Normal reflection measurement device and sample holder for normal reflection measurement device

Abstract

To provide a regular reflection measurement device that can cause a sample holder to hold a sheet-like member having flexibility without loosening, and thereby can accurately perform a regular reflection measurement with excellent reproducibility.SOLUTION: A regular reflection measurement device according to the present invention performs a regular reflection measurement to a sheet-like member having flexibility, and comprises: a sample holder (20;40) that has an external cylinder (21;41) and an inner cylinder (22;42) to be internally inserted into the external cylinder with prescribed gaps; an irradiation optical system (123;30, 331 and 343) that irradiates the sheet-like member covering one end 221 of the inner cylinder to be internally inserted into the external cylinder with measurement light; and a detector (14;35) that is arranged at a position where the measurement light to be regularly reflected by the sheet-like member covering the one end of the inner cylinder to be internally inserted into the external cylinder is incident.SELECTED DRAWING: Figure 1

Description

Technical Field

[0001] The present invention relates to a specular reflection measurement apparatus and a sample holder for a specular reflection measurement apparatus.

Background Art

[0002] Conventionally, the reflectance, gloss, haze, color tone, thickness, etc. of light in films such as polymer films have been determined by specular reflection measurement using a spectrophotometer. Generally, in specular reflection measurement, light is incident on a sample having a smooth surface at a predetermined incident angle (for example, about 10° with respect to the normal of the surface), and the light reflected from the surface (specularly reflected light) is detected. Patent Document 1 describes obtaining the reflectance and three parameters (L * value, a * value, and b * value) in the CIELAB color space based on the spectrum of the specularly reflected light from the film. Here, the CIELAB color space refers to a color space defined by the above three parameters for colors, formulated by the International Commission on Illumination (CIE: Commission internationale de l'eclairage (French)).

Prior Art Documents

Patent Documents

[0003]

Patent Document 1

Summary of the Invention

Problems to be Solved by the Invention

[0004] When there is slack in the film during specular reflection measurement, the specularly reflected light does not reflect in the original direction, and the specularly reflected light cannot be detected. In particular, when performing specular reflection measurement on a thin and flexible film with an ultraviolet-visible spectrophotometer, it is difficult to fix the measurement surface flat. Therefore, the shape of the measurement surface varies for each measurement, resulting in poor reproducibility and inability to perform accurate measurement. For this reason, it is necessary to hold the film in the sample holder without slack. Conventionally, cellophane tape or the like has been used to fix the film to the sample holder, but this requires time and effort in the work, and if the operator is not accustomed to it, the film may be fixed in a slack state.

[0005] So far, the film such as a polymer film has been described as an example, but the same problem occurs when performing specular reflection measurement on other flexible sheet-like members such as a sheet made of metal fibers.

[0006] The problem to be solved by the present invention is to provide a specular reflection measurement device and a sample holder for a specular reflection measurement device that can hold a flexible sheet-like member without slack, thereby enabling accurate specular reflection measurement with good reproducibility.

Means for Solving the Problem

[0007] The specular reflection measurement device according to the present invention made to solve the above problems is for performing specular reflection measurement on a flexible sheet-like member, and a sample chamber surrounded by a wall and having an opening in the wall, a cylindrical sample holder insertion part fixed to the periphery of the opening, a sample holder inserted into the sample holder insertion part with a predetermined gap and having a mark on its side surface, an irradiation optical system provided at a position for irradiating measurement light to the sheet-like member, which is the measurement target sample, covering one end of the sample holder inserted into the sample holder insertion part up to the mark, a detector provided at a position in the sample chamber where the measurement light specularly reflected by the sheet-like member covering one end of the sample holder inserted up to the mark is incident and includes .

[0008] According to the present invention In other aspects Regular reflection measurement device The position is , With respect to a flexible sheet-like member Performs regular reflection measurement Also and A sample chamber surrounded by a wall and having an opening in the wall, Fixed to the periphery of the opening cylinder A sample holder insertion part in the shape of and the above-mentioned Sample holder insertion part with a predetermined gap Insert is formed Cylindrical part and The cylindrical part a protruding portion protruding from the outer surface of the above A sample holder having An irradiation optical system provided at a position where measurement light is irradiated onto the sheet-like member, which is a measurement target sample, covering one end of the cylindrical part inserted into the sample holder insertion part up to a position where the protruding part abuts against one end of the sample holder insertion part; A detector provided at a position where the measurement light specularly reflected by the sheet-like member covering one end of the cylindrical part inserted into the sample chamber up to a position where the protruding part abuts against one end of the sample holder insertion part enters Comprising .

