft material holding device described in Patent Document 1, the skin as a sample is crumpled and inserted into a sample accommodation hole of a plate-like sample accommodation member having solution permeability. Therefore, in this soft material holding device, the distributed solution acts on the sample from the entire periphery of the sample. Therefore, this soft material holding device cannot separate the environment where the front and back surfaces of the sample are in contact and perform measurement by beam irradiation.

  An object of the present invention is to separate an environment where the front and back surfaces of a sample are in contact with each other and perform measurement by beam irradiation, and to provide a sample holding device therefor.

  The sample holding device according to the present invention includes a holder for holding a sample. The holder includes a front-side environment chamber formed so as to be in contact with the surface of the sample, a back-side environment chamber formed so as to be in contact with the back surface of the sample, a beam entrance for allowing a beam to enter the sample, and a beam from the sample. And a beam exit for emitting.

  According to this configuration, the environment in which the front and back surfaces of the sample are in contact with each other can be separated by the front-side environment chamber and the back-side environment chamber.

  Preferably, the boundary between the holder and the sample is sealed. As a result, the front-side environmental chamber and the back-side environmental chamber are effectively separated.

  Preferably, the holder further includes an environment communication passage that leads to one of the front environment chamber and the back environment chamber and opens to the outside. As a result, the environment of the front environment room or the back environment room can be measured or controlled.

  Preferably, the holder further includes a front side member disposed on the front side of the sample and a back side member disposed on the back side of the sample and attachable to and detachable from the front side member. The front side environmental chamber is formed in the front side member, and the back side environmental chamber is formed in the back side member. One of the beam entrance and the beam exit is formed in the front member, and the other of the beam entrance and the beam exit is formed in the back member. According to this structure, a holder can be divided | segmented into a front side member and a back side member. As a result, the sample can be easily exchanged.

  Preferably, the sample holding device includes a control member that is disposed in contact with the sample and controls experimental conditions of the sample. According to this configuration, since the control member is arranged in contact with the sample, the experimental conditions of the sample can be controlled.

  Preferably, the control member has a thermal conductivity higher than that of the holder. Thereby, for example, the temperature of the sample can be controlled.

  Preferably, the control member has an electrical resistance lower than that of the holder. Thereby, for example, an electric field can be applied to the sample.

  The sample analysis method according to the present invention separates the front-side environment in contact with the surface of the sample and the back-side environment in contact with the back surface of the sample and holds the sample, and the beam is incident on the sample and the beam emitted from the sample is observed A process.

  Preferably, the sample analysis method further includes a step of measuring at least one of the front side environment and the back side environment.

  Preferably, the sample analysis method further includes a step of controlling at least one of the front side environment and the back side environment.

  According to the present invention, measurement by beam irradiation can be performed by separating the environment where the front and back surfaces of the sample are in contact with each other. In addition, a sample holding device for that purpose is obtained.

It is a disassembled perspective view which shows schematic structure of the sample holding device by the 1st Embodiment of this invention. It is sectional drawing along the II-II line of FIG. It is a disassembled perspective view which shows schematic structure of the sample holding device by the 2nd Embodiment of this invention. FIG. 4 is a cross-sectional view taken along line IV-IV in FIG. 3. It is a schematic diagram which shows an example of control of the experimental condition by a control member. It is a disassembled perspective view which shows schematic structure of the sample holding device by the 3rd Embodiment of this invention. It is a disassembled perspective view which shows schematic structure of the sample holding device by the 4th Embodiment of this invention. It is a disassembled perspective view which shows schematic structure of the sample holding device by the 5th Embodiment of this invention. It is a figure for demonstrating an example of the sample analysis method, Comprising: It is typical sectional drawing of the sample holding device by one Embodiment of this invention. It is a figure for demonstrating the other example of the sample analysis method, Comprising: It is typical sectional drawing of the sample holding device by one Embodiment of this invention. It is a figure for demonstrating the other example of the sample analysis method, Comprising: It is typical sectional drawing of the sample holding device by one Embodiment of this invention. It is a graph which shows the temperature change of the transdermal moisture transpiration | evaporation amount of a human stratum corneum, and the order of a lipid molecule. It is a graph which shows the temperature change of the transdermal moisture transpiration | evaporation amount of a mouse | mouth stratum corneum, and the order of a lipid molecule.

  Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings. In the drawings, the same or corresponding parts are denoted by the same reference numerals and description thereof will not be repeated. In addition, the dimension of the member in each figure does not represent the dimension of an actual structural member, the dimension ratio of each member, etc. faithfully.

[First Embodiment]
FIG. 1 is an exploded perspective view showing a schematic configuration of a sample holding device 1 according to a first embodiment of the present invention. The sample holding device 1 includes a holder H1, O-rings 31 and 32, and polymer films 33 and 34.

