JP2019078557A - Particulate dispersed elastomer separation measuring device and separation measurement method - Google Patents

Abstract

A fine particle-dispersed elastomer capable of measuring, during a tensile test, the state of minute delamination at the interface between a synthetic rubber-based material and fine particles of an oxidizing agent, which occurs when a tensile load is applied to a composite propellant filled in a motor case. To provide a peeling measuring device and a peeling measuring method. A tensioning mechanism (20) for applying a tensile load to a test piece (W), a transmission side probe (4) arranged in contact with a front surface (Ws) of the test piece (W), and a transmission-side probe (4) arranged in contact with a rear surface (Wb) of the test piece (W) to perform transmission super-transmission. The transmission intensity of the transmitted ultrasonic wave TS received by the receiving probe 6 that receives the sound wave and the transmission intensity of the transmitted ultrasonic wave TS received by the receiving probe 6 in a state where no tensile load is applied to the test piece W is provided as the reference intensity V0 for calibration. , comparing the transmission intensity V of the transmitted ultrasonic wave T received with a tensile load applied to the test piece W with the reference intensity V0, and the average of the attenuation rate and peeling of the ultrasonic wave at the time of load application obtained by this comparison A calculation unit 12 is provided for measuring the state of minute flaking Wh at the interface between the synthetic rubber-based material Wg and the oxidizing agent Wm from the relationship with the length. [Selection drawing] Fig. 1

Description

  The present invention relates to a fine particle used for observing the distribution of separation (including cracks) generated at the interface between the elastomer substrate and the fine particles when conducting a tensile test of the fine particle dispersed elastomer in which the fine particles are dispersed in the elastomer substrate. The present invention relates to a peeling measurement device and a peeling measurement method of a dispersed elastomer.

  As the above-mentioned fine particle dispersed elastomer, for example, there is a composite propellant filled in the motor case of a solid rocket motor, and this composite propellant is an oxidizing agent (fine particles) in a synthetic rubber material (elastomer base material) such as polybutadiene. And metal powders such as aluminum).

  In a composite propellant in which an oxidizing agent and a metal powder are dispersed in such a synthetic rubber material, for example, when the molded product is accommodated in a motor case, the molded product may be deformed or cracked if the structural strength is not maintained. It will occur. Also, if the compounding ratio of the synthetic rubber material, which is the raw material, to the oxidizing agent or metal powder to be mixed with it is different, or if the degree of mixing is poor, the mechanical properties will deteriorate, so molding Each time, it is necessary to grasp the mechanical properties.

  Conventionally, for example, in the case of observing the distribution of minute peeling that occurs at the interface between a synthetic rubber material and fine particles of an oxidizing agent when a tensile load is applied, a cross section is prepared by collecting from a composite propellant. The test piece is subjected to a tensile testing machine to optically observe the cross section of the test piece at this time.

  Although the above-described micro-debonding detection method can detect micro-debonding at the interface between the synthetic rubber material and the oxidizing agent that appears in the cross section of the prepared test piece, the micro-debonding distribution in the inside of the test piece can be detected. Can not grasp.

  Heretofore, as a means for detecting the peeling occurring inside such a test piece, for example, the ultrasonic peeling detection method described in Patent Document 1 is known.

  The ultrasonic peeling detection method is a method of detecting peeling of the coating material applied to the surface of the pipe to the pipe. In this ultrasonic peeling detection method, an ultrasonic probe is disposed in contact with the coating material, and ultrasonic waves are transmitted from the ultrasonic probe toward the coating material and piping.

  Then, a reflection echo reflected by the pipe is received by the ultrasonic probe, and the peeling of the coating material from the pipe is detected based on the magnitude of the detection signal corresponding to the received reflection echo.

JP, 2013-108824, A

  However, in the ultrasonic peeling detection method as described above, for example, when it is used to measure the state of micro peeling at the interface between the synthetic rubber material and the oxidizing agent produced by applying a tensile load to the composite propellant, the tensile test is underway. There is a problem that the distribution of microdetachment at the interface between the synthetic rubber material and the oxidizing agent occurring in the above can not be measured in real time, and it is a conventional problem to solve this.

  The present invention has been made focusing on the above-described conventional problems, and, for example, a synthetic rubber-based material produced by applying a tensile load to a composite propellant filled in a motor case and an oxidant which is a fine particle An object of the present invention is to provide a peeling measurement apparatus and a peeling measuring method of a fine particle dispersed elastomer which can measure the state of micro peeling at an interface in real time during a tensile test.

