JP2009042007A - Orientation measuring instrument and orientation measuring method - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To enhance an S/N ratio when a dielectric resonator is rotated to measure orientation. <P>SOLUTION: An oscillator 12, a variable attenuator 32, a detection diode 36 and an amplifying circuit 38a are mounted on a rotor other than a detection part containing the dielectric resonator 4 to be integrally rotated. The oscillator 12 and the amplifying circuit 38a are connected to the rotary terminal provided to the rotor, a personal computer 18a and a power supply 42 are connected to the oscillator 12 through the contact of the fixed terminal of a slip ring 20 and the rotary terminal, and the amplifying circuit 38a and an A/D converter 38a are connected. <P>COPYRIGHT: (C)2009,JPO&INPIT

Description

  The present invention measures the orientation of these samples by microwaves, including three-dimensional articles such as polymer-like sheets containing paper, sheets such as paper, and molded articles such as plastics, resins, and rubbers. The present invention relates to an apparatus and a method. In particular, the present invention relates to an apparatus and method suitable for on-line measurement for measuring orientation along a running direction of a sample while the sample is in the form of a sheet.

  Conventionally, X-ray diffraction, infrared dichroism, mechanical breaking strength, ultrasonic wave propagation speed, birefringence, polarization fluorescence method, microwave method and the like have been used as methods for measuring the orientation of a sheet-like substance. Yes.

  Among these, the method that is practically used as a so-called on-line measuring device that can measure a sample while traveling is only a method using birefringence. This is a method for obtaining the anisotropy of the refractive index, that is, the birefringence or retardation (birefringence x thickness) in the sheet surface (see Patent Document 1). However, since the method using birefringence needs to be measured by transmitting visible light (polarized light), there is a problem in that it can be measured only by a substance that transmits light to some extent, such as a transparent film.

Therefore, the present inventors have devised a device for measuring orientation by using a microwave dielectric resonator to bring a detection unit into contact with or approaching from one side of a sample (see Patent Document 2). This method basically uses a change in resonance frequency when a dielectric resonator is in contact with or close to one side of a sample, and does not need to be a material that transmits light, and is a PET (polyethylene terephthalate) film. It is a method that can measure a sheet-like substance such as online.

FIG. 1 shows a plan view of one rectangular dielectric resonator 4 as seen from the sample measurement surface side.
A rectangular dielectric resonator 4 is excited by one rod antenna 2, and the transmitted energy by the dielectric resonator 4 is detected by the other rod antenna 6.

The rectangular dielectric resonator 4 excited by the rod antenna 2 takes a plurality of resonance modes. A measurement example of the resonance spectrum is shown in a waveform diagram in FIG. Of the various resonance modes, it is preferable to select a resonance mode in which the electric field vectors are parallel on the upper surface (sample measurement surface) of the dielectric resonator 4 and the interaction component with the sample is as large as possible. . In order to confirm such a resonance mode, an elongated paper impregnated with a radio wave absorber is placed so as to be parallel to the long side of the rectangular dielectric resonator, and the change in the resonance peak level is examined. If the electric field vector and the elongated paper are parallel, the peak level of the resonance curve is greatly attenuated. Conversely, if the electric field vector is orthogonal, the peak level hardly changes. By utilizing this, it is desirable to investigate all the resonance peaks and to select a peak having the largest peak level attenuation width and a high Q value. An example of the peak is indicated by an arrow. The resonance mode at this peak is considered to be the E ^X _{211 + δ} mode based on the calculation result of the resonance frequency. The electric field vector of this resonance mode E ^X _{211 + δ} is parallel to the long-side direction of the resonator, and there are two positions where the intensity is maximum in that direction. This electric field distribution coincides with the electric field distribution investigated using the radio wave absorber. A part of this electric field oozes out from the upper surface of the dielectric resonator and exists as a so-called evanescent wave, and its intensity decreases exponentially as the distance from the surface increases. This evanescent wave is used to measure the orientation of the sample.

  When a polymer sheet or the like is brought close to the vicinity of the sample measurement surface of the dielectric resonator, the resonance spectrum shifts to the low frequency side as shown in FIG. The shift amount changes according to the dielectric constant of the sample in the direction of the electric field vector, the gap between the dielectric resonator and the sample, the thickness of the sample, and the like. For example, FIG. 3 shows a shift in the resonance spectrum when one PE (polyethylene) sheet is placed as a polymer sheet on the sample measurement surface of the dielectric resonator 4 shown in FIG.

The theoretical calculation of the resonance frequency can be calculated by the formula described below. When the sample measurement surface of one dielectric resonator placed only on one side of the sample is placed on a measurement target sample with a known thickness under certain conditions and the resonance frequency is measured, the measurement is performed according to the following formula (1). The dielectric constant of the target sample is obtained.
β _g L = π / 2 + Pπ + tan ⁻¹ (α ₂ / β _g ) · tanh [tanh ⁻¹ (α ₃ / α ₂ ) + α ₂ L ₂ ] (1)
α ₂ = (k _c ² −ω ₀ ² ε ₀ μ ₀ ε _S ) ^1/2 α ₃
= (K _c ² −ω ₀ ² ε ₀ μ ₀ ) ^1/2 β _g
= (Ω ₀ ² ε ₀ μ ₀ ε _r −k _c ² ) ^1/2

Here, ε _S is the dielectric constant of the sample, ε _r is the dielectric constant of the dielectric resonator, L is the thickness of the dielectric resonator, ε ₀ is the dielectric constant of the measurement atmosphere (air), and μ ₀ is the measurement atmosphere. Permeability, ω ₀ is the microwave resonance angular frequency, L ₂ is the thickness of the sample to be measured, k _c is a constant (eigenvalue) determined by the shape of the dielectric resonator, electromagnetic field mode, etc. P is 0, 1, 2, 3 (this number means an integral multiple of the axial direction λ _g / 2). Here, the certain condition is that measurement is performed by bringing the sample measurement surface of the dielectric resonator into contact with the sample, or the sample measurement surface of the dielectric resonator is separated from the sample by a certain distance. Shows that From this equation, it can be seen that if the thickness of the sample is constant, the shift amount of the resonance frequency (difference between the resonance frequency when blanking and the resonance frequency when the sample is present) depends only on the dielectric constant of the sample.