  The holder H <b> 1 includes a front side member 10 and a back side member 20. The front side member 10 has a substantially rectangular parallelepiped shape and includes a recess 12 formed on the lower surface thereof. The back-side member 20 includes a substantially rectangular parallelepiped main body 21 and a convex portion 22 formed on the upper surface of the main body 21. The convex portion 22 is formed so as to fit into the concave portion 12. The holder H <b> 1 holds the sample 99 by sandwiching the sample 99 between the concave portion 12 and the convex portion 22. The sample 99 is typically plate-shaped, for example human skin.

  The material of the holder H1 is not particularly limited. The material of the holder H1 is, for example, an acrylic resin.

  For convenience of explanation, the x direction, the y direction, and the z direction are defined as shown in FIG. The x direction, the y direction, and the z direction coincide with one of the normals of the outer surface of the main body portion 21 of the front side member 10 and the back side member 20.

  The bottom surface of the concave portion 12 and the top surface of the convex portion 22 are substantially parallel. The recess 12 has a triangular prism shape that is tilted sideways. Specifically, the recess 12 has a triangular cross section, and the depth of the recess 12 increases toward the downstream in the y direction. Similarly to the concave portion 12, the convex portion 22 has a triangular prism shape that is tilted sideways. Specifically, the convex portion 22 has a triangular side surface, and the height of the convex portion 22 increases toward the downstream in the y direction.

  A groove 13 for arranging the O-ring 31 is formed on the slope of the recess 12. A groove 23 for arranging the O-ring 32 is formed on the slope of the convex portion 22. The holder H1 holds the sample 99 with the O-rings 31 and 32 interposed therebetween, whereby the boundary between the holder H1 and the sample 99 is sealed. That is, the holder H1 and the sample are brought into close contact (adherence) with a sealing property.

  The front side member 10 includes through holes 14 and 15 formed in parallel with the z direction. The back side member 20 includes through holes 24 and 25 formed in parallel with the z direction. The through hole 14 of the front side member 10 and the through hole 24 of the back side member 20 are formed to be coaxial with each other when the convex portion 22 is fitted into the concave portion 12. At this time, the through hole 15 and the through hole 25 are formed so as to be coaxial with each other. The front-side member 10 and the back-side member 20 can be fixed by passing a bolt (not shown) from one end of these through holes and tightening a bolt (not shown) at the other end. Moreover, the bolt and nut which were fastened can be loosened and the front side member 10 and the back side member 20 can be divided | segmented. That is, the front side member 10 and the back side member 20 are formed to be detachable.

  The front side member 10 includes a beam entrance 16 for allowing a beam to enter the sample 99. The beam entrance 16 has a cylindrical shape having a central axis parallel to the y direction. The beam entrance 16 opens on the side surface of the front side member 10 on the upstream side in the y direction and communicates with the recess 12. In other words, the beam entrance 16 penetrates the front side member 10 in the y direction.

  A polymer film 33 is bonded to the front member 10 so as to cover the opening on the upstream side in the y direction of the beam entrance 16. The opening on the upstream side in the y direction of the beam incident light 16 is sealed by the polymer film 33.

  The back side member 20 includes a beam emission port 26 for emitting a beam from the sample 99. The beam exit port 26 has a central axis parallel to the y direction, and has a conical shape whose diameter increases toward the downstream in the y direction. The beam exit 26 penetrates the convex portion 22 of the back side member 20 in the y direction.

  A polymer film 34 is bonded to the back member 20 so as to cover the opening on the downstream side in the y direction of the beam exit port 26. The opening on the downstream side in the y direction of the beam exit port 26 is sealed by the polymer film 34.

  The polymer films 33 and 34 preferably have a high beam transmittance. In general, the thinner the film, the higher the beam transmission. Therefore, it is preferable that the polymer films 33 and 34 can maintain high strength even if they are thinned. The polymer films 33 and 34 are polyimide films, for example.

  The front side member 10 further includes a front side environment communication passage 17. The front-side environment communication passage 17 has a cylindrical shape having a central axis parallel to the z direction. The front-side environment communication passage 17 opens on the upper surface on the upstream side in the z direction of the front-side member 10 and communicates with the recess 12. That is, the front-side environment communication passage 17 penetrates the front-side member 10 in the z direction.

  The back side member 20 further includes a back side environment communication passage 27. The back side environment communication passage 27 has a cylindrical shape having a central axis parallel to the z direction. The back-side environment communication passage 27 is open on the surface on the downstream side in the z direction of the main body portion 21 of the back-side member 20 and the top surface of the convex portion 22. That is, the back-side environment communication passage 27 penetrates the back-side member 20 in the z direction.

  FIG. 2 is a cross-sectional view taken along the line II-II in FIG. FIG. 2 shows the vicinity of the sample 99 in an enlarged manner.

  The sample holding device 1 is arranged so that the beam is incident from the upstream side in the y direction. Here, of the front and back surfaces of the sample 99, the surface on which the beam is incident is referred to as the front (front) surface, and the other surface is referred to as the back surface. The terms “front surface” and “rear surface” are for convenience and do not limit the arrangement method of the sample 99.