  According to a first aspect of the present invention, there is provided a peeling measurement device for a fine particle dispersed elastomeric material, which measures the state of peeling occurring at the interface between the elastomer substrate and the fine particles when a tensile load is applied to the fine particle dispersed elastomeric material. A tensile mechanism for applying a tensile load to the fine particle dispersed elastomeric material, and a transmitting probe which is disposed in contact with the surface along the direction of the tensile load applied by the tensile mechanism of the fine particle dispersed elastomeric material to transmit ultrasonic waves An ultrasonic wave reflected from the back surface of the fine particle dispersed elastomer material transmitted from the transmitting probe and disposed on or in contact with the front surface of the fine particle dispersed elastomer material or the back surface opposite to the front surface; A receiving side probe for receiving transmitted ultrasonic waves transmitted through a fine particle dispersed elastomeric material, and the fine particle dispersed elastomeric material The transmission intensity of the reflected ultrasonic wave transmitted by the transmission side probe and received by the reception side probe or the transmission intensity of the transmission ultrasonic wave when no tensile load is applied by the tension mechanism. As a reference strength for calibration, and in a state where the fine particle dispersed elastomer material is loaded with a tensile load by the tensile mechanism, an ultrasonic wave is transmitted from the transmitting probe and received by the receiving probe. The reflection intensity of the reflection ultrasonic waves or the transmission intensity of the transmission ultrasonic waves is compared with the reference intensity, and occurs at the interface between the elastomer substrate and the fine particles based on the attenuation rate under load obtained by the comparison. The configuration is provided with an operation unit that measures the state of peeling.

  According to a second aspect of the present invention, the ultrasonic wave transmitted from the transmission side probe is an ultrasonic wave of a frequency sweep waveform.

  According to a third aspect of the present invention, the transmitter probe also serves as the receiver probe.

  On the other hand, the fourth aspect of the present invention is a peeling measurement method of the fine particle dispersed elastomeric material for measuring the state of peeling occurring at the interface between the elastomer substrate and the fine particles when a tensile load is applied to the fine particle dispersed elastomeric material The transmitter-side probe is disposed in contact with the surface along the load load direction of the particulate-dispersed elastomeric material, and the receiver-side probe is disposed in contact with the front surface or the back surface opposite to the surface. The reflection intensity of the reflected ultrasonic wave reflected by the back surface of the fine particle dispersed elastomer material transmitted by the transmission side probe and received by the reception side probe in a state where no tensile load is applied to the elastomer material Alternatively, after the transmission intensity of the transmitted ultrasonic wave that has passed through the fine particle dispersed elastomer material is obtained as a reference strength for calibration, the fine particle dispersed elastomer is Reference is made to the reflection intensity of the reflected ultrasonic waves or the transmission intensity of the transmitted ultrasonic waves received by the receiving side probe by transmitting the ultrasonic waves from the transmitting side probe in a state where the material is loaded with a tensile load. The configuration is such that the state of peeling occurring at the interface between the elastomer base and the fine particles is measured based on the damping rate under load load obtained by the comparison as compared with the strength.

  In the peeling measurement device and the peeling measurement method of the fine particle dispersed elastomer material according to the present invention, for example, the synthetic rubber material and fine particles generated by applying a tensile load during the tensile test on the composite propellant filled in the motor case The very excellent effect that it is possible to measure the state of microdetachment in the interface with a certain oxidizing agent in real time is brought about.

BRIEF DESCRIPTION OF THE DRAWINGS It is front explanatory drawing which shows roughly one Embodiment of the peeling measurement apparatus of the microparticles | fine-particles dispersion | distribution elastomeric material which concerns on this invention. It is plane | planar explanatory drawing of the test piece part in the peeling measurement apparatus of the microparticles | fine-particles dispersion | distribution elastomeric material shown in FIG. FIG. 6 is a partially enlarged explanatory view showing a test piece in a state in which no tensile load is applied in the peeling measurement device for the fine particle dispersed elastomer material shown in FIG. 1. It is a partially expanded explanatory view which shows the test piece of the state which applied the tensile load in the peeling measurement apparatus of the microparticles | fine-particles dispersion | distribution elastomeric material shown in FIG. When the ultrasonic wave is transmitted from the transmitting probe in the state shown in FIG. 3 in which the tensile load is not loaded on the test piece, the tensile load is applied to the transmitted ultrasonic waveform diagram (a) acquired as the calibration waveform and the test piece It is a wave form diagram (b) of a transmitted ultrasonic wave acquired when transmitting an ultrasonic wave from a sending side probe in the state shown in Drawing 4 loaded. It is a graph which shows the relationship between the attenuation factor of the ultrasonic wave at the time of load loading obtained by comparing each transmitted intensity based on the waveform chart of Fig.5 (a) and the waveform chart of FIG.5 (b), and the average length of peeling. . It is the elements on larger scale which show other embodiment of the peeling measurement apparatus of the microparticles | fine-particles dispersion | distribution elastomeric material which concerns on this invention.

