The present invention relates to a measurement device for directly measuring the thickness, a change in the thickness, a reaction measurement, a thermal response, water adsorption, etc. of various measurement objects deployed on a thick film transparent medium used in the field of regenerative medicine without any other optical medium interposed.
It is conventionally difficult in the field of regenerative medicine to measure the film thickness of a transparent thin film sample arranged on a Petri dish (thick film transparent medium). In general, as a method of measuring the film thickness of a transparent thin film sample, for example, a film thickness measurement method is known in which the reflection interference spectroscopic measurement of a transparent thin film sample is performed and the film thickness of the transparent thin film sample is measured by conversion into the film thickness. However, in this film thickness measurement method, it is difficult to directly measure the film thickness of a transparent thin film sample arranged on a thick film transparent medium since there is too much optical noise caused by back surface reflection of a commercially available Petri dish or the like.
As a measurement device to measure the film thickness of a transparent thin film sample arranged on a thick film transparent medium using a lens system, a reflectance measurement device is known which is capable of measuring the spectral reflectance of only the transparent thin film sample by eliminating light reflected by the back surface of the thick film transparent medium, through adoption of a special optical system, without performing an antireflection treatment or similar treatment on the back surface of the thick film transparent medium (Non Patent Literature 1). However, although this reflectance measurement device can be used to calculate the film thickness at one point, it is difficult to reproduce the conditions of focus adjustment, and reflection interference components cannot be perfectly extracted, and thus the film thickness of the transparent thin film sample cannot be measured with high accuracy. In addition, continuous measurement of the film thickness cannot performed, nor is it possible to perform measurement in a combined manner in water and the air to measure the film thickness of the transparent thin film sample.
Meanwhile, reflectometric interference spectroscopy (RIfS) is known which is capable of measuring the film thickness of a transparent thin film sample by emitting white light onto a transparent thin film sample formed on a sensor chip and spectrally dispersing and analyzing interference components of the surface-reflected light reflected at the surface of the transparent thin film sample and the bottom surface-reflected light reflected at the bottom surface of the sensor chip applied with the transparent thin film sample by a spectroscope (Patent Literature 1). Since optical fibers are used to receive the surface-reflected light and the bottom surface surface-reflected light in this RIfS, it is not necessary to perform focus adjustment, and it is possible to easily perform continuous measurement of a light interference bottom peak shift that is related to a change in the film thickness of the transparent thin film sample. In addition, in this RIfS, a medium having a refractive index significantly different from that of the transparent thin film sample or a highly coherent SiN substrate is prepared as a sensor chip in order to improve the measurement accuracy, and the transparent thin film sample is formed on the SiN substrate to reduce the noise reflection on the back surface of the transparent thin film sample and to increase interference signals, thereby enabling highly accurate measurement of the film thickness and highly accurate continuous measurement of the film thickness. Note that since a SiN substrate can eliminate the influence of back surface reflection and can amplify interference signals, highly accurate continuous measurement of the film thickness can be performed both in water and in the air by arranging a transparent thin film sample on the SiN substrate.
Patent Literature 1: JP 3786073 B2
Non Patent Literature 1: Olympus Corporation “Industrial Microscope USPM-RU III,” Retrieved on Apr. 18, 2017, from http://www.olympus-ims.com/ja/metrology/lens-spectral/uspm-ru3/
However, the above RIfS has disadvantages that a transparent thin film sample needs to be in close contact with the sensor chip and that in a case where the film thickness of the sample exceeds approximately 10 μm, interference signals are attenuated by the sensor chip, thereby hindering acquisition of interference data.
The reflectometric interference spectroscopy using optical fibers also has a disadvantage that it is not possible to directly measure a transparent thin film sample on a thick film transparent medium. This is because reflection interference signals of the transparent thin film sample are buried in reflection noise of a Petri dish and thus cannot be obtained in a case where the transparent thin film sample having a thickness of about several tens of nanometers to several micrometers is arranged on the Petri dish since the thickness of the Petri dish used as the thick film transparent medium is about 1 mm.
An object of the present invention is to provide a measurement device capable of directly measuring a transparent thin film sample on a thick film transparent medium with high accuracy.
Prior to completing the present invention, the inventors first conducted the following verification of principles as experiments on which the inventive concept is based. This verification of principles was conducted to find out the reason why no interference signals of a transparent thin film sample on a thick film transparent medium can be obtained when a pan-focus receiving system of optical fibers excellent in continuous measurement is used.
White light was projected from the light projecting optical fiber 103 toward the gelatin using this optical system 101, and beam patterns of interference light of three components were observed on the gelatin as illustrated on the left of
In the verification of principles, it was found that any one of the beam patterns of interference light of three components can be selectively received by orthogonally arranging the optical axis of the light projecting optical fiber 103 and the optical axis of the light receiving optical fiber 110, arranging the light receiving optical fiber 110 at a position 120 mm away from the second lens 109, and changing the position of the light receiving surface of the light receiving optical fiber 110.
Specifically, it was found that interference light observed as a beam pattern 112 was received and that a spectrum illustrated in a graph 118 in the upper right of
Meanwhile, it was found that, in the case where the spectra of interference light of these three components were combined, that is, in the case where the components were not separated, the phases of the interference signals of the three components were mutually reversed and cancelled each other out and that no surface reflection interference waveform was obtained as illustrated in
On the basis of these findings, the inventors have completed the present invention to implement an optimum configuration which ensures that reflection interference signals of a transparent thin film sample not be buried in the reflection noise of a thick film transparent medium and enables separation of interference signals of three components having different phases to prevent the interference signals of the three-components from canceling each other out.