FIG. 4 shows the relationship between the molecular chain orientation of the sample and the anisotropy of the dielectric constant. FIG. 4 schematically shows the orientation state of the molecular chains of the sample in the upper stage, and a diagram in which the anisotropy of the dielectric constant of the sample in that state is measured is shown in combination in the lower stage. The lower diagram shows the magnitude of the dielectric constant in each direction. Here, if a molecular chain segment or a microcrystal is considered as one fiber, it is also applicable to a sample such as paper or nonwoven fabric. In that case, the fiber orientation is known. In that case, it is well known that the anisotropy of the dielectric constant is manifested depending on the arrangement of the fibers even when the fibers themselves are not oriented (for example, in the case of glass fibers). In any case, the dielectric constant takes the maximum value (εmax) in the direction in which the molecular chain or fiber faces, and the difference (Δε) from the minimum value (εmin) represents the degree of orientation. Therefore, by measuring which direction has the largest dielectric constant, the orientation direction can be determined.
Japanese Patent Laid-Open No. 4-89553 Japanese Patent No. 3731314

  As described above, since the basic principle is to measure the orientation of the sample from the anisotropy of the dielectric constant, one dielectric resonator is rotated while the sample and the dielectric resonator are close to or in contact with each other. (Theoretically, a half rotation is sufficient, and a quarter rotation is possible if the orientation direction is constant.) If the change of the resonance frequency is measured by a method in which a plurality of resonance frequencies are electrically measured at the same time (see Patent Document 2), the dielectric anisotropy, that is, the orientation is measured. be able to.

  In order to excite the dielectric resonator, a microwave signal must be transmitted to the excitation antenna. In the method of rotating the dielectric resonator, the excitation antenna and the detection antenna are rotated together with the dielectric resonator, but it has been common knowledge that the oscillator that generates the microwave signal is fixed. . In that case, it is a normal method to transmit a microwave signal to the excitation antenna through a rotating contact from a fixed oscillator.

  The present inventors also examined such a method, but found that it was difficult to suppress noise and it was not easy to increase the S / N (signal to noise) ratio.

  In view of this, the present invention aims to increase the S / N ratio when performing orientation measurement by rotating or rotating one dielectric resonator.

The orientation measuring apparatus of the present invention includes a measurement plane that is close to or in contact with a sample and is disposed only on one surface side of the sample, and substantially excludes the dielectric resonator except for the measurement plane. A shielding case made of a conductive material to be covered; an excitation antenna that is arranged inside the shielding case and generates an electric field vector having a unidirectional component in the dielectric resonator; and the dielectric resonator arranged inside the shielding case A detection unit comprising a detection antenna that detects transmission energy or reflection energy by the oscillation unit, an oscillation unit that is electrically connected to the excitation antenna and supplies a microwave signal and repeatedly sweeps the frequency of the microwave signal, and A detection unit having an amplifier circuit that is electrically connected to the detection antenna and amplifies the detected signal, and the detection unit is rotated in the measurement plane. Or a rotation mechanism that rotates, and a frequency sweep by the sweep unit that is electrically connected to the oscillation unit and the detection unit and is rotated or rotated by the rotation mechanism, and each frequency sweep is performed from the output of the detection unit. A control / calculation unit that detects the resonance frequency and obtains the dielectric anisotropy of the sample from the correspondence between the rotation angle of the detection unit and the resonance frequency is provided.
The rotation mechanism rotates or rotates not only the detection unit but also the oscillation unit and the detection unit as a unit.

  Further, the orientation measurement method of the present invention includes one dielectric resonator, a shield case made of a conductive material that substantially covers the dielectric resonator except for a measurement plane of the dielectric resonator, and the shield case An excitation antenna that is arranged inside the dielectric resonator and generates an electric field vector having a unidirectional component in the dielectric resonator, and a detection antenna that is arranged inside the shield case and detects transmitted energy or reflected energy by the dielectric resonator A detection unit comprising: an oscillation unit that supplies a microwave signal that is electrically connected to the excitation antenna and repeatedly sweeps the frequency of the microwave signal; and a signal that is electrically connected to the detection antenna and detected. Using a measuring device having a detection unit equipped with an amplifying circuit for amplifying, the measuring plane of the dielectric resonator approaches or contacts the sample In other words, it is arranged only on one surface side of the sample, and the detection unit, the oscillation unit, and the detection unit are integrally rotated or rotated in the measurement plane, and a frequency sweep is performed by the sweep unit while the detection unit is rotating or rotating. The resonance frequency in each frequency sweep is detected from the output of the detection unit, and the dielectric anisotropy of the sample is obtained from the correspondence between the rotation angle of the detection unit and the resonance frequency.

  A preferred application of the present invention further includes a sample supply mechanism for moving the sample while maintaining the sheet-like sample in a position where one surface thereof approaches or contacts the measurement plane of the dielectric resonator. This is an on-line measuring device that repeatedly measures the dielectric anisotropy of a sample with this orientation measuring device while running.

FIG. 5 schematically shows the present invention in a block diagram.
A microwave rod antenna (or loop antenna) 2 suitable as an excitation antenna for the dielectric resonator 4 is disposed at an appropriate position in an appropriate direction with respect to the dielectric resonator 4, and an oscillator as an oscillation unit A resonance mode in which a microwave signal having a predetermined frequency corresponding to a resonance frequency is supplied from 12 to the rod antenna 2 to cause the dielectric resonator 4 to resonate and an electric field vector protruding from the dielectric resonator 4 to the outside exists. make. As the resonance mode, there are a HEM mode when the sample measurement surface 4a of the dielectric resonator 4 is circular, a TM mode, a TE mode, and the like when the sample is a rectangle. The intensity of the electric field vector decreases almost exponentially as the distance from the dielectric resonator 4 increases, but the sample 10 is moved away from the dielectric resonator 4 or brought into contact with the dielectric resonator 4. By placing, the resonance frequency shifts according to the dielectric constant of the sample 10 due to electromagnetic coupling.