Hereinafter, a peeling measurement device and a peeling measurement method of the fine particle dispersed elastomer material according to the present invention will be described based on the drawings.
FIGS. 1 to 6 are views for explaining the peeling measurement device and the peeling measurement method of the fine particle dispersed elastomer material according to the embodiment of the present invention, and in this embodiment, the fine particle dispersed elastomer material is a motor case of a solid rocket motor. The case of the composite propellant to be filled in will be described as an example.

  The composite propellant is formed by kneading an oxidizing agent (fine particles) and a metal powder such as aluminum into a synthetic rubber material (elastomer base material) such as polybutadiene, and the like, and the peeling measurement of the fine particle dispersed elastomer material according to this embodiment. In the apparatus, when a tensile load is applied to the composite propellant, the state of peeling occurring at the interface between the synthetic rubber material and the oxidizing agent which is fine particles is measured.

  As shown in FIG. 1, this fine particle dispersed elastomer material peel measurement apparatus 1 comprises a pulse generator 2, a transmitter probe 4, a receiver probe 6, a pulse receiver 8, and analog / digital conversion. Device (hereinafter referred to as an A / D converter) 10, a computing unit 12, a monitor 14, and a tension mechanism 20 for applying a tensile load to the test piece W of the composite propellant.

  The transmitting side probe 4 is disposed on the surface Ws of the test piece W of the composite propellant formed in a flat plate shape via a contact medium such as jelly, and the frequency sweeping ultrasonic wave generated by the pulse generator 2 (Burst wave of frequency sweep waveform) is made to be incident on the test piece W. The ultrasonic wave generated by the pulse generator 2 may be a constant frequency ultrasonic wave (a burst wave of a constant frequency waveform).

  On the other hand, the receiving side probe 6 is disposed on the back surface Wb opposite to the front surface Ws of the test piece W via a contact medium such as jelly similarly to the transmitting side probe 4, and from the transmitting side probe 4 The transmitted ultrasonic waves transmitted through the test strip W of the transmitted frequency sweep ultrasonic waves are received.

  The tension mechanism 20 includes a pair of clamps 21 and 21 sandwiching both ends Wa and Wa of the test piece W from both the front surface Ws and the back surface Wb, and a clamp driving unit (not shown) operating the clamps 21 and 21. There is. The tension mechanism 20 operates the pair of clamps 21, 21 holding the both ends Wa, Wa of the test strip W in a direction (a white arrow direction in FIG. 1) separated from each other by the clamp drive unit. Apply tensile load.

  The transmitting probe 4 and the receiving probe 6 disposed in contact with the front surface Ws and the back surface Wb along the direction of the tensile load in the test piece W are probed as shown in FIG. 2 in this embodiment. The child holding frame 16 and the elastic body 18 hold the front surface Ws and the rear surface Wb of the test piece W in a pressed state.

  The calculation unit 12 acquires the transmission intensity of the transmission ultrasonic wave received by the reception side probe 6 when transmitting the frequency sweep ultrasonic wave from the transmission side probe 4 to the test strip W.

In this case, the calculation unit 12 includes a waveform recording unit 12A and a calibration unit 12B.
The waveform recording means 12A uses the transmission intensity of the transmission ultrasonic wave as the reference intensity V ₀ for calibration based on the waveform of the transmission ultrasonic wave acquired in the state shown in FIG. 3 in which no tensile load is loaded on the test piece W. To record.

On the other hand, the calibration means 12B is a reference for calibration of the transmission intensity V based on the waveform of the transmission ultrasonic wave T acquired in the state shown in FIG. 4 in which the tensile load is loaded on the test piece W. The damping factor ((V ₀ −V) / V ₀ (%)) under load is calculated as compared with the strength V ₀ . Then, as also shown in the enlarged circle in FIG. 4, the state of the peeling Wh generated at the interface between the synthetic rubber material (elastomer base material) Wg of the test piece W and the oxidizing agent Wm which is fine particles is measured.