That is, in order to implement at least one of the above-mentioned objects, a measurement device reflecting one aspect of the present invention includes the following.
[1] A measurement device for measuring a sample arranged on a thick film transparent medium, the measurement device including: a light source that emits white light; a light projecting part including a light projecting surface for projecting the white light emitted from the light source toward the sample; a light receiving part including a transmission path including a light receiving surface for receiving reflection interference light which is the white light, having been projected from the light projecting surface, reflected by a surface of the sample and a surface of the thick film transparent medium; a spectroscopic part that detects intensity of light of each certain wavelength interval included in the reflection interference light received by the light receiving surface; and a measurement part that measures the sample on the basis of the detection result of the spectroscopic part, in which the light projecting surface, the light receiving surface, the thick film transparent medium, and the sample are set so as to satisfy the following inequation (α) for eliminating noise light reflected from a back surface of the thick film transparent medium.
h<(L/n3)·√((2H/D2)·(2H/D2)−n3·n3+1) Inequation (α)
(In inequation (α), h denotes a distance from the light receiving surface to the sample, L denotes a half of an interval between the light projecting surface and the light receiving surface, n3 denotes the refractive index of the thick film transparent medium, H denotes a thickness of the thick film transparent medium, and D2 denotes the aperture of the light receiving surface).
According to the present invention, it is possible to provide a measurement device capable of directly measuring a transparent thin film sample on a thick film transparent medium with high accuracy.
A measurement device of the present invention includes the followings.
[1] A measurement device for measuring a sample arranged on a thick film transparent medium, the measurement device including: a light source that emits white light; a light projecting part including a light projecting surface for projecting the white light emitted from the light source toward the sample; a light receiving part including a transmission path including a light receiving surface for receiving reflection interference light which is the white light, having been projected from the light projecting surface, reflected by a surface of the sample and a surface of the thick film transparent medium; a spectroscopic part that detects intensity of light of each certain wavelength interval included in the reflection interference light received by the light receiving surface; and a measurement part that measures the sample on the basis of the detection result of the spectroscopic part, in which the light projecting surface, the light receiving surface, the thick film transparent medium, and the sample are set so as to satisfy the following inequation (α) for eliminating noise light reflected from a back surface of the thick film transparent medium.
h<(L/n3)·√((2H/D2)·(2H/D2)−n3·n3+1) Inequation (α)
(In inequation (α), h denotes a distance from the light receiving surface to the sample, L denotes a half of an interval between the light projecting surface and the light receiving surface, n3 denotes the refractive index of the thick film transparent medium, H denotes a thickness of the thick film transparent medium, and D2 denotes the aperture of the light receiving surface).
[2] The measurement device according to [1], in which the measurement device is set to satisfy the following formulas (β) for causing reflection light, which has been incident on the sample at an incident angle less than or equal to a numerical aperture of the light projecting part and reflected at a surface of the sample, to be incident on the light receiving part at an incident angle less than or equal to a numerical aperture of the light receiving part:
h≥L/tan β1 and h≥L/tan β2 Formulas (β)
(in formulas (β), β1 denotes the numerical aperture of the light projecting part, and β2 represents the numerical aperture of the light receiving part).
[3] The measurement device according to [1] or [2], in which the measurement device is set to satisfy the following formula (γ) for avoiding a component having an inverted phase from entering a light beam incident on the light receiving surface:
|ΔAA−ΔBB|=2×n2×d×(2π/λ)×|cos γθ−cos γα1|<π Formula (γ)
(in formula (γ), ΔAA denotes a phase difference of the light beam in a shortest optical path, ΔBB denotes a phase difference of the light beam in a longest optical path, n2 denotes a refractive index of the sample, d denotes a film thickness of the sample (mm), denotes a reflection angle in the sample, θ denotes a reflection angle in the shortest optical path, and α1 denotes a reflection angle in the longest optical path).
[4] The measurement device according to any one of [1] to [3], in which an aperture of the light receiving surface is 200 nm, the interval between the light projecting surface and the light receiving surface is 0.2 mm, and the interval between the light receiving surface and the sample is 0.5 mm or more and 0.6 mm or less.
[5] The measurement device according to any one of [1] to [3], in which an aperture of the light receiving surface is 200 nm, the interval between the light projecting surface and the light receiving surface is 0.3 mm or 0.4 mm, and the interval between the light receiving surface and the sample is 0.8 mm or more and 1.0 mm or less.
[6] The measurement device according to any one of [1] to [3], in which an aperture of the light receiving surface is 100 nm, the interval between the light projecting surface and the light receiving surface is 0.2 mm or more and 0.4 mm or less, and the interval between the light receiving surface and the sample is 1.0 mm or more and 2.0 mm or less.
[7] The measurement device according to any one of [1] to [3], in which an aperture of the light receiving surface is 50 nm, the interval between the light projecting surface and the light receiving surface is 0.2 mm or more and 0.4 mm or less, and the interval between the light receiving surface and the sample is 1.0 mm or more and 3.0 mm or less.
[8] The measurement device according to any one of [1] to [7], further including: a single light transmission part that accommodates the light projecting part and the light receiving part, in which the light transmission part projects the white light from the light projecting surface of the light projecting part and receives the reflection interference light by the light receiving surface of the light receiving part.
Hereinafter, with reference to the drawings, a measurement system according to an embodiment will be described by taking an example of a measurement system used for measurement of a sample arranged on a thick film transparent medium.