  As shown in FIG. 2, the front side member 10 includes a front side environmental chamber 18 formed so as to be in contact with the surface of the sample 99. The back-side member 20 includes a back-side environment chamber 28 formed so as to be in contact with the back surface of the sample 99.

  The front environment communication passage 17 communicates with the front environment chamber 18. Similarly, the back-side environment communication passage 27 communicates with the back-side environment chamber 28.

  The schematic configuration of the sample holding device 1 has been described above. The holder H1 can be manufactured by a known processing method such as machining that cuts a material such as resin, or injection molding that fills a mold with a material such as resin. Further, well-known O-rings 31 and 32 and polymer films 33 and 34 can be used.

[Sample Analysis Method and Effects of First Embodiment]
Next, a sample analysis method using the sample holding device 1 will be described. In the sample analysis method, the front side environment in contact with the surface of the sample 99 and the back side environment in contact with the back side of the sample 99 are separated to hold the sample 99, and the beam incident on the sample 99 and the beam emitted from the sample 99 are emitted. A step of observing.

  First, the sample 99 is held by the holder H1 of the sample holding device 1. Specifically, the sample 99 is disposed between the concave portion 12 and the convex portion 22. Since the front side member 10 and the back side member 20 are configured to be detachable, the sample 99 can be easily replaced.

  As will be described later, by holding the sample 99 by the holder H <b> 1 of the sample holding device 1, the front side environment in contact with the surface of the sample 99 and the back side environment in contact with the back surface of the sample 99 can be separated.

  The beam incident on the sample 99 includes, for example, electromagnetic waves such as γ rays, X rays, ultraviolet rays, visible rays, infrared rays, terahertz waves, microwaves, and millimeter waves, and electron beams, neutron rays, α rays, heavy particle rays, And particle beams such as ion beams. The beam may be monochromatic or have a wide energy distribution.

  The beam emitted from the sample 99 is, for example, a beam diffracted or scattered by the sample 99 or a beam transmitted through the sample 99. The beam emitted from the sample 99 includes a beam partially absorbed by the sample 99 or emitted from the sample 99. In addition, the energy distribution of the beam emitted from the sample 99 may be different from the energy distribution of the incident beam.

  Observing the beam emitted from the sample 99 is, for example, observing an angle change or intensity change due to diffraction or scattering, an intensity change due to absorption or radiation, or a change in energy distribution due to interaction. Typical examples of such observation (measurement) are X-ray diffraction and X-ray scattering, neutron diffraction and neutron scattering, infrared absorption, ultraviolet-visible absorption spectrum, circular dichroism, Raman spectrum, electron spin resonance, nucleus Examples include magnetic resonance as well as fluorescence analysis.

  Referring to FIG. 2, the beam enters the sample 99 from the beam entrance 16. The beam diffracted or scattered by the sample 99, the beam transmitted through the sample 99, or the beam emitted from the sample 99 is emitted to the beam exit 26.

  As described above, the beam exit port 26 has a conical shape having a central axis parallel to the y direction and increasing in diameter toward the downstream in the y direction. Accordingly, the beam diffracted or scattered by the sample 99 or the beam emitted from the sample 99 can be emitted to the outside of the sample holding device 1. Of course, when observing a beam emitted parallel to the y direction, the beam emission port 26 may be cylindrical. The beam entrance 16 may be conical. If the beam entrance 16 is conical, the beam can be incident obliquely.

  The front side member 10 and the back side member 20 include a front side environment chamber 18 and a back side environment chamber 28. The front-side environment chamber 18 is in contact with the surface of the sample 99, and the back-side environment chamber 28 is in contact with the back surface of the sample 99. With this configuration, the sample holding device 1 can separate the environment in which the surface of the sample 99 is in contact with the environment in which the back surface of the sample 99 is in contact. Then, the environment in which the front and back surfaces of the sample 99 are in contact with each other can be separated, and measurement by beam irradiation can be performed.

  Here, “environment” is, for example, a medium (including solid, liquid, and gas), temperature, humidity, pressure, electric field, and magnetic field.

  O-rings 31 and 32 seal the boundary between the holder H1 and the sample 99. Thereby, the front-side environment chamber 18 and the back-side environment chamber 28 are effectively separated. Specifically, fluids (gas, liquid, etc.) in the front environment chamber 18 and the back environment chamber 28 do not circulate with each other by the O-rings 31 and 32.

  The front member 10 includes a front environment communication passage 17 that communicates with the front environment chamber 18. The back side member 20 includes a back side environment communication passage 27 that communicates with the back side environment chamber 28. Through the front-side environment communication passage 17, the environment of the front-side environment chamber 18 can be measured and controlled. Similarly, the environment of the front-side environment chamber 28 can be measured and controlled through the back-side environment communication passage 27. Then, observation by beam irradiation can be performed by measuring or controlling the front and back environment.