Next, a description will be given of the manner of measurement of peeling of the fine particle dispersed elastomer material according to the present embodiment by the peeling measurement device 1.
First, as shown in FIG. 1, the transmitting probe 4 and the receiving probe 6 are disposed in contact with the front surface Ws and the back surface Wb of the test piece W of the composite propellant formed in a flat plate shape.
At this time, as shown in FIG. 2, the transmission probe 4 and the reception probe 6 are pressed against the front surface Ws and the rear surface Wb of the test piece W by the probe holding frame 16 and the elastic body 18 respectively. Hold on.

Next, a frequency sweeping ultrasonic wave is transmitted from the transmission side probe 4 in a state where no tensile load is applied to the test piece W by the tensile mechanism 20, and at this time, the test piece W received by the reception side probe 6 is transmitted. based on the waveform shown in FIG. 5 (a) of the attenuated transmitted ultrasonic TS Te, as a reference intensity V ₀ which for calibrating the transmission intensity of the transmitted ultrasonic TS, is recorded in the waveform recording unit 12A of the arithmetic unit 12.

  After that, the frequency sweeping ultrasonic wave is transmitted from the transmission side probe 4 while applying a tensile load by the tensile mechanism 20 to the test piece W, and at this time, it passes through the test piece W received by the reception side probe 6 The waveform shown in FIG. 5 (b) of the attenuated transmission ultrasonic wave T is acquired.

Then, based on the waveform shown in FIG. 5 (b) of the reference force V ₀ for calibration shown in FIG. 5 (a) and included in the waveform recording means 12A in the calibration means 12B of the operation unit 12 A comparison with the transmission intensity V is made, and as shown in FIG. 6, the average attenuation length ((V ₀ −V) / V ₀ (%)) of ultrasonic wave under load and the average length of peeling obtained in this comparison From the relationship with (μm), the distribution state of the peeling Wh generated at the interface between the synthetic rubber material Wg of the test piece W and the oxidizing agent Wm as fine particles is measured.

In the peeling measurement apparatus 1 and the peeling measurement method of the fine particle dispersed elastomer material according to this embodiment, the ultrasonic wave transmitted through the test strip W is received during the tensile test on the test strip W of the composite propellant filled in the motor case. Then, the transmitted intensity V based on the waveform of the transmitted ultrasonic wave is compared with the reference intensity V ₀ for calibration acquired in advance (the transmitted intensity based on the waveform of the transmitted ultrasonic wave in a state where no tensile load is applied to the test piece W) Since the attenuation factor of the ultrasonic wave at the time of loading is obtained, the distribution of micro peeling Wh at the interface between the synthetic rubber material Wg and the oxidizing agent Wm which is a fine particle caused by the application of tensile load is real time Can be measured by

  Further, in the peeling measurement apparatus 1 and the peeling measurement method of the fine particle dispersed elastomer material according to this embodiment, since the ultrasonic wave of the frequency sweep waveform is adopted as the ultrasonic wave transmitted from the transmission side probe 4, that is, Since the attenuation characteristics of ultrasonic waves are used, it becomes easy to measure the distribution of the minute peeling Wh.

  In the above-described embodiment, the transmission side probe 4 is disposed on the surface Ws of the test piece W of the composite propellant, and frequency sweeping ultrasonic waves are made to enter the test piece W, and the transmitted ultrasonic waves transmitted through the test piece W are tested. Although it is made to receive with the receiving side probe 6 arrange | positioned on the back surface Wb of the piece W, it is not limited to this, As shown in FIG. 7, the transmitting side which doubles as a receiving side probe The probe 4A may be employed.

  In this case, the frequency sweeping ultrasonic wave is made to enter into the test piece W from the transmission side probe 4A disposed on the surface Ws of the test piece W of the composite propellant, and the reflection of the frequency sweeping ultrasonic wave on the test piece W The ultrasonic wave is to be received by the transmitting probe 4A.

  On the basis of the waveform of the reflected ultrasonic wave (corresponding to the waveform of the transmitted ultrasonic wave TS shown in FIG. 5A) reflected by the back surface Wb of the test piece W received by the transmission side probe 4A, After the reflection intensity is acquired as a reference strength for calibration, a frequency sweep ultrasonic wave is transmitted from the transmission side probe 4A while applying a tensile load by the tensile mechanism 20 to the test piece W, and at this time, the transmission side probe The reflection intensity of the reflected ultrasonic wave acquired based on the waveform of the reflected ultrasonic wave (corresponding to the waveform of the transmitted ultrasonic wave T shown in FIG. 5B) received by the probe 4A at the test strip W is compared with the reference intensity Do.