Note that the white light source 2, the spectroscope 4, and the light transmission part 6 are preferably accommodated in the main body of the measurement device 10, and the controller 8 in the form of, for example, a personal computer (PC) is connected to the main body of the measurement device in a controllable manner.
The white light source 2 includes a light source lamp (not illustrated) and a housing (not illustrated) for housing the lamp. The housing has a communication function with the controller 8, and preferably enables adjustment of the light quantity by the controller 8 in a software-based manner. The light source lamp is only required to perform continuous light emission in the visible to near infrared light such as 400 to 800 nm or 400 to 1000 nm. For example, a halogen lamp, a xenon lamp, or a white LED may be used.
The light transmission part 6 includes a light projecting optical fiber 6a for projecting the white light emitted by the white light source 2 onto the sample 12 and a light receiving optical fiber 6b for receiving reflection interference light of the white light emitted from the light projecting optical fiber 6a and guiding the reflection interference light to the spectroscope 4. Here, there are two types of light transmission parts 6: a light transmission part 6 which separately includes a light-projecting light transmission part 6A and a light-receiving light transmission part 6B (hereinafter referred to as a separate-axes-system light transmission part 6) as illustrated in
Meanwhile in the separate-axes-system light transmission part 6, the substantially cylindrical light receiving optical fiber 6b may not surround the light projecting optical fiber 6a. For example, the substantially cylindrical light projecting optical fiber 6a and the substantially cylindrical light receiving optical fiber 6b may be bundled. In this case, when the light transmission part 6 is viewed from the lower end surface side, the light receiving surface 6d and the light projecting surface 6c each having a circular shape are adjacent to each other as illustrated in
In a case where the light projecting optical fiber 6a and the light receiving optical fiber 6b are bundled in this manner, it is possible for the light receiving surface 6d to receive the interference light even if a light receiving angle θ1 is increased.
Note that the single light transmission part 6 is more preferable as the light transmission part 6 since it is more compact than the separate-axes-system light transmission part 6 and allows surface reflection interference light to be efficiently incident on the light receiving surface 6d.
The spectroscope 4 is an analysis instrument for detecting the intensity of light of each certain wavelength interval included in the light received through the light receiving optical fiber 6b.
The controller 8 has a function of controlling the respective parts of the measurement device 10 in an integrated manner, and receives input of execution of detection operation from an operator, and outputs an execution instruction of the detection operation control to the measurement device 10. The controller 8 also has an operation function of performing an operation on the basis of data acquired from the spectroscope.
The Petri dish 14 representing the thick film transparent medium includes a cylindrical circumferential wall 14b surrounding a disk 14a as illustrated in
The sample 12 is a measurement object made of a transparent material, and is arranged on the surface of the disk 14a as a thin film having a thickness of 1 nm to 100 μm upon measurement. Here, for example, a scaffold material for regenerative medicine such as gelatin or collagen is used as the sample 12.
Hereinafter, a process of measuring the sample 12 using the measurement device 10 of the embodiment will be described. Note that a case in which collagen is used as the sample 12 and the Petri dish 14 made of polystyrene is used will be described as an example here.
First, an operator places an aqueous solution of the sample 12 on the surface of Petri dish 14 and then evaporates the water to obtain deposit of the sample 12. Alternatively, the sample 12 may be deposited over time after the placement of the aqueous solution. Further alternatively, the Petri dish 14 on which the aqueous solution of the sample 12 is arranged is mounted on a spin coater (not illustrated), and a thin film of the sample 12 is formed on the surface of the Petri dish 14 while the rotation speed of the spin coater is adjusted.
Next, when the Petri dish 14 is arranged at a predetermined position below the light transmission part 6 and the white light source 2 is turned on, white light transmitted through the light projecting optical fiber 6a is emitted from the light projecting surface 6c, and the sample 12 is irradiated with the white light. As a result, a beam pattern 20a of first sample surface reflection interference light, a beam pattern 20b of sample surface transmission interference light, and a beam pattern 20c of second sample surface reflection interference light appears as beam patterns of interference light on the sample 12 as illustrated in
In the measurement device 10 of the present embodiment, it is possible to spatially separate interference light to be measured from other interference light that becomes noise and to selectively receive the interference light to be measured by appropriately setting the apertures of the light projecting part 6A and the light receiving part 6B, the N/A (numerical aperture) of the light receiving part 6B, the distance between the light projecting part 6A and the light receiving part 6B, the distance between the light projecting part 6A and the Petri dish 14, and the distance between the light receiving part 6B and the Petri dish 14. This prevents a plurality of interference waves of the different phases from being combined and canceling each other out, and thus it is possible to measure the film thickness of the sample 12 and changes in the film thickness with high accuracy.
Here, each beam of interference light will be described. As illustrated in
Meanwhile, the sample surface transmission interference light is obtained by interference among the reflection light reflected by the bottom surface of the Petri dish 14, the reflection light first reflected by the front surface of the Petri dish 14, then at the front surface of the sample 12, and further reflected at the bottom surface of the Petri dish 14, and the interference light first reflected at the bottom surface of the Petri dish 14, then at the front surface of the sample 12, and further reflected at the front surface of the Petri dish 14 as illustrated in
In addition, the second sample surface reflection interference light is obtained by interference between the reflection light first reflected at the bottom surface of the Petri dish 14, then at the front surface of the Petri dish 14, and then again at the bottom surface of the Petri dish 14 and the reflection light first reflected at the bottom surface of the Petri dish 14, then at the front surface of the sample 12, and reflected again at the bottom surface of the Petri dish 14 as illustrated in
Next, when the interference light incident on the light receiving surface 6d is guided to the spectroscope 4 via the light receiving optical fiber 6b, the spectroscope 4 detects the intensity of light of each certain wavelength interval included in the interference light incident on the light receiving surface 6d and outputs as the spectrum intensity to the controller 8.