[0009] The predetermined gap is set to a gap that can sandwich the sheet-like member.

Effects of the Invention

[0010] According to the present invention, while covering one end of the inner cylinder with a sheet-like member, the inner cylinder is inserted into the outer cylinder from the one end side, and a part of the sheet-like member is sandwiched between the inner surface of the outer cylinder and the outer surface of the inner cylinder, whereby the flexible sheet-like member can be held in the sample holder without slack, and thereby regular reflection measurement can be accurately performed with good reproducibility.

Brief Description of the Drawings

[0011]

Figure 1

Figure 2

Figure 3

Figure 4

Figure 5

Embodiments for Carrying Out the Invention

[0012] Embodiments of the specular reflection measurement device and the sample holder for the specular reflection measurement device according to the present invention will be described with reference to FIGS. 1 to 5.

[0013] (1) First Embodiment First, as the first embodiment of the present invention, an ultraviolet-visible spectrophotometer 1 which is a specular reflection measurement device, and a sample holder 20 included in the ultraviolet-visible spectrophotometer 1 will be described.

[0014] (1-1) Configuration of the Ultraviolet-Visible Spectrophotometer 1 and the Sample Holder 20 in the First Embodiment In the ultraviolet-visible spectrophotometer 1 of the first embodiment, as shown in FIG. 1, a light source 11, a sample chamber 12, a diffraction grating 13, and a detector 14 are housed in a housing 15.

[0015] The light source 11 is a light source that emits light including wavelengths in the region from the ultraviolet region to the visible region. The light emitted by the light source 11 may include wavelengths in the near-infrared region in addition to the ultraviolet region and the visible region.

[0016] An irradiation light window 121 and a detection light window 122 are provided on the wall of the sample chamber 12. These windows are arranged at positions where the irradiation light emitted from the light source 11 enters the irradiation light window 121, and the light (measurement light specularly reflected by the sample S) emitted from the detection light window 122 enters the diffraction grating 13.

[0017] A part of the wall of the sample chamber 12 is in contact with the inner wall surface of the housing 15. An opening 201 that penetrates the walls of the sample chamber 12 and the housing 15 is provided at the portion where the wall of the sample chamber 12 is in contact with the inner wall surface of the housing 15.

[0018] Inside the sample chamber 12, a part of the sample holder 20, an irradiation light reflecting mirror 123 (corresponding to the irradiation optical system), and a detection light reflecting mirror 124 are accommodated. The irradiation light reflecting mirror 123 is a mirror that reflects the irradiation light introduced into the sample chamber 12 from the irradiation light window 121 so as to be incident on the surface of the sample S held by the sample holder 20 at a predetermined incident angle as described later. The detection light reflecting mirror 124 is a mirror that reflects the reflected light (detection light) specularly reflected from the surface of the sample S so as to introduce it into the detection light window 122.

[0019] The sample holder 20 has an outer cylinder 21 and an inner cylinder 22. In the present embodiment, the outer cylinder 21 is cylindrical, and one end 211 is fixed to the wall of the sample chamber 12 at the periphery of the opening 201. Thereby, the cylinder of the outer cylinder 21 and the opening 201 communicate with each other. The inner cylinder 22 is a cylinder whose outer diameter is slightly (for example, 0.5 mm) smaller than the inner diameter of the outer cylinder 21. Thereby, a gap (for example, 0.25 mm) is formed between the outer cylinder 21 and the inner cylinder 22 such that a sheet-like member is sandwiched therebetween.

[0020] The sample holder 20 of the present embodiment further includes a protruding portion 23 that protrudes outward from a part of the outer surface of the inner cylinder 22. The protruding portion 23 has a donut-shaped disc shape. The protruding portion 23 is provided at a position equidistant from both ends of the inner cylinder 22 (the center in the longitudinal direction). When viewed with reference to the protruding portion 23, the inner cylinder 22 extends by the same length in directions different from each other by 180° from the protruding portion 23.