  The sample analysis method and the effects of the first embodiment have been described above. In the present embodiment, the concave portion 12 and the convex portion 22 are formed so that the sample 99 is arranged with an inclination of about 45 ° with respect to the incident beam. However, the angle at which the sample 99 is inclined is arbitrary. The concave portion 12 and the convex portion 22 are arbitrarily designed according to experimental conditions.

  In this embodiment, O-rings 31 and 32 are arranged on both sides of the sample 99 to seal the boundary between the holder H1 and the sample 99. However, this configuration is not essential. For example, consider the case of conducting an experiment in which a liquid is brought into contact with the surface of the sample 99. In this case, it is sufficient that the liquid filled in the front-side environment chamber 18 does not leak into at least the back-side environment chamber 28. Depending on the experimental conditions such as the viscosity of the liquid to be filled, one or both of the O-rings 31 and 32 may be unnecessary.

  In the present embodiment, the front side environmental chamber 18 is formed on the front side member 10, and the back side environmental chamber 28 is formed on the back side member 20. Further, the beam entrance 16 is formed in the front member 10, and the beam exit 26 is formed in the back member 20. However, the front side environment chamber 18, the back side environment chamber 28, the beam incident port 16, and the beam emission port 26 are arbitrarily formed. For example, the beam emitting port 26 may be formed in the front side member 10 and the beam incident port 16 may be formed in the back side member 20.

[Second Embodiment]
FIG. 3 is an exploded perspective view showing a schematic configuration of the sample holding device 2 according to the second embodiment of the present invention. Unlike the first embodiment, the sample holding device 2 includes a holder H2 and a control member 60 for controlling the temperature of the sample 99.

  The holder H <b> 2 includes a front side member 40 and a back side member 50. The front side member 40 and the back side member 50 have substantially the same configurations as the front side member 10 and the back side member 20 in the first embodiment. However, the front side member 40 further includes a guide groove 41 for arranging the control member 60 in addition to the configuration of the front side member 10. In addition to the configuration of the back side member 20, the back side member 50 further includes a guide groove 51 for arranging the control member 60 and screw holes 52 and 53 for fixing the control member 60.

  The control member 60 includes a frame-shaped part 61 and an inclined part 62. The frame-shaped part 61 is plate-shaped and has a shape in which the center is opened in a rectangular shape. The inclined portion 62 has a plate shape and is formed continuously on one side of the opening of the frame-shaped portion 61. As shown in FIG. 3, when the frame-like portion 61 is arranged perpendicular to the y direction, the inclined portion 62 is formed so as to be substantially parallel to the inclined surface of the concave portion 12 and the inclined surface of the convex portion 22.

  The frame-like portion 61 of the control member 60 includes through holes 63 and 64. The through holes 63 and 64 are formed so as to be coaxial with the screw holes 52 and 53 of the back side member 50 when the control member 60 is disposed in the guide groove 51 of the back side member 50. Therefore, the control member 60 can be fixed to the back side member 50 with a screw (not shown).

  The inclined portion 62 of the control member 60 includes a beam passage port 65.

  The material of the control member 60 is, for example, aluminum, copper, or iron. The control member 60 can be manufactured as follows, for example. First, through holes 63 and 64 and a beam passage hole 65 are formed in an aluminum flat plate. Subsequently, slits are formed on three sides of the rectangular shape that is slightly smaller than the flat plate, and the inclined portions 62 are formed by bending the slits. By forming the inclined portion 62, the remaining portion becomes the frame-shaped portion 61.

  4 is a cross-sectional view taken along line IV-IV in FIG. FIG. 4 shows an enlarged view of the vicinity of the sample 99.

  The front side member 40 and the back side member 50 include the front side environment chamber 18 and the back side environment chamber 28, similarly to the front side member 10 and the back side member 20. The front environment chamber 18 is in contact with the surface of the sample 99. The back environment chamber 28 is in contact with the back surface of the sample 99. Note that the back-side environment chamber 28 is in contact with the back surface of the sample 99 via the beam passage port 65 formed in the inclined portion 62 of the control member 60.

[Sample Analysis Method and Effects of Second Embodiment]
Next, a sample analysis method using the sample holding device 2 will be described. The sample analysis method using the sample holding device 2 is substantially the same as the sample analysis method using the sample holding device 1.

  First, the sample 99 is held by the holder H2 of the sample holding device 2. As shown in FIGS. 3 and 4, the control member 60 is disposed between the back side member 50 and the sample 99. The control member 60 may be disposed between the front side member 40 and the sample 99.

  The control member 60 is disposed in contact with the sample 99. Specifically, the inclined portion 62 of the control unit 60 is disposed so as to contact the sample 99. The control member 60 and the sample 99 are preferably arranged in close contact with each other. In order to arrange the control member 60 and the sample 99 in close contact with each other, grease or the like may be applied to the inclined portion 62.

  O-rings 31 and 32 are arranged between the front side member 40 and the sample 99 and between the back side member 50 and the sample 99. Thereby, the boundary between the holder H2 and the sample 99 is sealed. However, as in the first embodiment, this configuration is not essential.