The controller 8 acquires data of the spectrum intensity of the interference light from the spectroscope 4 and divides the spectrum intensity of the interference light by the spectrum intensity of the white light serving as a reference to calculate the reflectance for each wavelength band. The spectrum intensity data of the reference light may be measured and held in advance at the time of assembly and adjustment of the measurement device, or may be acquired upon each measurement by other means. The controller 8 generates a reflection interference spectrum on the basis of the calculated reflectance, and determines the bottom (minimum value) and the peak (maximum value) of the reflectance. Then, the controller 8 calculates the film thickness of the sample 12 by substituting the minimum and the maximum wavelengths (λ) of the reflectance into, for example, a predetermined calculation formula having been simulated in advance. Alternatively, the controller 8 can acquire the amount of change (Δλ) of a measured reflectance minimum or maximum wavelength with respect to a minimum or maximum wavelength of a reference reflectance (baseline). In this case, the amount of change of the film thickness is calculated on the basis of the amount of change (Δλ) of the reflectance minimum wavelength.
According to the measurement system 1 of the present embodiment, it is possible to suppress the reflectance of light at the bottom surface of the Petri dish 14 by appropriately setting the apertures of the light projecting part 6A and the light receiving part 6B, the N/A (numerical aperture) of the light receiving part 6B, the distance between the light projecting part 6A and the light receiving part 6B, the distance between the light projecting part 6A and the Petri dish 14, and the distance between the light receiving part 6B and the Petri dish 14. As a result, the interference light to be measured is not buried in the reflection noise on the bottom surface of the Petri dish 14, and thus the sample 12 arranged on the Petri dish 14 can be directly measured without arranging a special sensor chip on the Petri dish 14. In addition, since the interference light is received using the optical fiber, it is not necessary to adjust the focus every time the film thickness changes, and the sample 12 arranged on the Petri dish 14 can be continuously measured in water and in the air.
Note that although the description has been given using the light projecting optical fiber 6a and the light receiving optical fiber 6b as the transmission paths in the embodiment; however, these are merely examples, and the transmission paths may not necessarily be optical fibers.
Next, conditions for eliminating the noise light reflected from the back surface of the Petri dish 14 to measure the sample 12 in the embodiment will be described.
The main elements of specific conditions include the following (1) to (6) illustrated in
(1) Aperture of the light receiving part 6B
(2) N/A (numerical aperture) of the light receiving part 6B
(3) Distance between the light transmission parts 6
(4) Distance between the light receiving part 6B and the sample 12
(5) Refractive index of the Petri dish 14
(6) Thickness of the Petri dish 14
(7) Distance between the light projecting part 6A and the sample 12
(8) Aperture of the light projecting part 6A
(9) N/A (numerical aperture) of the light projecting part 6A
In this measurement, it is possible to acquire film thickness information of the sample 12 with highly accuracy by allowing only signals to be incident on the Light receiving optical fiber 6b out of light interference components of the sample 12, which are the signals, and transmission reflection components in the Petri dish 14, which are noise. Next, the positional relationship of the light interference signals, the noise, the light projecting part, and the light receiving part will be described. In the case of the separate-axes-system light transmission part 6, although the light projecting optical fiber 6a may be inclined to adjust the amount of incident light in some cases; however, the optical axis does not change in terms of a numerical value in theoretical calculation, and thus it suffices to describe by the aperture of the tip, the positional relationship, etc.
First, according to (3), the distance between the light projecting part 6A and the light receiving part 6B, and (4) and (7), the distances from the sample 12, the white light emitted from the light projecting optical fiber 6a is reflected at and the bottom surface and the front surface of the sample 12, the beams of light intersect and interfere with each other, then are reflected at the same angle as that projected onto the sample 12, and enters the light receiving optical fiber 6b.
In reality, since the light transmission part 6 expands as the effective diameter (aperture×N/A) increases, the smaller the effective diameter of the light transmission part 6 is, the higher the performance of sorting signal components becomes.
Meanwhile, the light transmitted through the Petri dish 14 and reflected from the bottom surface of the Petri dish 14 also has a noise component that cancels out the light interference signal and thus are to be avoided from entering the light receiving optical fiber 6b as much as possible. This noise is refracted depending on the refractive index×thickness of the Petri dish 14 when transmitted by the Petri dish 14, and is transmitted by the thickness of the Petri dish 14. As for the noise light reflected by the bottom surface of the Petri dish 14, light projection/reception conditions for emission at a position shifted from that of the signal light can be derived from a theoretical formula.
When the light receiving optical fiber 6b and the sample 12 are close to each other, although the light utilization efficiency is good, noise components are likely to enter the light receiving optical fiber 6b. When they are too distant from each other, the light interference signal are degraded, and thus a relationship that enables a good balance is necessary. Similarly, the reflection light angles of light projection/reception (determined by the distance between the light projecting part 6A and the light receiving part 6B and the distances from the surface of the sample 12) need to be inclined to some extent to cause light interference. However, if it is too large, the signal light cannot be received.
Next, conditions for measurement of film thickness interference fringes of the sample 12 arranged on the Petri dish 14 will be described with reference to
Condition 1. The reflection light having been incident on the sample 12 at an incident angle less than or equal to the N/A of the light projecting part 6A and reflected at the front surface thereof enters the light receiving part 6B at an incident angle less than or equal to the light reception N/A.