[0021] The distance between the protruding portion 23 and one end 221 of the inner cylinder 22 is set such that when the inner cylinder 22 is inserted into the outer cylinder 21 until the protruding portion 23 abuts against one end 211 of the outer cylinder 21, one end 221 of the inner cylinder 22 reaches a position where the irradiation light reflected by the irradiation light reflecting mirror 123 is incident on the surface of the sample S. Further, in the present embodiment, the distance between the protruding portion 23 and the other end 222 of the inner cylinder 22 is made the same as the distance between the protruding portion 23 and one end 221 of the inner cylinder 22. Thereby, no matter which side of the one end 221 side or the other end 222 side of the inner cylinder 22 , protruding is inserted until the protruding portion 23 abuts against one end 211 of the outer cylinder 21, one end 221 or the other end 222 of the inner cylinder 22 reaches the same position.

[0022] The diffraction grating 13 is an optical element that separates the detection light reflected by the sample S for each wavelength. The detector 14 detects the light for each wavelength separated by the diffraction grating 13 and measures the intensity of the light for each of those wavelengths.

[0023] (1-2) Method of using and operation of the ultraviolet-visible spectrophotometer 1 and the sample holder 20 according to the first embodiment First, a sample S, which is a flexible sheet-like member, is attached to the sample holder 20 by the following method. First, the sample S is placed over the opening 2210 at one end 221 of the inner cylinder 22. In this embodiment, the protruding portion 23 is provided at a position equidistant from both ends of the inner cylinder 22, and since the inner cylinder 22 extends from the protruding portion 23 in both sides in directions that are 180° different from each other, the sample S may be placed over either end on those two sides. In this state, the inner cylinder 22 is inserted into the outer cylinder 21 from the end on the side where the sample S is placed until the protruding portion 23 abuts against one end 211 of the outer cylinder 21 (FIG. 2).

[0024] By inserting the inner cylinder 22 until the protruding portion 23 abuts against one end 211 of the outer cylinder 21 in this way, the end of the inner cylinder 22 on the side where the sample S is placed reaches the position where the irradiation light irradiated from the irradiation optical system (irradiation light reflecting mirror 123) is incident on the surface of the sample S. Therefore, the sample S placed over the end is disposed at the incident position of the irradiation light. Further, when the inner cylinder 22 and the sample S are inserted into the outer cylinder 21, the portion of the sample S that contacts the inner surface of the outer cylinder 21 is prevented from moving in the insertion direction due to the friction with the inner surface, while the one end 221 of the inner cylinder 22 moves in the insertion direction, so that the sample S at the portion facing the opening 2210 extends, whereby the sheet-like member can be held in the sample holder 20 without slack.

[0025] In addition, in this embodiment, the distance between the protruding portion 23 and one end 221 of the inner cylinder 22 is set such that when the inner cylinder 22 is inserted into the outer cylinder 21 until the protruding portion 23 abuts against one end 211 of the outer cylinder 21, the one end 221 reaches a position where the irradiation light emitted from the light source 11 and reflected by the irradiation light mirror 123 is incident on the surface of the sample S. Therefore, the position of the sample S can be accurately adjusted to the position where the irradiation light is incident. As a result, specular reflection measurement can be accurately performed with good reproducibility.

[0026] The operation of the measurement by the ultraviolet-visible spectrophotometer 1 is the same as that of the conventional one. Specifically, the light source 11 emits irradiation light, introduces the irradiation light into the sample chamber 12 through the irradiation light window 121, and reflects it with the irradiation light mirror 123, thereby irradiating the surface of the sample S. The reflected light reflected from the surface of the sample S enters the diffraction grating 13 through the detection light mirror 124 and the detection light window 122, and is separated by the diffraction grating 13 for each wavelength. The light for each wavelength separated in this way is detected by the detector 14, and the intensity for each wavelength is obtained. Based on the intensity for each wavelength in the reflected light of the sample thus obtained and the intensity for each wavelength of the light reflected by the reference mirror measured separately, the reflectance for each wavelength in the sample is obtained.