  Referring to FIG. 4, the beam enters the sample 99 from the beam entrance 16. The beam diffracted or scattered by the sample 99, the beam transmitted through the sample 99, or the beam emitted from the sample 99 is emitted to the beam exit 26 through the beam passage hole 65 of the inclined portion 62.

  The sample holding device 2 can also separate the environment where the front and back surfaces of the sample 99 are in contact with each other by the front environment chamber 18 and the back environment chamber 28. Then, the environment in which the front and back surfaces of the sample 99 are in contact with each other can be separated, and measurement by beam irradiation can be performed. Further, the front and back environment communication passages 17 and the back side environment communication passage 27 can measure or control the front and back environments.

  In the sample holding device 2, the experimental condition of the sample 99 can be further controlled by the control member 60. The control member 60 is disposed in contact with the sample 99. Therefore, the experimental conditions of the sample 99 can be controlled quickly.

  FIG. 5 is a schematic diagram illustrating an example of control of experimental conditions by the control member 60. In the example shown in FIG. 5, a Peltier element 91 and a heat sink 92 for releasing heat of the Peltier element 91 are attached to the frame-shaped portion 61 of the control member 60. A thermocouple 93 is attached to a portion of the inclined portion 62 close to the sample 99.

  According to this configuration, the temperature of the sample 99 can be controlled by the Peltier element 91. Further, the temperature of the sample 99 can be measured by the thermocouple 93.

  In this case, the holder H2 is preferably made of a material having low thermal conductivity. As a result, when the sample 99 is cooled, the amount of heat inflow per unit time from the holder H2 is reduced, so that the sample 99 can be further cooled. When the sample 99 is heated, the amount of heat flowing out to the holder H2 per unit time is reduced, so that the sample 99 can be further heated. In any case, the temperature of the sample 99 can be made uniform throughout.

  On the other hand, the control member 60 is preferably formed of a material having high thermal conductivity. As a result, the amount of heat flowing out to the control member 60 per unit time or the amount of heat flowing in from the control member 60 per unit time increases. Therefore, the temperature of the sample 99 can be quickly controlled. Moreover, the temperature of the control part 60 can be made uniform throughout. Thus, the temperature of the sample 99 that is in contact with the control member 60 can also be made uniform throughout. Further, when the temperature of the control member 60 and the temperature of the sample 99 approach each other, the thermocouple 93 can measure the accurate temperature of the sample 99.

  That is, it is preferable that the control member 60 has a thermal conductivity higher than that of the holder H2. Thereby, the temperature of the sample 99 can be quickly controlled.

  In the present embodiment, the control member 60 includes a frame-shaped portion 61 and an inclined portion 62. This configuration is exemplary. For example, the control member 60 may have a shape obtained by bending a flat plate by 45 °.

[Third Embodiment]
FIG. 6 is an exploded perspective view showing a schematic configuration of the sample holding device 3 according to the third embodiment of the present invention. Unlike the first embodiment, the sample holding device 3 includes control members 70A and 70B.

  The control members 70A and 70B are made of, for example, aluminum, copper, or iron. The control members 70A and 70B have a plate shape and include a beam passage port 71 at the center.

  Control members 70A and 70B are arranged in contact with sample 99. Specifically, the control member 70 </ b> A contacts the surface of the sample 99 and is disposed between the sample 99 and the front side member 10. The control member 70 </ b> B is disposed between the sample 99 and the back member 20 in contact with the back surface of the sample 99.

  O-rings 31 and 32 are arranged between the front side member 10 and the control member 70A and between the back side member 20 and the control member 70B. Thereby, the boundary between the holder H1 and the sample 99 is sealed. However, as in the first embodiment, this configuration is not essential.

[Effect of the third embodiment]
In the sample holding device 3, the control members 70 </ b> A and 70 </ b> B are arranged in contact with both surfaces of the sample 99. An electric field can be applied to the sample 99 by the control members 70A and 70B. For example, by connecting the control member 70A to the potential V1 and the control member 70B to the potential V2, an electric field can be applied in a direction intersecting the surface of the sample 99. Alternatively, a current can be passed in a direction that intersects the surface of the sample 99. The potentials V1 and V2 may be constant potentials, AC potentials, or pulses.

  In this case, the holder H1 is preferably formed of a material having high electrical resistance. Thereby, when an electric field is applied to the sample 99, the current leaking to the holder H1 can be reduced. The holder H1 is more preferably an insulator.

  On the other hand, the control members 70A and 70B are preferably formed of a material having low electrical resistance. Thereby, the entire potential of the control member 70A and the entire potential of the control member 70B can be made uniform. Therefore, a uniform electric field can be applied to the sample 99. Alternatively, a uniform current can be passed through the sample 99.

  That is, it is preferable that the control members 70A and 70B have an electrical resistance lower than that of the holder H1. Thereby, a uniform electric field can be applied to the sample 99. Alternatively, a uniform current can be passed through the sample 99.