Condition 2. The reflection light reflected at the bottom surface of the Petri dish 14 do not enter the light receiving part 6B.
Condition 3. A difference |ΔA−ΔB| between a phase difference ΔA of a light beam A in the shortest optical path of the sample 12 and the phase difference ΔB of the longest optical path difference light beam B of the sample 12 is <π. That is, there is no component having an inverted phase in the light beam incident on the light receiving part 6B.
Lower limit conditional expressions of the distance h between the light projecting surface 6c/the light receiving surface 6d and the sample 12 (hereinafter referred to as the measurement instrument-measurement plane distance h) are determined from the above Condition 1:
h≥L/tan β1 and h≥L/tan β2 <1>.
From the above Condition 2, an upper limit conditional expression of the measurement instrument-measurement plane distance h is determined:
h<(L/n3)·√((2H/D2)·(2H/D2)−n3·n3+1) <5>′″.
Furthermore, according to the above condition 3, the distance 2L between the light projecting part 6A and the light receiving part 6B (hereinafter referred to as the light projection-light reception interval 2L), the size D1 of the light projecting part 6A, and the size D2 of the light receiving part 6B are determined. That is, conditions for avoiding a component having an inverted phase from entering a light beam incident on the light receiving surface is determined:
|ΔAA−ΔBB|=2×n2×d×(2π/λ)×|cos γθ−cos γα1|<π. <7>.
Note that the contents denoted by the symbols illustrated in
h: measurement instrument-measurement plane distance, L: distance from the light projecting part 6A or the light receiving part 6B to the midpoint, D1: aperture of the light projecting part 6A, D2: aperture of the light receiving part 6B, β1: N/A (numerical aperture) of the light projecting part 6A, β2: N/A of the light receiving part 6B, α1: reflection angle in the longest optical path (from far end to far end), α: reflection angle from the near end of the light projecting part 6A to the far end of the light receiving part 6B, θ: reflection angle in shortest optical path (middle point, from near end to near end), θ1: reflection angle of a light beam incident from the far end of the light projecting part 6A to the near end of the light receiving part 6B, n1: medium refractive index between the light projecting surface 6c or the light receiving surface 6d and the sample 12 (1 in the atmosphere, 1.33 in the water), n2: refractive index of the sample 12, n3: refractive index in the Petri dish 14, γ: reflection angle in the sample 12, H: film thickness of the sample 12, ΔAA: phase difference of a light beam in the shortest optical path, and ΔBB: phase difference of a light beam in the longest optical path.
Next, the method of deriving a theoretical formula regarding the conditions for measurement of film thickness interference fringes on the Petri dish 14 will be described in detail.
Lower limit conditional expressions regarding the condition 1 are derived as below.
θ≤β1 (light projection N/A) and θ≤β2 (light reception N/A) <1>
α≤β1 and α≤β2 <2>
θ1≤β1 and θ1≤β2 <3>
α1≤β1 and α1≤β2 <4>
Here,
tan θ=L/h
tan α=(2L+D2)/2h, and
tan θ1=(2L+D1)/2h.
Substitution of tan α1=(2L+D1+D2)/2h into <1>, <2>, <3>, and <4> leads the following lower limit conditional expressions of h.
L/h≤tan β1 and L/h≤tan β2
→h≥L/tan β1 and h≥L/tan β2 <1>
h≥(L+D2/2)/tan β1 and h≥(L+D2/2)/tan β2 <2>
h≥(L+D1/2)/tan β1 and h≥(L+D1/2)/tan β2 <3>
h≥(L+(D1+D2)/2)/tan β1 and h≥(L+(D1+D2)/2)/tan β2 <4>
Upper limit conditional expressions regarding the condition 2 are derived as illustrated below.
PS>2L+D2 <5>
Here,
PQ=L=h·tan θ
QR=OB=2H·tan φ
RS=h·tan φ
∴PS=PQ+QR+RS
=h·tan θ+2H·tan φ+h·tan θ
=2(h·tan θ+H·tan φ)
=2(L+H·tan φ)
Substitution of this into <5> leads to
2(L+H·tan φ)>2L+D2.
∴tan φ>D2/2H <5>′
Here, from Snell's law,
n1·sin θ=n3·sin φ
∴sin φ=sin θ/n3
∴cos φ=√(1−sin φ·sin φ)
=√(1−sin θ·sin θ/(n3·n3))
Substitution of these into <5>′ leads to
sin θ/√(n3·n3−sin θ·sin θ)>D2/2H <5>″.
Here, sin θ=L/√(L·L+h·h) is substituted to obtain
√((n3·n3−1)+(n3·h/L)·(n3·h/L))<2H/D2
∴(n3·n3−1)+(n3·h/L)·(n3·h/L)<(2H/D2)·(2H/D2)
∴(n3·h/L)·(n3·h/L)<(2H/D2)·(2H/D2)−(n3·n3−1)
∴n3·h/L<√((2H/D2)·(2H/D2)−n3·n3+1)
∴h<(L/n3)·√((2H/D2)·(2H/D2)−n3·n3+1) <5>═″
P′S′>2L+D1+D2 <6>
Here,
P′Q′=h·tan θ1=(2L+D1)/2
Q′R′=O′B′=2H·tan φ1R′S′=h·tan θ1
∴P′S′=P′Q′+Q′R′+R′S′
=h·tan θ1+2H·tan φ1+h·tan θ1
=2(h·tan θ1+H·tan φ1)
=2((2L+D1)/2+H·tan φ1)
=2L+D1+2H·tan φ1
Substituting this into <6> leads to
2L+D1+2H·tan φ1>2L+D1+D2.