[0027] (1-3) Experiments using the ultraviolet-visible spectrophotometer 1 of this embodiment Next, the experimental results obtained using the ultraviolet-visible spectrophotometer 1 of this embodiment will be described. In this experiment, for nine sheet-like samples of the same type, (a) three samples (samples A1 to A3) fixed to the sample holder 20 of this embodiment, (b) three samples (samples B1 to B3) fixed to the conventional sample holder with cellophane tape, and (c) three samples (samples C1 to C3) placed without being fixed to the conventional sample holder, the reflectance spectra were measured respectively.

[0028] The measurement results are shown in FIG. 3. All of the samples A1 to A3 fixed to the sample holder 20 of the present embodiment were measured to have higher reflectance than when using conventional sample holders (samples B1 to B3, samples C1 to C3). Further, in the present embodiment, there is almost no variation in the measured reflectance values among the three samples A1 to A3, whereas when using a conventional sample holder, variation in the measured values was seen for each sample. These experimental results indicate that, with a conventional sample holder, different-shaped relaxations occur for each sample in a state where the sample is fixed or placed on the sample holder, resulting in a small measured value and variation for each sample, while in the sample holder 20 of the present embodiment, no such relaxation occurs, meaning that the measured value is large and the variation for each sample is small.

[0029] (2) Second Embodiment Next, as a second embodiment of the present invention, a Fourier Transform InfraRed Spectrophotometer (FTIR) 3, which is a normal reflection measurement device, will be described.

[0030] In the FTIR 3 of the present embodiment, as shown in FIG. 4, an interferometer chamber 30, a parabolic mirror 331, a sample chamber 34, an ellipsoidal mirror 332, and an infrared light detector 35 are housed in a housing 37.

[0031] Inside the interferometer chamber 30, a main interferometer composed of an infrared light source 300, a condenser lens 301, a collimator mirror 302, a beam splitter 303, a fixed mirror 304, and a movable mirror 305 is provided. Also, inside the interferometer chamber 30, a control interferometer composed of a laser light source 306, a first laser mirror 307, a second laser mirror 308, a laser detector 309, and the beam splitter 303, the fixed mirror 304, and the movable mirror 305 common to the main interferometer is provided. The main interferometer is for generating main interference light to irradiate the sample, and the control interferometer is for controlling the position of the movable mirror 305. A driver 3051 for moving the movable mirror 305 is connected to the movable mirror 305. Also, on the wall of the interferometer chamber 30, a main interference light window 32, which is a window for passing the main interference light generated by the main interferometer, is provided.

[0032] A part of the wall of the sample chamber 34 is in contact with the inner wall surface of the housing 37. An opening 401 penetrating the walls of the sample chamber 34 and the housing 37 is provided at the portion where the wall of the sample chamber 34 is in contact with the inner wall surface of the housing 37.

[0033] Inside the sample chamber 34, as shown in FIG. 5, a part of a sample holder 40, an in-sample-chamber irradiation optical system 343, and an in-sample-chamber detection optical system 344 are accommodated. The in-sample-chamber irradiation optical system 343 is composed of three plane mirrors, and is an optical system for making the main interference light (irradiation light) introduced into the sample chamber 34 from an irradiation light window 341 incident on the surface of a sample S held by the sample holder 40 at a predetermined incident angle as described later. The in-sample-chamber detection optical system 344 is composed of three plane mirrors, and is an optical system for introducing the reflected light (detection light) specularly reflected from the surface of the sample S into a detection light window 342.

[0034] The sample holder 40 has an outer cylinder 41, an inner cylinder 42, and a protruding portion 43. The configurations of these outer cylinder 41, inner cylinder 42, and protruding portion 43 are the same as those of the outer cylinder 21, inner cylinder 22, and protruding portion 23 in the first embodiment. One end 411 of the outer cylinder 41 is fixed to the wall of the sample chamber 34 at the periphery of the opening 401. The distance between the protruding portion 43 and one end 421 of the inner cylinder 42 is set such that when the inner cylinder 42 is inserted into the outer cylinder 41 until the protruding portion 43 abuts against one end 411 of the outer cylinder 41, one end 421 of the inner cylinder 42 reaches a position where the irradiation light irradiated from the sample chamber irradiation optical system 343 is incident on the surface of the sample S.