  The microwave emitted from the dielectric oscillator 4 is magnetically coupled to the dielectric resonator 4 by a rod antenna (or loop antenna) 6 as a detection antenna, and the dielectric resonator 4 can be in a resonance state. The electric field vector of the dielectric resonator 4 appears in a form substantially parallel to the surface of the sample 10 and interaction with the dipole moment of the sample 10 occurs.

In order to increase the Q value of the resonance curve by the microwave signal detected by the rod antenna 6, a shield case 8 made of a conductive material that substantially covers the dielectric resonator 4 except for the measurement plane 4a of the dielectric resonator 4. Is provided.
The dielectric resonator 4, the rod antennas 2 and 6, and the shield case 8 constitute a detection unit.

  Here, the angle between the sample 10 and the dielectric resonator 4 is changed while maintaining the state in which the sample measurement surface 4a of the dielectric resonator 4 is close to or in contact with the sample 10, thereby detecting the detector as a detector. By detecting the microwave intensity appearing at 14 corresponding to the rotation angle, the orientation state can be obtained from the angular dependence of the intensity. The controller 16 controls the frequency of the microwave generated from the oscillator 12 and takes in the microwave intensity from the detector 14. The computer 18 functions as a data processing device, receives a signal from the controller 16, and obtains the orientation state from the angle dependency of the detected microwave intensity. The controller 16 and the computer 18 implement a control / arithmetic unit.

  In order to change the angle formed between the sample 10 and the dielectric resonator 4, the sample 10 is rotated or rotated in the parallel plane between the sample 10 and the dielectric resonator 4, or the dielectric resonator 4 is moved to the sample 10. And rotating in a plane parallel to the dielectric resonator 4.

  FIG. 6 shows an example in which the dielectric resonator 4 is rotated in a parallel plane between the sample 10 and the dielectric resonator 4. A detection unit including the dielectric resonator 4, the rod antennas 2 and 6, and the shield case 8 is attached to the oscillator 12, and the oscillator 12 and the detector 14 are rotated or rotated together with the detection unit. The oscillator 12 includes a sweep circuit that repeatedly sweeps the frequency of the generated microwave signal, and the detector 14 includes an amplifier circuit that amplifies the detected signal. The oscillator 12 is supplied with AC 100 volt power via a slip ring 20. The slip ring 20 is an example of a rotating mechanism having a fixed terminal and a rotating terminal that are in contact with each other and maintain an electrical connection. The rotating terminal is electrically connected to the oscillator 12 and the detector 14, and the fixed terminal is a computer. 18 is electrically connected. As the rotation drive system, for example, a motor 22 such as a stepping motor is used, and a mechanism capable of adjusting the rotation speed by controlling the input pulse by the computer 18 is provided. Information on the angle formed by the dielectric resonator 4 with respect to the sample 10 is detected by an angle detection mechanism provided in the motor 22 and transferred to the computer 18.

Further, the principle of orientation measurement will be described. In a dielectric resonator, there is a relationship as shown in FIG. 7A between transmitted microwave intensity and frequency. This resonance curve is called a Q curve. The Q curve changes according to the following relationship by placing the sample.

  FIG. 7B shows the change. When the sample has anisotropy in a plane facing the sample measurement surface of the dielectric resonator, when the sample or the dielectric resonator is rotated in a plane parallel to the plane, for example, as shown in FIG. In addition, the peak frequency (resonance frequency) of the Q curve changes for each relative rotation angle position (S) of the sample with respect to the dielectric resonator.

In the first method of orientation measurement, in this rotation, for example, in the Q curve shifted to the highest frequency side, the transmission microwave detection intensity at the peak frequency is I, and the detection intensity on the high frequency side is I / 2. Let f ₁ be the frequency at which The transmission microwave detection intensity at each rotation angle at the frequency f ₁ is shown as a cross section in FIG. When it is rewritten with the rotation angle S as the horizontal axis, it is as shown in FIG. Furthermore, when it is rewritten in the polar coordinate system, it becomes an ellipse as shown in FIG. 9B, and the orientation angle (φ) and the orientation degree (a / b) can be obtained from this result. a is the major axis length of the ellipse, and b is the uniaxial length.

  Since high speed is required for on-line measurement, when the method of rotating the dielectric resonator is taken, the measurement object moves during the rotation time. If the angle formed by the electric field vector is changed at high speed, the resonance frequency corresponding to the angle is measured, and the orientation pattern is obtained from the plurality of data, high-speed measurement is possible.

  In the second method of orientation measurement, the difference between the resonance frequency when blanking and the resonance frequency when there is a sample is used as a shift amount, and this is represented by Δf. When the sample is oriented, since there is anisotropy of dielectric constant, the resonance frequency changes depending on the relative rotation angle position, and thus Δf also changes. The rotation angle at which Δf is the largest is the direction with the maximum dielectric constant, and the direction in which the fibers or molecular chains are oriented. When Δf is rewritten in the polar coordinate system, an orientation pattern as shown in FIG. 10 is obtained. In FIG. 10, the MD (Machine Direction) direction is the sample traveling direction in the case of online measurement, and this direction is taken as the reference direction. MT is a direction orthogonal to the reference direction, and in the case of online measurement, it is the width direction of the sample. φ (angle formed between the reference direction and the maximum dielectric constant) represents the orientation angle, and the difference between the major axis a and the minor axis b or the value obtained by dividing it by the major axis a or the minor axis b is the degree of anisotropy. Represents.