∴tan φ1>D2/2H <6>′
Here, from Snell's law,
n1·sin θ1=n3·sin θ1
∴sin θ1=sin θ1/n3
∴cos φ1=√(1−sin θ1·sin φ1)
=√(1−sin θ1·sin θ1/(n3·n3))
Substitution of these into <6>′ leads to
sin θ1/√(n3·n3−sin θ1·sin θ1)>D2/2H <6>″.
Here, substitution of sin θ1=(L+D1/2)/√(h·h+(L+D1/2)·(L+D1/2)) leads to
(L+D1/2)/√(n3·n3·{h·h+(L+D1/2)·(L+D1/2)}−(L+D1/2)(L+D1/2))>D2/2H.
∴h<(L+D1/2)/n3×{{(2H/D2)·(2H/D2)−n3·n3+1 <6>′″
The upper limit value is h that satisfies both the derivation formulas (1) (<5>′″) and (2) (<6>″′). In practical terms, formula <5>′″ is the maximum value.
Conditional expressions of the film thickness d of the sample 12 and the dimensions of the measurement instrument (sensor interval L, aperture D1 of the light projecting part, and aperture D2 of the light receiving part) regarding the condition 3 are derived as below.
OA=d/cos γ=AB
OB=2d·tan γ
OC=OB·sin θ=2d·tan γ·sin θ
From Snell's Law,
n1 sin θ=sin θ=n2·sin γ.
The optical path length difference Δ between <1> and <2> is expressed as below:
Therefore, the phase difference ΔAA of the light beam AA in the shortest optical path is expressed as below:
ΔAA=2·n2·d·(2π/λ)·cos γθ.
The phase difference ΔBB of the light beam BB in the longest optical path is expressed as below:
ΔBB=2·n2·d·(2π/λ)·cos γα1.
Therefore, the conditional expressions for the difference between the phase differences is as follows:
|ΔAA−ΔBB|=2·n2·d·(2π/λ)·|cos γθ−cos γα1|<π <7>
Detailed calculation is further illustrated below.
cos γθ=√(1−sin γθ·sin γθ).
From Snell's Law,
n1·sin θ=sin θ=n2·sin γθ.
Substitution into the above equation leads to
cos γθ=√(1−(sin θ/n2)·(sin θ/n2)).
Here,
From sin θ=L/√(L·L+h·h),
Similarly,
cos γα1=√(1−sin γα1·sin γα1).
From Snell's Law,
n1·sin α1=sin α1=n2·sin γα1.
Substitution into the above equation leads to
cos γα1=√{1−(sin α1/n2)·(sin α1/n2)}.
Here,
sin α1={(2L+D1+D2)/2}/√[{(2L+D1+D2)·(2L+D1+D2)/4}+h·h].
From this equation,
Surface reflection interference light can be received by substituting equations <8> and <9> into formula <7>.
The relationship between the film thickness d to be measured and the dimensions of the measurement device (the light projection-light reception interval 2L, the aperture D1 of the light projecting part, and the aperture D2 of the light receiving part) is obtained.
Next, derivation of a theoretical formula regarding the conditions for measurement of film thickness interference fringes on the Petri dish 14 will be described.
Next, a theoretical design for the above three conditions will be described. As a measurement system, the sizes of the light projecting part 6A and the light receiving part 6B, and the distance between the light projecting part 6A and the light receiving part 6B can be set as desired. It is also possible to change the distance between the sample 12 and the light projecting part 6A and the distance between the sample 12 and the light receiving part 6B. Note that, in the present embodiment, in place of the light projecting optical fiber 6a and the light receiving optical fiber 6b, optical components such as lenses that do not require focus adjustment may be used for light projection and light reception. Alternatively, small projector and receiver may be directly disposed.
Meanwhile, in order to extract only the surface reflection interference components, it is necessary to satisfy conditions defined by theoretical formulas. That is, the condition that the surface reflection interference light, generated from the light beam having been emitted from the light projecting part 6A an incident on the sample 12, be incident on the light receiving part 6B gives the lower limit of the measurement instrument-measurement plane distance h. Moreover, the condition that noise components, transmitted to and reflected at the back surface of a container out of the irradiation light, not be included gives the upper limit of the measurement instrument-measurement plane distance h. It is important to satisfy the both conditions in the measurement of the surface reflection interference component.
Meanwhile, the received interference components include various light beams: for example in
Note that the structure of the light transmission part 6 is not limited as long as the conditions 1 to 3 are satisfied. For example, the light projecting part and the light receiving part may be coaxial or have separate axes. Moreover, one of them may be at a different position, the two may have opposite angles, or one of the two may be orthogonal to a measurement plane, whereas the other is inclined.
Note that the calculation of the interference phase difference is performed by using a formula obtained by dividing both sides by π:
|ΔAA−ΔBB|=2×n2×d×(2/λ)×|cos γθ−cos γα1|<1.
In designing a measurement device using the theoretical formulas, the following actual measurement values of an MI-Affinty (manufactured by Konica Minolta, INC.) dedicated optical fiber trusted as a coaxial optical fiber for reflection interference measurement were used as initial values. The present invention is not limited to these design examples since there are many design elements.