[Fourth Embodiment]
FIG. 7 is an exploded perspective view showing a schematic configuration of the sample holding device 4 according to the fourth embodiment of the present invention. Unlike the first embodiment, the sample holding device 4 includes a control member 80.

  The control member 80 has a plate shape and includes a beam passage port 81 at the center. The control member 80 includes conductive portions 82 and 83 and an insulating portion 84. The insulating part 84 is formed between the conductive parts 82 and 83 and insulates the conductive parts 82 and 83. The conductive portions 82 and 83 are made of aluminum, for example. The insulating part 84 is made of, for example, epoxy resin or polyethylene.

  The control member 80 is disposed in contact with the sample 99. As shown in FIG. 7, the control member 80 is disposed between the sample 99 and the back member 20 in contact with the back surface of the sample 99. The control member 80 may be disposed between the sample 99 and the front side member 10 in contact with the surface of the sample 99.

  O-rings 31 and 32 are disposed between the front side member 10 and the sample 99 and between the back side member 20 and the control member 80. Thereby, the boundary between the holder H1 and the sample 99 is sealed. However, as in the first embodiment, this configuration is not essential.

[Effect of the fourth embodiment]
In the sample holding device 4, the control member 80 is disposed in contact with the sample 99. An electric field can be applied to the sample 99 by the control member 80. For example, the electric field can be applied in the in-plane direction of the sample 99 by connecting the conductive portion 82 of the control member 80 to the potential V1 and the conductive portion 83 to the potential V2. Alternatively, a current can be passed in the in-plane direction of the sample 99.

  Similar to the third embodiment, the holder H1 is preferably formed of a material having high electrical resistance. Conductive portions 82 and 83 are preferably formed of a material with low electrical resistance. That is, it is preferable that the conductive parts 82 and 83 have an electrical resistance lower than that of the holder H1. Thereby, a uniform electric field can be applied to the sample 99. Alternatively, a uniform current can be passed through the sample 99.

  A magnetic field can also be applied to the sample 99 using a configuration in which the sample holding device 4 is deformed. For example, the magnetic field can be applied in the in-plane direction of the sample 99 by arranging the S pole instead of the conductive part 82 and the N pole instead of the conductive part 83.

[Fifth Embodiment]
FIG. 8 is an exploded perspective view showing a schematic configuration of the sample holding device 5 according to the fifth embodiment of the present invention. Unlike the first embodiment, the sample holding device 5 includes control members 80A and 80B.

  The control members 80A and 80B have the same configuration as the control member 80.

  Control members 80A and 80B are arranged in contact with sample 99. Specifically, the control member 80 </ b> A contacts the surface of the sample 99 and is arranged between the sample 99 and the front side member 10. The control member 80B is disposed between the sample 99 and the back side member 20 in contact with the back surface of the sample 99.

  O-rings 31 and 32 are arranged between the front side member 10 and the control member 80A and between the back side member 20 and the control member 80B. Thereby, the boundary between the holder H1 and the sample 99 is sealed. However, as in the first embodiment, this configuration is not essential.

[Effect of Fifth Embodiment]
In the sample holding device 5, the control members 80 </ b> A and 80 </ b> B are arranged in contact with both surfaces of the sample 99. An electric field can be applied to the sample 99 by the control members 80A and 80B. For example, the conductive portion 82 of the control member 80A is connected to the potential V1, and the conductive portion 83 is connected to the potential V2. Further, the conductive portion 82 of the control member 80B is connected to the potential V3, and the conductive portion 83 is connected to the potential V4. Thereby, an electric field can be applied in the direction intersecting the surface of the sample 99 and in the in-plane direction. Alternatively, a current can be passed in the direction intersecting the surface of the sample 99 and in the in-plane direction. Some of the potentials V1 to V4 may be equal.

  Similar to the third embodiment, the conductive portions 82 and 83 of the control members 80A and 80B preferably have an electrical resistance lower than the electrical resistance of the holder H1. Thereby, a uniform electric field can be applied to the sample 99. Alternatively, a uniform current can be passed through the sample 99.

  A magnetic field can also be applied to the sample 99 using a configuration in which the sample holding device 5 is deformed. For example, instead of the conductive portions 82 and 83 of the control members 80A and 80B, by arranging the S pole and the N pole, respectively, a magnetic field can be applied in the direction intersecting the surface of the sample 99 and in the in-plane direction. it can.

  A magnetic field can also be applied to the sample 99 by winding a coil around the entire sample holding device 1-5.

  In the above description, the example in which the temperature of the sample 99 and the electric and magnetic fields applied to the sample 99 are controlled using the control members 60, 70A, 70B, 80, 80A, and 80B has been described. In addition to this, the control member can be configured to control a mechanical external force such as applying tension to the sample 99.