  An actual electrical signal processing system is shown in FIG. A microwave signal emitted from a microwave sweep oscillator (sweeper) 30 as an oscillating unit that is electrically connected to an excitation antenna and supplies a microwave signal and repeatedly sweeps the frequency of the microwave signal is converted into a variable attenuator 32 and an isolator. 34, and supplied to the dielectric resonator 4 via an excitation antenna (not shown). The intensity of the microwave signal transmitted through the dielectric resonator 4 is detected by a detection antenna (not shown) and converted into a voltage by the detection diode 36. A variable attenuator 32 inserted between the microwave sweep oscillator 30 and the excitation antenna is a variable amount signal attenuator / amplifier and adjusts the intensity of the microwave signal supplied to the dielectric resonator 4. The microcomputer 16a corresponding to the controller 16 in FIG. 5 compares the detected resonance peak level with a separately set target resonance peak level, and attenuates or amplifies the variable attenuator 32 so as to approach the target resonance peak level. Control by sending a signal to change the degree. It is desirable to set the target resonance peak level voltage to a value close to the maximum value within the input range of the amplifier and analog / digital conversion circuit unit 38. This means that the dynamic range can be widened by taking as large a value as possible in the input range of the analog / digital converter circuit, which means that the accuracy is improved, and a margin at the time of overshoot is left by slightly lowering the maximum value. That is the purpose.

  The isolator 34 is a two-port nonreciprocal passive circuit device that transmits microwaves in the forward direction and absorbs microwaves in the reverse direction. By using the isolator 34, the reflected wave can be easily removed.

  A voltage from the detection diode 36 is amplified by an amplifier and an A / D converter 38 and A / D converted, and a peak position is detected by a peak detection circuit 40. The frequency sweeping by the microwave sweep oscillator 30 under the control of the microcomputer 16a is repeated at a constant cycle, and a synchronization signal that is at a high level only during the sweep is simultaneously output from the microwave sweep oscillator 30. If the microcomputer 16a measures the time from when the signal becomes high level until the transmission intensity reaches the maximum value, the resonance frequency can be obtained.

  The resonance frequency obtained by the microcomputer 16a is sent to the personal computer 18a. The personal computer 18a controls the rotation or rotation of the dielectric resonator 4, and obtains the orientation of the sample from the relationship between the rotation angle and the resonance frequency sent from the microcomputer 16a. The microcomputer 16a and the personal computer 18a implement a control / arithmetic unit.

  The entire configuration including the rotation mechanism in the electric signal processing system of FIG. 11 is as shown in FIG. 12 or FIG. In the configuration of FIG. 12, the rotation mechanism is a slip ring 20. The slip ring 20 includes a stator that is provided with a fixed terminal so as not to rotate, and a rotor that is provided with a rotation terminal and is rotated with respect to the stator. Stay connected. In addition to the detection unit including the dielectric resonator 4, the rotor of the slip ring 20 includes an oscillator 12 (a microwave sweep oscillator 30 as an example), a variable attenuator 32, a detection diode 36, and an amplifier circuit 38a. Can be rotated as In electrical connection, the oscillator 12 and the amplifier circuit 38a are connected to a rotation terminal provided on the rotor. On the other hand, the personal computer 18a, the power source 42, and the A / D converter 38a are connected to a fixed terminal provided on the stator, and the personal computer 18a and the power source 42 are connected to the oscillator 12 through contact between the fixed terminal of the slip ring 20 and the rotating terminal. The amplifier circuit 38a and the A / D converter 38a are connected.

  In FIG. 12, electrical connection is made via the slip ring 20, but since the oscillator 12 is mounted on the rotor of the slip ring 20 and rotated together with the detection unit, a fixed terminal and a rotary terminal are provided in the transmission path of the microwave signal. The contact portion is not interposed, and the generation of noise can be suppressed. Further, a contact portion between the fixed terminal and the rotation terminal is interposed between the amplifier circuit 38a and the A / D converter 38a. Since the analog signal passing through the portion is amplified, the analog signal before amplification is amplified. Compared with the contact portion between the fixed terminal and the rotating terminal interposed in the transmission line, it is possible to suppress a decrease in the S / N ratio.

  The configuration of FIG. 13 is different from the configuration of FIG. 12 in that the A / D converter 38a is also mounted on the rotor of the slip ring 20 and rotated as a unit. In this case, a contact portion between the fixed terminal and the rotation terminal is interposed between the A / D converter 38a and the peak detection circuit 40. Since the portion that passes through this portion is a digital signal, it is also amplified in that case. Compared with the case where the contact portion between the fixed terminal and the rotating terminal is interposed in the previous analog signal transmission path, it is possible to suppress a decrease in the S / N ratio.

FIG. 14 is a time chart when the Bw MHz frequency range is swept at t ₁ sec (seconds). The sweep of the Bw MHz frequency range is repeated at t ₁ sec at intervals of T ₂ sec.

  When measuring the orientation of a sheet-like material in a short time, as represented by on-line measurement, in a method irrelevant to the individual difference of dielectric resonators, one dielectric resonator is used as described above. It is necessary to collect the data of the resonance frequency shift at each angle in a short time by changing the angle formed by the electric field vector of the dielectric resonator with respect to the sample as fast as possible.

Here, the measurement of the resonance frequency shift amount by the sample will be described with reference to the flowchart of FIG. In step S1, the resonance frequency F ₀ is measured in a state where there is no sample (blank). In step S2, the resonance frequency F _s of the sample is measured, and in step S3, a difference Δf (= F ₀ −F _s ) between the resonance frequency in the blank state and the state where the sample is present is calculated. Through the above steps, the resonance frequency shift amount Δf in the sample is obtained.

FIG. 14 shows a polar coordinate display of the resonance curve associated with the microwave frequency sweep for measuring the frequency shift amount of the sample with respect to the angle formed by the sample and the dielectric resonator. The amount of change in the angle of the dielectric resonator with respect to the MD direction of the sample at time t ₁ and t ₂ [sec] is θ ₁ and θ ₂ , respectively. Using a microwave sweep oscillator with a microwave sweep time t ₁ [sec] and a time t ₂ [sec] from the end of the sweep to the start of the next sweep, the sweep was started when the angle was 0 degrees And The time from the start of peak position detection to the start of the next sweep is t ₁ + t ₂ .