In the measurement device of the present invention, it can be understood that the interference measurement conditions exists only between 0.42 and 0.596 where the measurement instrument-measurement plane distance h (mm) is much shortened than usual (see
It can be seen that the film thickness thicker than or equal to 6 μm cannot be measured under these device conditions since the phases of the interference waveforms are reversed to cancel each other out when the film thickness of the sample 12 is allowed to vary (see
It can be understood that although this level of size differences of the light projecting part 6A have little influence on the lower limit and the upper limit of the measurement instrument-measurement plane distance h, the interference phase difference may become too large when the size becomes too large (see
The lower limit value of the light projection h becomes large when the N/A of the light projecting part 6A is too small; however, this level of differences have no significant influence (see
(5) Theoretical Design Example 5: Influence of Increase of light Projection-Light Reception Interval 2L (Improved Design)
It can be understood that by increasing the light projection-light reception interval 2L from the initial 0.2 mm to 0.3 mm or 0.4 mm, the allowance of measurement increases and that in relation to the size of the light receiving part 6B, the lower limit value (best) of the measurement instrument-measurement plane distance h on the light receiving side, capable of receiving most of the reflection interference light, is also satisfied for the light receiving part 6B sized less than or equal to 0.1 mm (see
(6) Theoretical Design Example 6: Influence of Increase in size of Light Projection-Light Reception (Deteriorated Design)
It can be seen that the interference phase difference exceeds 1 when the size of the light projecting part 6A is increased and exceeds 1 mm and that interference measurement becomes completely impossible (see
Hereinafter, examples of experiments performed using the measurement system 1 according to the embodiment will be described.
[Sample Preparation 1] Prior to performing examples 1 to 5, an operator first prepared five 30 ml sample tubes, and weighed 0.1 g, 0.25 g, 0.5 g, 1 g, and 2 g of gelatin (Gelatin Type A manufactured by MP Biomedicals, Inc) as the sample 12 as illustrated in Table 2. Further, ultrapure water was added to each portion of the gelatin so that the total weight of the gelatin and the ultrapure water in a sample tube weights 10 g each. Next, each sample tube was left to be allowed to swell at room temperature for 30 minutes, and then the water and the gelatin in each sample tube were heated to 50° C. while being stirred. The gelatin was dissolved in water in this manner to obtain gelatin solutions at concentrations of 1 wt %, 2.5 wt %, 5 wt %, 10 wt %, and 20 wt %. The samples of the prepared gelatin solutions of the respective concentrations were numbered Gel1, Gel2, Gel3, Gel4, and Gel5, respectively.
Next, five cut-outs, obtained by cutting a polystyrene Petri dish 14 (manufactured by Iwaki Glass Co. Ltd.) into a size of 26 mm×20 mm, were prepared as the thick film transparent medium. Then the cut-out five polystyrene Petri dishes were sequentially set on a spin coater, and the above five types of gelatin solutions were applied onto the polystyrene Petri dishes. Note that each of the gelatin solutions was applied onto the polystyrene Petri dish in such a manner that the spin coater was pre-accelerated to a rotational speed of 500 rpm five seconds after the start of the rotation, and then allowed to rotate for 60 seconds to allow the solution which had been excessively applied to be removed. Next, the polystyrene Petri dish applied with the gelatin was dried by heating in a drier set at 60° C. for 30 minutes to allow gelatin of different thicknesses to be formed on the five polystyrene Petri dishes. Next, after taking a photograph of a cross section of the gelatin by an electron microscope, the film thickness of the gelatin was obtained.
The following theoretical formulas were used in the configuration of the measurement device of the examples. Although expressions 1 and 2 both define the lower limit value of h, a larger one is determined as the lower limit value of h. The distance h between a sample and a light receiving sensor needs to be set between the lower limit value and the upper limit value of the above expressions. If the distance h between the sample and the light receiving sensor is not set between the lower limit value and the upper limit value of the above expressions, noise increases and the reflected interference signal decreases.
L/tan β1 Expression 1:
Lower limit value of light projection h (light projecting part A-measurement plane distance): Condition for capturing surface reflection interference light
L/tan β2 Expression 2:
Lower limit value of light reception h (light receiving part B-measurement plane distance): Condition for capturing surface reflection interference light
(L/n3)·√(2H/D2)·(2H/D2)−n3·n3+1) Expression 3:
Upper limit value of light reception h: Condition for elimination of back surface reflection
|ΔAA−ΔBB|=2×n2×d×(2π/λ)×|cos γθ cos γα1<1 Formula 4:
Interference phase difference in the light receiving surface 6d:
The MI-Affinity coaxial optical fiber was placed in a dark box, and its height was made adjustable by a Z stage. In addition, a non-transmissive mask made of steel was prepared which has a size that completely closes a φ200 μm core part of the light receiving part 6B and has a 100 μm pinhole opened at the center part thereof. The coaxial optical fiber was improved by attaching the optically black mask so that the core diameter becomes 100 μm and that light projection-light reception interval becomes 0.3 mm. Measurement data was imported from the spectroscope 4 into a personal computer via USB, and spectrum intensity data of the polystyrene Petri dishes applied with the gelatin was normalized and divided by a normalized spectrum intensity of a reference Petri dish not applied with the gelatin to obtain spectral reflectance. The configuration of these measurement devices, theoretical calculation results, and measurement results of the film thickness are shown below.