  And based on the attenuation factor at the time of load loading obtained by this comparison, distribution state of exfoliation Wh which arises in an interface of synthetic rubber material Wg of test piece W and oxidizing agent Wm which is particulates is measured.

  As described above, also in the case where the transmitting probe 4A that doubles as the receiving probe is adopted and the transmitting probe 4A receives the reflected ultrasonic wave of the frequency-swept ultrasonic wave at the test strip W It is possible to measure in real time the distribution state of the minute peeling Wh at the interface between the synthetic rubber material Wg and the oxidizing agent Wm which is a fine particle, which is generated when a tensile load is applied.

  Further, in the above-described embodiment, although the case where the fine particle dispersed elastomeric material is a composite propellant filled in the motor case of a solid rocket motor has been described as an example, it is not limited thereto.

  The configurations of the peeling measurement device and the peeling measurement method of the fine particle dispersed elastomer material according to the present invention are not limited to the above embodiments.

1 Peeling Measurement Device for Particulate-Dispersed Elastomer Material 4 Transmitter Probe 6 Receiver Probe 12 Arithmetic Unit 12A Waveform Recording Means (Operator)
12B Calibration means (calculation unit)
20 tensioning mechanism T, TS transmitted ultrasonic _{V 0} transmitted intensity W specimens Wb backside Wg synthetic rubber material during the reference intensity V load for load calibration (elastomeric substrate)
Wh Release Wm Oxidizer (fine particles)
Ws surface

Claims (4)

A particulate measurement device for a particulate dispersed elastomeric material, which measures the state of the particulate which is generated at the interface between the elastomeric substrate and the particulate when a particulate load is applied to the particulate elastomeric material,
A tensile mechanism for applying a tensile load to the particulate dispersed elastomeric material;
A transmitting probe which is disposed in contact with the surface of the fine particle dispersed elastomeric material along the direction of the tensile load applied by the tensile mechanism to transmit ultrasonic waves;
Reflected ultrasonic waves or fine particles reflected on the back surface of the fine particle dispersed elastomeric material of the ultrasonic wave transmitted from the transmitting probe and arranged in contact with the front surface of the fine particle dispersed elastomeric material or the back surface facing the front surface A receiving probe for receiving the transmitted ultrasonic wave transmitted through the dispersed elastomeric material;
The reflection intensity or the transmission of the reflected ultrasonic wave transmitted from the transmitting probe and received by the receiving probe in a state where the tensile load by the pulling mechanism is not applied to the fine particle dispersed elastomer material An ultrasonic wave is transmitted from the transmission side probe in a state in which the transmission strength of ultrasonic waves is used as a reference strength for calibration and the tensile load by the tensile mechanism is applied to the fine particle dispersed elastomer material, and the reception side probe is transmitted. Comparing the reflection intensity of the reflected ultrasonic wave received by the child or the transmission intensity of the transmission ultrasonic wave with the reference intensity, the elastomer base material and the fine particles based on the attenuation factor at load given by the comparison Peeling measurement device of fine particle dispersed elastomer material provided with operation part which measures the state of the peeling which arises in the interface with.   The apparatus according to claim 1, wherein the ultrasonic wave transmitted from the transmission side probe is an ultrasonic wave of a frequency sweep waveform.   The peeling measurement apparatus of the fine particle dispersed elastomer material according to claim 1 or 2, wherein the transmission side probe doubles as the reception side probe. A method for measuring the peeling of a particulate dispersed elastomeric material, which measures the state of peeling that occurs at the interface between the elastomeric substrate and the particulate when a tensile load is applied to the particulate dispersed elastomeric material,
The transmitter probe is disposed in contact with the surface of the fine particle dispersed elastomer material along the direction in which the tensile load is applied, and the receiver probe is disposed in contact with the front surface or the back surface opposite to the surface.
Reflected ultrasonic waves reflected on the back surface of the fine particle dispersed elastomer material transmitted by the transmitting probe and received by the receiving probe in a state where no tensile load is applied to the fine particle dispersed elastomer material After acquiring the reflection intensity of the above or the transmission intensity of the transmitted ultrasonic wave that has passed through the fine particle dispersed elastomer material as a reference intensity for calibration,
In a state where a tensile load is applied to the fine particle dispersed elastomer material, an ultrasonic wave is transmitted from the transmission side probe and a reflection intensity of the reflection ultrasonic wave received by the reception side probe or a transmission of the transmission ultrasonic wave A method of measuring peeling of a particulate dispersed elastomeric material, comparing strength with the reference strength, and measuring the state of peeling occurring at the interface between the elastomer base and the fine particles based on the damping rate under load obtained by the comparison .

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