Since the angle of the dielectric resonators with respect to MD direction of the sample is started sweeping at 0 degrees and the time until the n-th sweep is terminated and T _n,
T ₁ = t ₁ [sec]
T ₂ = t ₁ + t ₂ + t ₁ = 2t ₁ + t ₂ [sec]
...
T _n = nt ₁ + (n−1) t ₂ [sec]
Get a relationship.

Similarly, when the n-th sweep is terminated, when the angle of the dielectric resonators with respect to MD direction of the sample and A _n A ₁ = θ ₁
A ₂ = θ ₁ + θ ₂ + θ ₁ = 2θ ₁ + θ ₂
...
_{A n = nθ 1 + (n} -1) θ 2
It is written. And T _n and A _n is the corresponding.
However, it is desirable that θ ₁ and θ ₂ be as close to 0 degrees as possible.

  If the resonance frequency shift amount Δf in the sample corresponding to the angle A of the dielectric resonator with respect to the sample is measured and Δf is displayed in polar coordinates with respect to A, a pattern representing the orientation of the sample can be obtained. Thus, two examples of a method for obtaining an orientation pattern are shown: a method of rotating a dielectric resonator with respect to a sample and a method of swinging.

(Embodiment 1)
First, the produced sample is running, and the dielectric resonator is placed close to or in contact with the running sample, and the dielectric resonator rotates at a constant angular velocity with respect to the sample, and the fiber orientation Consider the case of measuring sex online. As shown in FIGS. 16A and 16B, the angle of the dielectric resonator with respect to the MD direction of the sample is θ.

A method for calculating the orientation pattern for each rotation period of the dielectric resonator with respect to the sample will be described with reference to the flowchart of FIG. First, for the sake of simplicity, the case where the rotation speed N is 1 is shown. In step S11, the resonance frequency shift amount Δf at each angle is calculated in accordance with the resonance frequency shift amount measurement method of FIG. In step S12, the rotational speed is identified. Since the rotation speed of the dielectric resonator relative to the sample is 1, angle A _n is 0 degrees <A _n ≦360_Donohan'idekurikaeshiderutafnoshutokuotsuzuke,A _n of the dielectric resonator relative to the MD direction of the sample> Since the first rotation ends when 360 degrees is satisfied, the process proceeds to step S13. In step S13, the data obtained in the first rotation, that is, Δf obtained in the range of 0 ° <A _n ≦ 360 ° is displayed in polar coordinates. The polar coordinates are displayed as shown in FIG. 18, and when the last sweep number satisfying A _n ≦ 360 degrees is m, the number of sweep times from the first time to the m-th is data for the first rotation speed of the resonator. That is, the data of the second rotation number of the resonator is the data from the number of sweeps m + 1.

  In step S14, elliptical approximation is performed on the obtained Δf data, and the process proceeds to step S15. When displaying raw data as it is, step S14 may be skipped. In step S15, an orientation pattern representing fiber orientation is displayed on the computer. Through the above steps, an alignment pattern in the case where the rotational speed is 1 is derived.

Subsequently, FIG. 19 shows a flowchart in the Nth rotation, generalizing the case where the orientation pattern is calculated for each rotation period of the dielectric resonator with respect to the sample. In step S21, the resonance frequency shift amount Δf at each angle is calculated in accordance with the resonance frequency shift amount measurement method of FIG. In step S22, the rotational speed is identified. When the rotational speed of the dielectric resonator of the N to the sample, N-th rotation (N is a positive integer) repeating acquisition of Δf in the range A _n is 360 (N-1) degree <A _n ≦ 360N degree in Subsequently, when A _n > 360 N degrees is satisfied, the routine proceeds to step 3. In step S23, the data obtained in the first rotation, that is, Δf obtained in the range of 360 (N−1) degrees <A _n ≦ 360 N degrees is displayed in polar coordinates. In step S24, ellipse approximation is performed on the obtained data of Δf, and the process proceeds to step S25. When displaying raw data as it is, step S24 may be skipped. In step S25, an orientation pattern representing fiber orientation is displayed on the computer. Through the above steps, an alignment pattern in the case where the rotation speed is N is derived.

The angle A _n, other than the above method is 0 ° ≦ A _n <360, may be a method of A _n is reset to 0 degrees Once turned 360 degrees.

Next, an example in which an alignment pattern is obtained by using an average of frequency shift data of N rotations will be described. When calculating the data average of the frequency shift amount, A _m = mθ ₁ + (m−1) θ ₂ = 360 degrees, so that the angular velocity returns to the angle at the start of the first sweep when the m + 1th sweep starts. Is selected, the relative angle of the dielectric resonator with respect to the sample does not depend on the rotational speed. In other words, a cycle having the same relative angle may appear with a cycle of m sweeps.

Therefore, when the relative angle of the dielectric resonator with respect to the MD direction of the sample is φ (0 degree ≦ φ <360 degrees) as shown in FIG.
φ ₁ = A ₁ relative angle = A _{m + 1} relative angle = A _{2m + 1} relative angle = ... = A _{Nm + 1} relative angle φ ₂ = A ₂ relative angle = A _{m + 2} relative angle = Relative angle of A _{2m + 2} = ... = Relative angle of A _{Nm + 2} ...
φ _r = A _r relative angle = A _{m + r} relative angle = A _{2m + r} relative angle =... = A _{Nm + r} relative angle and A having the same relative angle appear in m cycles. Here, r is represented by a positive integer satisfying 0 <r ≦ m, and the definition of the relative angle Φ is 0 degree ≦ φ <360 degrees, and when N rotations, r = n− (N−1) m (n is Number of sweeps, r is a positive integer satisfying 0 <r ≦ m)
It can be expressed as.