Even with a coaxial optical fiber for reflection interference spectroscopy, it is difficult to efficiently extract only the surface reflection interference light if it is not designed for removing the back surface reflection noise, and thus no interference signal can be obtained. From the theoretical formula, it is desirable that the light receiving part 6B be placed at a position that satisfies the lower limit condition of h, which is the condition for receiving the front surface reflection interference light, and the upper limit condition of h related to the back surface noise. However, as illustrated in
Note that the film thickness of the gelatin was approximately calculated using equation 5, which is derived from Snell's law, and then was calculated by detailed fitting using an interference waveform simulator. The refractive index n1 of the gelatin is set to 1.53.
d=N·λ1·λ2/(λ1−λ2)×1/(2·n1·cos θ) Equation 5
Contrast=(a−b)/(a+b) Equation 6
In the configuration of the measurement device of example 1, only the light projecting optical fiber 6a forming the cladding portion was connected to a white light source (lamp housing MHF-V501, halogen lamp MORITEX LM-50 12V 50 W, both manufactured by MORITEX Corp.) without connecting the light receiving optical fiber 6b that forms the core portion of the attached coaxial optical cable to a light source. Meanwhile, an optical fiber was selected from the following list of optical fibers (manufactured by Edmund Optics) the diameter of which varies, secured at an angle of 0 degrees with respect to the sample surface, and connected to a spectroscope (mini-spectroscope C10535CA-51 manufactured by Hamamatsu Photonics K.K.).
Next, the interval between the light projecting optical fiber 6a and the light receiving optical fiber 6b and the distance between the light receiving optical fiber 6b and the sample 12 were adjusted as illustrated in the table.
A measurement device of a two-axes measurement system using a 50 μm optical fiber F1 for the light receiving part 6B was used. In both of comparative examples 1 and 2, the incident interference light cause phase inversion, and thus the theoretical formula is not satisfied. As a result, the gelatin thin film on the Petri dish was not measured correctly. On the other hand, it can be seen that the interference light can be measured accurately and that the film thickness is calculated with no problem in the measurement device of the measurements 1 to 4 satisfying the theoretical formulas of the present invention. That is, it became clear that a thin film on the petri dish 14 can be accurately measured by the measurement device of the present invention in which the aperture of the light receiving surface 6d is set to φ50 μm, the distance between the light projecting surface 6c and the light receiving surface 6d is set to be within a range of 0.2 mm and 0.4 mm, and the interval between the sample and the light receiving surface 6d is set to be within a range of 2.2 mm and 3 mm.
A measurement device of a two-axes measurement system using a 100 μm optical fiber F2 for the light receiving part 6B was used. In the comparative example 1, the incident interference light causes phase inversion, and in the comparative example 2, h is set outside the range between the upper limit and the lower limit of h and thus does not satisfy the theoretical formulas. As a result, the gelatin thin film on the Petri dish was not measured correctly. On the other hand, it can be seen that the interference light can be measured accurately and that the film thickness is calculated with no problem in the measurement device of the measurements 1 to 4 satisfying the theoretical formulas of the present invention. That is, it became clear that a thin film on the petri dish 14 can be accurately measured by the measurement device of the present invention in which the aperture of the light receiving surface 6d is set to φ100 μm, the distance between the light projecting surface 6c and the light receiving surface 6d is set to 0.4 mm, and the interval between the sample 12 and the light receiving surface 6d is set to 2.2 mm.
A measurement device of a two-axes measurement system using a 200 μm optical fiber F3 for the light receiving part 6B was used. In both of the comparative examples 1 and 2, h does not satisfy the lower limit nor the upper limit of the theoretical calculation, and in the comparative example 1 the incident interference light causes phase inversion. In either respect, the theoretical formulas are not satisfied. As a result, the gelatin thin film on the Petri dish 14 could not be measured correctly. On the other hand, it can be seen that the interference light can be measured accurately and that the film thickness is calculated with no problem in the measurement device of the measurements 1 to 4 satisfying the theoretical formulas of the present invention. That is, it became clear that a thin film on the petri dish 14 can be accurately measured by the measurement device of the present invention in which the aperture of the light receiving surface 6d is set to φ200 μm, the distance between the light projecting surface 6c and the light receiving surface 6d is set to 0.3-0.5 mm, and the interval between the sample 12 and the light receiving surface 6d is set to a range between 0.9 mm and 1.5 mm.
A measurement device of a two-axes measurement system using a 400 μm optical fiber F4 for the light receiving part 6B was used. In both of comparative examples 1 and 2, the lower limit value and the upper limit value of the distance h between the light receiving surface and the sample are reversed, and in the comparative example 2, the incident interference light causes phase inversion. The theoretical formulas are not at all satisfied. As a result, the interference waveform could not be measured. Although this fiber diameter has a small measurable area, it can be seen that the interference light can be measured accurately and that the film thickness is calculated with no problem in the measurement 1 satisfying the theoretical formulas of the present invention. That is, even in the case where the aperture of the light receiving surface 6d is φ400 μm, it became clear that a thin film on the petri dish 14 can be accurately measured by the measurement device of the present invention, in which the distance between the light projecting surface 6c and the light receiving surface 6d is set to 0.8 mm and the interval between the sample 12 and the light receiving surface 6d is set to 1.2 mm on the basis of the theoretical formulas.
1 Measurement system
2 White light source
4 Spectroscope
6 Light transmission part
6A Light-projecting light transmission part (light projecting part)
6B Light-receiving light transmission part (light receiving part)
6
a Light projecting optical fiber
6
b Light receiving optical fiber
6
c Light projecting surface
6
d Light receiving surface
8 Controller
10 Measurement device
12 Sample
14 Petri dish
Number | Date | Country | Kind |
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2017-104415 | May 2017 | JP | national |
Filing Document | Filing Date | Country | Kind |
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PCT/JP2018/016264 | 4/20/2018 | WO | 00 |