[Specific example of sample analysis method]
A specific example of the sample analysis method using the sample holding devices 1 to 5 will be described. The sample analysis method according to the present invention is not limited to the following specific examples. 9 to 11 are diagrams for explaining an example of the sample analysis method, and are schematic cross-sectional views of the sample holding device 2. In these drawings, a case where measurement is performed using the sample holding device 2 is illustrated. However, the same applies to the measurement using the sample holding device 1 and the sample holding devices 3 to 5.

  In the example shown in FIG. 9, the back side of the sample 99, specifically, the beam emission port 26, the back side environment communication passage 27, and the back side environment chamber 28 are filled with water W. A closed transpiration meter 94 is disposed at the opening of the front-side environment communication passage 17. In this example, the amount of moisture transpiration of the sample 99 can be measured by the closed type transpiration meter 94. The beam incident port 16 and the beam exit port 26 can perform measurement by beam irradiation in parallel with the measurement of the moisture transpiration amount.

  Note that the surface side of the sample 99 may be filled with water W, and the closed-type transpiration meter 94 may be disposed at the opening of the back-side environment communication passage 27.

  In the example shown in FIG. 10, the back side of the sample 99 is filled with water W as in the example shown in FIG. 9. On the other hand, an open transpiration meter 95 is disposed at the opening of the front-side environment communication passage 17. A second environment communication passage 19 is added to the front member 40 so as to communicate with the front environment chamber 18. In the example shown in FIG. 10, dry nitrogen is blown from the second environment communication passage 19. Alternatively, the second environment communication passage 19 may not be added, and an air supply pipe may be inserted into the front side environment communication passage 17 and dry nitrogen may be blown from there. Thereby, the open transpiration meter 95 measures the moisture transpiration amount of the sample 99. The beam incident port 16 and the beam exit port 26 can perform measurement by beam irradiation in parallel with the measurement of the moisture transpiration amount.

  Also in the example shown in FIG. 10, the surface side of the sample 99 may be filled with water W, and the open transpiration meter 95 may be disposed at the opening of the back side environment communication passage 27. In this case, dry nitrogen is blown from a second environment communication passage (not shown) provided in the back side member 50 or an air supply pipe inserted into the back side environment communication passage 27.

  In the example shown in FIG. 11, the surface side of the sample 99, specifically, the beam incident port 16, the front-side environment communication passage 17, and the front-side environment chamber 18 are filled with water W. An ultrasonic element 96 is disposed in the opening of the front environment communication passage 17. With the ultrasonic element 96, the surface of the sample 99 can be exposed to ultrasonic waves. The beam entrance 16 and the beam exit 26 can perform measurement by beam irradiation in parallel with ultrasonic exposure.

  Note that the back side of the sample 99 may be filled with water W, and the ultrasonic element 96 may be disposed in the opening of the back side environment communication passage 27.

  Particularly suitable samples for the present invention are, for example, biological thin film samples or polymer sheets, or solids or liquids applied to them. The biofilm sample is, for example, mammalian or avian skin, reptiles, amphibians, or fish scales, or plant skins. The polymer sheet is, for example, cellophane tape or wrap. The solid or liquid applied to these is, for example, a cosmetic or formulation applied on the skin, or a coating applied to the substrate.

[Structural analysis of stratum corneum]
An important function of the skin stratum corneum is to isolate the living body from the outside world and maintain the homeostasis of the living body. This function is called the skin barrier function. In rough skin, dry skin, atopic dermatitis and the like, the barrier function is lowered. Therefore, in order to improve the symptoms, it is necessary to supplement the barrier function by applying medicines and cosmetics from the outside. On the other hand, the skin barrier function is a great barrier when it is desired to penetrate a transdermal drug or cosmetic into the body. In recent years, it has been found that when the skin stratum corneum is irradiated with synchrotron radiation, a scattering peak thought to be derived from cellular lipids is observed. Based on this information, attempts have been made to elucidate the stratum corneum structure that plays an important role in the barrier function, and to analyze the interaction between various preparations and the stratum corneum. ADVANTAGE OF THE INVENTION According to this invention, the structural change of a stratum corneum when living body skin is exposed to various solutions can be analyzed in real time.

[Analysis of stratum corneum structure change during percutaneous penetration of pharmaceuticals and cosmetics]
A transdermal drug or cosmetic applied on the skin permeates through the stratum corneum while interacting with the stratum corneum. The stratum corneum originally functions as a defense wall against the invasion of foreign substances, but it can be efficiently penetrated into the body by devising the structure of the preparation and actively interacting with the stratum corneum. By using this sample holding device, it becomes possible to analyze the structural change of the stratum corneum that occurs in the percutaneous absorption process, and also the temperature characteristics thereof, which can be useful for the development of a high-absorption type preparation. It is also speculated that cosmetics form new structures on the skin surface when applied to the skin. According to the present invention, it is also possible to observe in real time the structural change of a cosmetic or formulation itself applied to the skin.

[Iontophoresis or electroporation]
The sample holding device according to the present invention holds a sample in a sheet form. Therefore, an electrode or the like can be arranged on the surface of the sample. As a result, structural changes that occur during ion introduction or electroporation can be analyzed.