（ｉ＝は正の整数）
と表記される。このように、各相対角度においてＮ回転あたりの周波数シフト量の平均を算出し、楕円パターンを計算すれば、外的要因などに依るデータのばらつきを抑えることができる。 With data mean frequency shift amount of up to N-th rotation from one rotation, when calculating the elliptical pattern, in position relative angle phi ₁ is
(Δf of A ₁ + Δf of A _{m + 1 +} Δf of A _{2m + 1} +... + _{Af of} A _{Nm + 1} ) / N
Relative angle φ in ₂ positions (the Delta] f + A _{m + 2} A ₂ Δf ₊ A _2m + ₂ of Δf ₊ ... + A _Nm + ₂ in Delta] f) / N
...
At the position of the relative angle φ _r (Δf of A _{r +} Δf of Am + _r + Δf of A _{2m + r} + ... + Δf of A _{Nm + r} ) / N
Then, the average of the frequency shift amount for every N rotations at each relative angle is obtained. When this is expressed by an equation, when the n-th sweep is completed, the Δf average value at the relative angle Φ _r per N rotations is obtained by replacing the number of rotations with i.

(I = is a positive integer)
It is written. In this way, by calculating the average frequency shift amount per N rotations at each relative angle and calculating the elliptical pattern, it is possible to suppress variation in data due to external factors and the like.

In addition, some examples of how to average are given.
(1) Method of independently outputting the average every N rotations

(2) Accumulation method (moving average method) in which the first data is deleted and N averages are output when acquiring N + 1 rotation data

(3) Furthermore, a method of performing weighting processing on the latest data (weighted average method) can be used.

A data interpolation method can be applied as a method for obtaining more data than the number of data obtained by performing frequency sweep to obtain Δf. As shown in FIG. 21, seeking Δf by performing a frequency sweep by the detection unit rotation angle of the A _n, the Δf in the detector rotation angle position of the detection unit rotation angle position of A _n for (A _n + 180 °) Interpolate with Δf. As a result, the number of data that is twice the number of data actually measured can be obtained, and the accuracy of the required dielectric anisotropy is improved.

(Embodiment 2)
The concept of the method of rotating (swinging) the dielectric resonator with respect to the sample is almost the same. As shown in FIG. 22, the case where the dielectric resonator is swung every 180 degrees with respect to the MD direction of the sample with reference to the center of the dielectric resonator is taken as an example. Consider the case where the absolute value of the angular change rate (angular velocity) of the dielectric resonator with respect to the sample is constant, the angle starts sweeping from 0 degrees, and turns back at 180 degrees. Changes in the angle of the orientation device with respect to the sample at t ₁ and t ₂ [sec] are θ ₁ and θ ₂ , respectively, as shown in FIG. If the sweep is started when the angle of the dielectric resonator with respect to the sample is 0 degree, the time T _n until the n-th sweep is finished is
T ₁ = t ₁ [sec]
T ₂ = t ₁ + t ₂ + t ₁ = 2t ₁ + t ₂ [sec]
...
T _n = nt ₁ + (n−1) t ₂ [sec]
It becomes.

Similarly, when the n-th sweep is terminated, when the angle of the orientation device for MD direction of the sample and A _n A ₁ = θ ₁
A ₂ = θ ₁ + θ ₂ + θ ₁ = 2θ ₁ + θ ₂
...
A _n = nθ ₁ + (n−1) θ ₂
It is written. And T _n and A _n is the corresponding. However, it is desirable that θ ₁ and θ ₂ be as close to 0 degrees as possible.

FIG. 23 shows a flowchart for calculating the orientation pattern for each swing period of the dielectric resonator with respect to the sample. In step S31, the resonance frequency shift amount Δf at each angle is calculated in accordance with the resonance frequency shift amount measurement method of FIG. In step S32, the number of swings is identified. If the angle A _n of the dielectric resonators with respect to MD direction of the sample meets 0 degrees <A _n <180 continues to acquire repeated Delta] f, the step S33 when the A _n is 0 or 180 degrees To reverse the sign of the angular velocity of the swing. In step S34, using Δf at 0 degree <A _n <180 degrees obtained during the N-th swing, data of A _n +180 degrees is interpolated. In step S35, the data of Δf obtained in step 4 is displayed in polar coordinates as shown in FIG.

  In step S36, ellipse approximation is performed on the obtained Δf, and the process proceeds to step S37. When displaying raw data as it is, step S36 may be skipped. In step S37, an orientation pattern representing fiber orientation is displayed on the computer. Through the above steps, an alignment pattern in the case where the rotation speed is N is derived.

  Next, in the method of swinging the dielectric resonator every 180 degrees with respect to the sample MD direction as a reference, the orientation pattern is obtained using the average of the frequency shift amount data of N rotations. Give up. When calculating the data average of the frequency shift amount, the angle of the dielectric resonator with respect to the sample is constant regardless of the number of swings, as in the case of calculating the data average of the frequency shift amount by the rotation method. It is desirable. An example of a method for solving this will be given.

The angle changes of the alignment apparatus with respect to the sample at t ₁ and t ₂ [sec] are θ ₁ and θ ₂ , respectively, and one swing is performed from the start of the swing to 180 degrees, and then the number of swings is increased by 1 every time it is turned 180 degrees. . In order for the angle of the dielectric resonator to the sample to be constant, as shown in FIG. 25, after the m-th data acquisition, the angle of the dielectric resonator with respect to the sample MD direction at the start of the m + 1-th sweep is the m-th sweep. Wrap it up to match that at the end. For this purpose, as shown in FIG. 26, the angle of orientation device for the sample MD direction starts sweeping at theta _2/2 degrees, yet the angle of the sweep at the end of the m-th 180-θ _2/2 If it is a degree, it will be sufficient. Given these conditions, time T _n up to the n-th of the sweep is completed,
_{T 0 = (t 2/2} ) [sec]
_{T 1 = (t 2/2} ) + t 1 [sec]
_{T 2 = (t 2/2} ) + t 1 + t 2 + t 1 = 2t 1 + (3/2) t 2 [sec]
...
T _n = nt ₁ + (n−1 / 2) t ₂ [sec]
It becomes.