[0035] The infrared light detector (corresponding to the detector in the specular reflection measurement apparatus according to the present invention) 35 is arranged at a position where the measurement light specularly reflected by the sample S is reflected by the elliptical mirror 332 and then incident on the infrared light detector 35, and detects the incident measurement light which is infrared light.

[0036] In addition, the FTIR 3 has a control unit 36 that controls each part constituting the main interferometer and the control interferometer, and receives the detection signal obtained by the infrared light detector 35 to perform signal processing.

[0037] The method of mounting the sample S on the sample holder 40 in the second embodiment is the same as the method of mounting the sample S on the sample holder 20 in the first embodiment. Also, the operation of measurement by the FTIR 3 is the same as that of a conventional FTIR. Therefore, detailed descriptions of these methods and operations are omitted.

[0038] (3) Modifications The present invention is not limited to the above embodiments, and various modifications can be made along the gist of the present invention.

[0039] For example, in the above-described embodiment, the inner cylinders 22 and 42 are hollow, but instead, a solid one with a recess provided at one end may be used. By inserting the solid inner cylinder into the outer cylinder with the sheet-like sample covering the recess, the sheet-like sample is held tightly over the recess. However, in order to more surely prevent reflection of light by the inner cylinder, it is preferable that the inner cylinder be hollow.

[0040] In the above-described embodiment, the inner cylinders 22 and 42 are provided so as to extend from the protruding portions 23 and 43 by the same length in directions different from each other by 180°, but they may extend by different lengths. Also, the inner cylinders 22 and 42 may extend only in one direction from the protruding portions 23 and 43. In that case, a gripping portion that a user grasps when setting a sample may be provided on the side without the inner cylinders 22 and 42 as viewed from the protruding portions 23 and 43, or there may be nothing.

[0041] In the above-described embodiment, the protruding portions 23 and 43 are provided on the outer surfaces of the inner cylinders 22 and 42, but the protruding portions 23 and 43 may be omitted. In that case, it is preferable to attach a mark indicating a position that coincides with the position of the outer surface of the housing 15 and 37 when the inner cylinders 22 and 42 are inserted into the outer cylinders 21 and 41 (in other words, the length into which the inner cylinders 22 and 42 should be inserted) on the outer surfaces of the inner cylinders 22 and 42.

[0042] In the above-described embodiment, an ultraviolet-visible spectrophotometer and an FTIR are used as the specular reflection measurement device, but other specular reflection measurement devices may be used.

[0043] [Aspect] It is obvious to those skilled in the art that the above-described exemplary embodiments are specific examples of the following aspects.

[0044] (Item 1) The specular reflection measurement device according to Item 1 performs specular reflection measurement on a flexible sheet-like member, and includes a sample holder having an outer cylinder and an inner cylinder inserted into the outer cylinder with a predetermined gap, and an irradiation optical system that irradiates measurement light onto the sheet-like member covering one end of the inner cylinder inserted into the outer cylinder. A detector disposed at a position where the measurement light that is specularly reflected by the sheet-like member covering one end of the inner cylinder inserted into the outer cylinder is incident is provided.

[0045] (Item 4) The sample holder for a specular reflection measurement device according to Item 4 is for holding a sample that is a flexible sheet-like member in a specular reflection measurement device that performs specular reflection measurement, an outer cylinder, an inner cylinder inserted into the outer cylinder is provided.

[0046] The predetermined gap is set to a gap such that the sheet-like member is sandwiched.

[0047] The inner cylinder may be hollow or solid, but in order to more reliably prevent reflection of light by the inner cylinder, it is preferably hollow. In the case of a solid inner cylinder, in order to suppress the irradiation light from being reflected at one end of the inner cylinder and being erroneously detected, a concave portion is provided at the one end so that at least a part of the sheet-like member and one end of the inner cylinder do not come into contact.

[0048] According to the specular reflection measurement device according to Item 1 and the sample holder for a specular reflection measurement device according to Item 4, while covering one end of the inner cylinder with a sheet-like member, the inner cylinder is inserted into the outer cylinder from the one end side, and a part of the sheet-like member is sandwiched between the inner side surface of the outer cylinder and the outer side surface of the inner cylinder, whereby a flexible sheet-like member can be held in the sample holder without slack, and thereby specular reflection measurement can be accurately performed with good reproducibility.