[Application to the field of tribology]
In a high-density hard disk, the disk and the head must be brought close to each other. Therefore, lubrication between the disk and the head is an important issue. Therefore, a carbon film or a lubricating oil film is applied to the disk surface to suppress wear of the disk and head. In order to perform surface treatment with high performance, structural analysis of the surface is necessary. According to the present invention, the structure analysis of the substance applied to the substrate surface can be performed.

[Development of polymer film]
ADVANTAGE OF THE INVENTION According to this invention, the dynamic structural analysis of the structural change which arises at the time of chemical resistance evaluation or chemical exposure of a polymer film can be performed.

  As mentioned above, although embodiment about this invention was described, this invention is not limited only to each above-mentioned embodiment, A various change is possible within the scope of the invention. Moreover, each embodiment can be implemented in combination as appropriate.

  Hereinafter, the present invention will be specifically described based on examples. In addition, this Example does not limit this invention.

  Using the sample holding device 2 according to the second embodiment, the correlation between the transdermal water loss (TEWL) of the stratum corneum collected from human and mouse skin and the order of lipid molecules was investigated. .

  The measurement was performed in the arrangement shown in FIG. The back side of the sample 99 (corner layer), specifically, the beam exit port 26, the back side environment communication passage 27, and the back side environment chamber 28 were filled with water W. Then, a closed transpiration meter 94 was placed in the opening of the front-side environment communication passage 17 and the TEWL of the sample 99 was measured. In parallel with the TEWL measurement, synchrotron radiation X-rays monochromatized from the beam incident light 16 were incident on the sample 99, and the diffracted light emitted from the beam exit 26 was observed. These measurements were performed by changing the temperature of the sample 99 to 20 to 70 ° C.

  The results are shown in FIGS. FIG. 12 and FIG. 13 are graphs in which the horizontal axis indicates the temperature (° C.) of the sample 99 and the vertical axis indicates the integrated intensity (arbitrary unit) and TEWL (arbitrary unit) of the diffracted X-ray near the surface interval of 0.41 nm. is there. FIG. 12 shows the measurement results of the human stratum corneum, and FIG. 13 shows the measurement results of the mouse stratum corneum. As shown in FIGS. 12 and 13, there was a correlation between TEWL and lipid molecule ordering in both the human and mouse stratum corneum.

  According to the present invention, the environment of the front and back surfaces of the sample can be separated and measurement by beam irradiation becomes possible. As a result, the correlation between TEWL and the order of lipid molecules was clarified.

  The present invention can be industrially used as a sample holding device and a sample analysis method.

1 to 5 Sample holding device H1, H2 Holder 10, 40 Front side member 12 Recess 13 Groove 14, 15 Through hole 16 Beam entrance 17 Front side environment communication passage 18 Front side environment chamber 20, 50 Back side member 21 Main body part 22 Projection part 23 Groove 24, 25 Through hole 26 Beam exit port 27 Back side environment communication passage 28 Back side environment chamber 31, 32 O-ring 33, 34 Polymer film 60, 70, 80 Control member 99 Sample

Claims (10)

A holder for holding the sample;
The holder is
A front-side environment chamber formed so as to be in contact with the surface of the sample;
A back environmental chamber formed so as to be in contact with the back surface of the sample;
A beam entrance for allowing a beam to enter the sample;
A sample holding device including a beam exit for emitting a beam from the sample. The sample holding device according to claim 1,
A sample holding device in which a boundary between the holder and the sample is sealed. The sample holding device according to claim 1 or 2,
The holder further includes
A sample holding device including an environment communication passage that leads to one of the front-side environment chamber and the back-side environment chamber and opens to the outside. The sample holding device according to any one of claims 1 to 3,
The holder further includes
A front member disposed on the front side of the sample;
A back side member disposed on the back side of the sample and detachable from the front side member;
The front-side environment chamber is formed in the front-side member, the back-side environment chamber is formed in the back-side member, and one of the beam incident port and the beam emission port is formed in the front-side member, and the beam incident port And the other of the beam exit ports is formed in the back member. The sample holding device according to any one of claims 1 to 4, further comprising:
A sample holding device provided with a control member arranged in contact with the sample and controlling an experimental condition of the sample. The sample holding device according to claim 5,
The sample holding device, wherein the control member has a thermal conductivity higher than that of the holder. The sample holding device according to claim 5,
The sample holding device, wherein the control member has an electrical resistance lower than that of the holder. Separating the front-side environment in contact with the surface of the sample and the back-side environment in contact with the back surface of the sample, and holding the sample;
And a step of observing the beam emitted from the sample and entering the sample. The sample analysis method according to claim 8, further comprising:
A sample analysis method comprising a step of measuring at least one of the front side environment and the back side environment. The sample analysis method according to claim 8 or 9, further comprising:
A sample analysis method comprising a step of controlling at least one of the front side environment and the back side environment.

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