Similarly, when the n-th sweep is terminated, when the angle of the orientation device for MD direction of the sample and _{A n A 0 = (θ 2} /2)
_{A 1 = (θ 2/2} ) + θ 1
_{A 2 = (θ 2/2} ) + θ 1 + θ 2 + θ 1 = 2θ 1 + (3/2) θ 2
...
A _n = nθ ₁ + (n−1 / 2) θ ₂
It is written. And T _n and A _n is the corresponding. However, it is desirable that θ ₁ and θ ₂ be as close to 0 degrees as possible.

Therefore, after the m-th data acquisition, the condition for the angle of the dielectric resonator with respect to the sample MD direction at the start of the m + 1-th sweep to coincide with that at the end of the m-th sweep is:
_{A m + (θ 2/2} )
_{= Mθ 1 + (m-1} /2) θ 2 + (θ 2/2)
= M (θ ₁ + θ ₂ )
= 180 degrees (m: positive integer)
It becomes.

beyond the A _m is 180 degrees began to m-th data after acquisition, when swinging the folding opposite direction and phi (0 ° ≦ phi ≦ 180 degrees as shown in FIG. 27 the relative angle of the dielectric resonators with respect to MD direction of the sample ). From the swing start A _m is up to 180 degrees and 1 swing, since the swing speed is increased by one each time the wrap then 180 degrees, when the swing times is N,
phi ₁ = A ₁ relative angle = A _2m relative angle = A _{2m + 1} relative angle = A _4m relative angle = A _{4m + 1} relative angle = ... = a A _Nm relative angle = A _{Nm + 1} relative angle phi ₂ = a ₂ relative angle = a _2m-1 relative angle = a _{2m + 2} relative angle = a _4m-1 relative angle = a _{4m + 2} relative angle = ... = a _Nm-1 of Relative angle = A _{Nm + 2} relative angle ...
phi _r = A _r relative angle = A relative angle _{Nm (r-1)} (N = an even _{number) = A (N-1)} m + r relative angle (N = an odd number)
It becomes. Here, the relative angle Φ is 0 degree ≦ Φ ≦ 180 degrees, and r is a positive integer satisfying 0 <r ≦ m. R = n− (N−1) m (N is an odd number)
r = Nm-n + 1 (N is an even number)
(N is the number of sweeps, r is a positive integer that satisfies 0 <r ≦ m)
It becomes.

［ｓ＝１，２，３，…，Ｎ（Ｎが奇数）］

［ｓ＝１，２，３，…，Ｎ（Ｎが偶数）］ Using the above relationship, when calculating the elliptic pattern with the data average of the frequency shift amount for every N swings,
In the relative angle φ ₁ position,
(Of A ₁ of Δf + A _2m Δf + of _{A 2m + 1 Δf + ... +} A Nm of Δf ₊ A _Nm + ₁ of Δf) / N
Relative angle φ in ₂ positions (A ₂ Δf + A _2m-1 of Δf ₊ A _2m + ₂ of Δf + ... + A _Nm-1 of Δf ₊ A _Nm + ₂ in Delta] f) / N
It becomes. To generalize this, when the number of swings is i and i is an average of 1 to N times, the following equation is obtained with respect to the position of the relative angle φ _r .

[S = 1, 2, 3,..., N (N is an odd number)]

[S = 1, 2, 3,..., N (N is an even number)]

  In this way, by calculating the average frequency shift amount per number of swings N at each position and calculating the elliptic pattern, it is possible to suppress variation in data due to external factors and the like.

When performing polar coordinate display, or elliptic approximation, as shown in FIG. 24, the frequency shift amount of the angle A _n = the angle A _n +180 degrees frequency shift amount, it may supplement the data.

  Furthermore, as for the averaging method, as in the rotation method, a method of outputting an average for every N rotations independently, and when acquiring N + 1 rotation data, the first data is deleted and N averages are obtained. And a method of weighting the latest data.

  In the second embodiment, when rotating the dielectric resonator with respect to the sample, a slip ring can be used for the rotation mechanism as in the first embodiment. Further, the electrical connection between the oscillation unit and the detection unit mounted on the rotation mechanism and rotating together with the detection unit, and the control / calculation unit fixedly installed may be performed by a flexible cable. .

Since the swing range in the second embodiment is 180 degrees and the data of A _n +180 degrees is interpolated using the Δf measurement value at 0 degrees <A _n <180 degrees, the data over 360 degrees is excessive or insufficient. It is the most preferable because it can earn income. However, the swing range in the second embodiment is not limited to 180 degrees, and may be an angle smaller than 180 degrees, for example, 90 degrees.

It is a top view which shows the detection part in one Example roughly. It is a wave form diagram which shows the example of the resonance spectrum by a dielectric resonator. It is a wave form diagram which shows the change of the resonance spectrum by the presence or absence of a sample. It is a figure which shows the relationship between the molecular chain orientation of a sample, and the anisotropy of a dielectric constant. It is a block diagram which shows the present invention roughly. It is a schematic block diagram which shows one Example which rotates a dielectric resonator with respect to a sample. (A) is a waveform diagram showing the relationship between the transmitted microwave intensity and frequency in the dielectric resonator, and (B) is a waveform diagram showing changes due to the presence or absence of a sample. (A) is a figure which shows the Q curve with respect to the relative rotation angle position (S) of the sample with respect to a dielectric resonator, (B) is a figure which shows the state cut | disconnected by the specific frequency. (A) is a graph showing a cross section of FIG. 8 (B), (B) is a graph displaying it in a polar coordinate system. It is a graph which shows the orientation pattern which displayed the frequency shift amount obtained by rotating a dielectric resonator by a polar coordinate system. It is a block diagram which shows the electric signal processing system in an Example. It is a block diagram showing an example of an electric signal processing system including a rotation mechanism. It is a block diagram which shows the other example of the electric signal processing system containing a rotation mechanism. It is a time chart which sweeps a predetermined frequency range with a microwave sweep oscillator. It is a flowchart which shows the measuring method of the resonant frequency shift amount by a sample. It is a figure which shows the angle of the dielectric resonator with respect to MD direction of a sample. It is a flowchart which shows the method of calculating an orientation pattern for every rotation period of the dielectric resonator with respect to a sample. It is a graph which shows the data (DELTA) f obtained by 1 rotation, displaying in polar coordinates. It is a flowchart figure which shows generally the case where an orientation pattern is calculated for every rotation period of the dielectric resonator with respect to a sample. It is a figure which shows the relative angle of the dielectric resonator with respect to MD direction of a sample. And Δf at 0 ° <A _n <360 °, is a graph showing by polar coordinates data A _n +180 degrees interpolated using them. It is a top view which shows the Example which swings a dielectric resonator for every 180 degree | times on the basis of the center of a dielectric resonator with respect to MD direction of a sample. It is a flowchart which shows the method of calculating an orientation pattern for every swing period of the dielectric resonator with respect to a sample. It is a graph which shows ₍ DELTA) f in 0 degree < _An <180 degree | times, and the data of _An + 180 degree | times which were interpolated using them are displayed as a polar coordinate. It is a figure which shows the state which returns after the mth data acquisition so that the angle of the dielectric resonator with respect to the sample MD direction at the time of the m + 1th time sweep start may correspond with that at the time of the mth time sweep end. It is a figure which shows the method of returning after the mth data acquisition so that the angle of the dielectric resonator with respect to the sample MD direction at the time of the m + 1th sweep start may coincide with that at the end of the mth sweep. It is a figure which shows the relative angle of the sweep area in multiple swings.