[0049] (Item 2) The specular reflection measurement device according to Item 2 is the specular reflection measurement device according to Item 1, wherein the sample holder further has a protruding portion protruding from the outer side surface of the inner cylinder, the distance between the protruding portion and one end of the inner cylinder is set such that when the inner cylinder is inserted into the outer cylinder until the protruding portion abuts against one end of the outer cylinder, the irradiation light irradiated from the irradiation optical system reaches one end of the inner cylinder.

[0050] According to the specular reflection measurement apparatus according to the second aspect, by inserting the inner cylinder to the position where the protruding portion abuts against one end of the outer cylinder, the position of the sheet-like member covering one end of the inner cylinder with respect to the irradiation optical system can be accurately set.

[0051] (Third aspect) The specular reflection measurement apparatus according to the third aspect is the specular reflection measurement apparatus according to the second aspect, wherein the distance between the protruding portion and one end of the inner cylinder is equal to the distance between the protruding portion and the other end of the inner cylinder.

[0052] According to the specular reflection measurement apparatus according to the third aspect, no matter which of one end side and the other end side of the inner cylinder is inserted into the outer cylinder, by inserting to the position where the protruding portion abuts against one end of the outer cylinder, the position of the sheet-like member with respect to the irradiation optical system can be accurately set.

Explanation of reference numerals

[0053] 1…UV-visible spectrophotometer (specular reflection measurement apparatus) 11…Light source 12, 34…Sample chamber 121, 341…Irradiation light window 122, 342…Detection light window 123…Irradiation light reflecting mirror (irradiation optical system) 124…Detection light reflecting mirror 13…Diffraction grating 14…Detector 15, 37…Housing 20, 40…Sample holder 201, 401…Opening of sample chamber 21, 41…Outer cylinder 211, 411…One end of outer cylinder 22, 42…Inner cylinder 221, 421…One end of inner cylinder 2210…Opening of one end of inner cylinder 222…The other end of the inner cylinder 23, 43 …Protruding portion 3…FTIR (specular reflection measurement apparatus) 30…Interferometer chamber 300…Infrared light source 301…Condensing lens 302… Collimator mirror 303… Beam splitter 304… Fixed mirror 305… Moving mirror 3051… Driver 306… Laser light source 307… Mirror for the first laser 308… Mirror for the second laser 309… Laser detector 32… Main interference light window 331… Parabolic mirror 332… Ellipsoidal mirror 343… Irradiation optical system in the sample chamber 344… Detection optical system in the sample chamber 35… Infrared detector 36… Control unit

Claims

1. It is for performing specular reflection measurement on a flexible sheet-like member, a sample chamber surrounded by a wall and having an opening in the wall, a cylindrical sample holder insertion part fixed to the periphery of the opening, a sample holder inserted into the sample holder insertion part with a predetermined gap and having a mark on its side surface, an irradiation optical system provided at a position for irradiating measurement light to the sheet-like member which is the measurement target sample covering one end of the sample holder inserted into the sample holder insertion part up to the mark, a detector provided at a position in the sample chamber where the measurement light specularly reflected by the sheet-like member covering one end of the sample holder inserted up to the mark enters. A specular reflection measurement apparatus comprising the above.

2. It is for performing specular reflection measurement on a flexible sheet-like member, a sample chamber surrounded by a wall and having an opening in the wall, a cylindrical sample holder insertion part fixed to the periphery of the opening, a sample holder having a cylindrical part inserted into the sample holder insertion part with a predetermined gap and a protruding part protruding from the outer surface of the cylindrical part, an irradiation optical system provided at a position for irradiating measurement light to the sheet-like member which is the measurement target sample covering one end of the cylindrical part inserted into the sample holder insertion part up to the position where the protruding part abuts against one end of the sample holder insertion part, a detector provided at a position in the sample chamber where the measurement light specularly reflected by the sheet-like member covering one end of the cylindrical part inserted up to the position where the protruding part abuts against one end of the sample holder insertion part enters. A specular reflection measurement apparatus comprising the above.

3. The specular reflection measurement apparatus according to claim 2, wherein the distance between the protruding part and one end of the cylindrical part is equal to the distance between the protruding part and the other end of the cylindrical part.

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