Explanation of symbols

2 Microwave Antenna 4 Dielectric Resonator 4a Sample Measurement Surface of Dielectric Resonator 6 Detection Antenna 8 Shield Case 12 Oscillator 14 Detector 16 Controller 18 Computer 20 Slip Ring

Claims (8)

One dielectric resonator having a measurement plane approaching or contacting the sample and disposed only on one side of the sample, and a shield case made of a conductive material that substantially covers the dielectric resonator except for the measurement plane An excitation antenna that is arranged inside the shield case and generates an electric field vector having a unidirectional component in the dielectric resonator, and detects transmitted energy or reflected energy by the dielectric resonator arranged inside the shield case A detection unit comprising a detection antenna that performs
An oscillation unit that is electrically connected to the excitation antenna to supply a microwave signal and repeatedly sweeps the frequency of the microwave signal;
A detection unit including an amplification circuit that amplifies the detected signal electrically connected to the detection antenna;
A rotation mechanism that rotates or rotates the detection unit, the oscillation unit, and the detection unit as a unit within the measurement plane;
While being connected to the oscillating unit and the detection unit and repeating the frequency sweep by the sweep unit during rotation or rotation by the rotation mechanism, the resonance frequency in each frequency sweep is detected from the output of the detection unit, and A control / calculation unit for obtaining the dielectric anisotropy of the sample from the correspondence between the rotation angle of the detection unit and the resonance frequency;
An orientation measuring apparatus comprising: The rotating mechanism includes a fixed terminal and a rotating terminal that contact each other and maintain electrical connection;
The rotation terminal is electrically connected to the oscillation unit and the detection unit, and the fixed terminal is electrically connected to the control / calculation unit,
The rotation mechanism rotates the rotation terminal in one direction together with the detection unit, the oscillation unit, and the detection unit,
The orientation measuring apparatus according to claim 1, wherein the control / calculation unit controls a rotation speed or a sweep time so that a rotation angle of a detection unit that performs frequency sweeping matches in each rotation.   The orientation measuring apparatus according to claim 2, wherein the control / calculation unit interpolates data of a detection unit rotation angle position that is point-symmetric with respect to the rotation center based on data at the detection unit rotation angle that has been subjected to frequency sweep. The rotation mechanism is a rotation mechanism that repeatedly rotates in a reciprocating direction,
The control / arithmetic unit controls the rotation speed or sweep time so that the rotation angle of the detection unit that performs frequency sweeping coincides in each rotation, and the data of the detection unit rotation angle region that does not rotate is the rotation center. The orientation measuring apparatus according to claim 1, wherein interpolation is performed using data at a rotational angle position of a point-symmetric detection unit with respect to. The rotating mechanism includes a fixed terminal and a rotating terminal that contact each other and maintain electrical connection;
The rotation terminal is electrically connected to the oscillation unit and the detection unit, and the fixed terminal is electrically connected to the control / calculation unit,
The orientation measuring apparatus according to claim 4, wherein the rotation mechanism rotates the rotation terminal together with the detection unit, the oscillation unit, and the detection unit.   The orientation measurement apparatus according to claim 4, wherein electrical connection between the control / calculation unit, the oscillation unit, and the detection unit is performed by a flexible cable. A sample supply mechanism for running the sample while maintaining the sheet-like sample so that one surface thereof is close to or in contact with the measurement plane of the dielectric resonator;
The orientation measuring apparatus according to any one of claims 1 to 6, wherein the orientation measuring apparatus is an on-line measuring apparatus that repeatedly measures the dielectric anisotropy of the sample with the orientation measuring apparatus while the sample is running. One dielectric resonator, a shield case made of a conductive material that substantially covers the dielectric resonator except for the measurement plane of the dielectric resonator, and the dielectric resonator disposed inside the shield case An excitation antenna that generates an electric field vector having a unidirectional component at the same time, and a detection unit that is disposed inside the shield case and detects a transmission energy or reflection energy by the dielectric resonator, and the excitation antenna. An oscillation unit that supplies an electrically connected microwave signal and repeatedly sweeps the frequency of the microwave signal, and a detection unit that includes an amplifier circuit that is electrically connected to the detection antenna and amplifies the detected signal. Use the measuring device provided,
The measurement plane of the dielectric resonator is disposed only on one side of the sample so as to approach or contact the sample,
The detection unit, the oscillation unit and the detection unit are integrally rotated or rotated in the measurement plane,
The frequency sweep by the sweep unit is repeated during rotation or rotation of the detection unit, and the resonance frequency in each frequency sweep is detected from the output of the detection unit, and the rotation angle and resonance frequency of the detection unit are Orientation measurement method for obtaining the dielectric anisotropy of a sample from the corresponding relationship.

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