Device and method for preparing microbead debonding sample

Abstract

The invention discloses a device and a method for preparing a microbead debonding sample. The device comprises a bracket, a rotary sample loading device, a plurality of samples, an extrusion device and a feeding and discharging device. The rotary sample loading device is rotatably arranged on the support, the multiple samples are distributed at intervals in the circumferential direction of the rotary sample loading device, the extrusion device is located above the rotary sample loading device and used for containing a prefabricated resin solution, and the feeding and discharging device is connected with the extrusion device and used for adjusting the air pressure in the extrusion device. The feeding and discharging device is matched with the extrusion device to enable the prefabricated resin solution in the extrusion device to enter and exit from the extrusion device and remove bubbles in the prefabricated resin solution in the extrusion device, and the feeding and discharging device is matched with the rotary sample loading device to enable the prefabricated resin solution extruded from the liquid outlet end of the extrusion device to be transferred to fiber monofilaments of a sample located below the extrusion device. Through cooperation of the rotary sample loading device, the feeding and discharging device and the extrusion device, high-efficiency and high-quality sample preparation can be completed.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of composite material testing, in particular to a microsphere debonding sample preparation device and method. BACKGROUND

[0002] In carbon fiber reinforced resin composites, the effective bonding between carbon fibers and resin matrix is the guarantee for the excellent performance of the composite material. The interfacial bonding strength is related to the surface morphology structure of the fiber and the matrix, and the interfacial layer formed between the two will also have an important influence, thereby further affecting the performance of the composite material, therefore, it is necessary to use effective characterization means to determine the interfacial bonding strength of the composite material.

[0003] The microsphere debonding test method is a commonly used method for interfacial debonding strength, which has been maturely used for evaluating the interfacial debonding strength of thermosetting resin and fiber, but the interfacial debonding strength value of the composite material tested by the microsphere debonding method has a large fluctuation and error, which is greatly related to the resin microspheres on the fiber single wire. The traditional manual sample preparation method is too slow for some resins with fast curing speed, resulting in that the resin inside has begun to react but the sample preparation has not been completed, and the manual single sample preparation cannot control the size of the resin microspheres on the fiber, which is difficult to meet the testing requirements in the experiment, and there is an urgent need for a sample preparation device and method that can meet the experimental requirements and be efficiently prepared. SUMMARY

[0004] In order to overcome the problems in the related art, the present application provides a microsphere debonding sample preparation device and method.

[0005] According to the embodiments of the present application, a microsphere debonding sample preparation device is provided, comprising: a support; a rotating sample loading device, which is rotatably arranged on the support; a plurality of samples, which are detachably arranged on the rotating sample loading device, the plurality of samples are distributed along the circumferential direction of the rotating sample loading device, and the fiber single wires on each sample paperboard on the rotating sample loading device are parallel to the extension direction of the fiber single wires; an extrusion device, which is arranged on the support and located above the rotating sample loading device, the extrusion device is used for containing a pre-prepared resin solution, and the bottom of the extrusion device is provided with a plurality of liquid outlets, which are distributed along the extension direction of the fiber single wires on the rotating sample loading device; An inlet and outlet device connected to the extrusion device, the inlet and outlet device being used to adjust the air pressure in the extrusion device so that the pre-made resin solution in the extrusion device can be transferred in and out of the extrusion device and remove the air bubbles in the pre-made resin solution in the extrusion device, the inlet and outlet device cooperating with the rotary sample loading device so that the pre-made resin solution extruded from the liquid outlet end can be transferred to the fiber filaments located below the extrusion device.

[0006] In some embodiments, the extrusion device comprises: A containing tank fixed to the support frame; A plurality of extrusion needles arranged at the bottom of the containing tank and in communication with the containing tank, and the plurality of extrusion needles are spaced apart along the direction of extension of the fiber filaments, the end of the extrusion needles away from the containing tank constituting the liquid outlet end; A plurality of needle caps corresponding to the plurality of extrusion needles, the needle caps being detachably arranged on the end of the corresponding extrusion needles away from the containing tank.

[0007] In some embodiments, the inlet and outlet device comprises: An inlet pipe, the first end of the inlet pipe being in communication with the containing tank, the inlet pipe being used to transport the pre-made resin solution to the containing tank; A liquid storage part arranged on the support frame and in communication with the second end of the inlet pipe, the liquid storage part being used to store the pre-made resin solution; An air pipe, the first end of the air pipe being in communication with the top of the containing tank; A gas delivery device in communication with the second end of the air pipe, the gas delivery device being used to adjust the air pressure in the extrusion device through the air pipe.

[0008] In some embodiments, the inlet and outlet device further comprises: A first valve arranged on the inlet pipe; A second valve arranged on the air pipe.

[0009] In some embodiments, the microbead debonding sample preparation device further comprises: An air pressure detection part, the air pressure detection part being used to detect the air pressure of the containing tank.

[0010] In some embodiments, the rotary sample loading device comprises: A rotating shaft, both ends of the rotating shaft being rotatably connected to the support frame; At least two discs are arranged on the rotating shaft, the at least two discs are arranged along the axial direction of the rotating shaft, the radial direction of each disc is perpendicular to the axial direction of the rotating shaft, and a plurality of clamping grooves are arranged on the outer circumferential surface of the disc, and the plurality of clamping grooves on at least adjacent discs correspond one by one, and the sample paperboard is fixed in the corresponding at least two clamping grooves. A driving part is connected to one of the two ends of the rotating shaft, and the driving part is used for driving the rotating shaft to rotate.

[0011] In some embodiments, the sample paperboard is provided with a groove, the fiber monofilament is located in the groove, and the two ends of the fiber monofilament are fixed to the opposite two groove side walls of the groove.

[0012] The second aspect of the present application also provides a preparation method of a microbead debonding sample, which is prepared by using a microbead debonding sample preparation device, and the preparation method comprises the following steps: S1, preparing a pre-prepared resin solution and a plurality of samples, the samples comprising sample paperboards and fiber monofilaments arranged on the sample paperboards, and assembling the plurality of samples on a rotating sample loading device; S2, forming a negative pressure state in a containing tank of an extrusion device by using an inlet and outlet device, the negative pressure state being capable of transporting the pre-prepared resin solution into the containing tank, and continuously maintaining the negative pressure state in the containing tank by using the inlet and outlet device to remove air bubbles in the pre-prepared resin solution; S3, injecting gas into the containing tank by using the inlet and outlet device to extrude the pre-prepared resin solution in the containing tank from a plurality of liquid outlet ends at the bottom of the containing tank, and forming resin droplets at the liquid outlet ends from the pre-prepared resin solution extruded from the liquid outlet ends; S4, rotating the rotating sample loading device to make the fiber monofilaments of the plurality of samples pass through the bottom of the containing tank in sequence, so that a plurality of resin droplets are transferred to the fiber monofilaments to form a plurality of resin microbeads, and an intermediate sample is obtained; S5, performing a solidification and cooling treatment on the intermediate sample to obtain a microbead debonding sample.

[0013] In some embodiments, the inlet and outlet device comprises an inlet pipe, a gas pipe, a liquid storage part, and a first valve arranged on the inlet pipe, one end of the inlet pipe is in communication with the containing tank, the other end of the inlet pipe is in communication with the liquid storage part, one end of the gas pipe is in communication with the top of the containing tank, the other end of the gas pipe is connected with a gas conveying device, and in step S2, The gas conveying device is used to form the negative pressure state in the containing tank, so that the prepared resin solution enters the containing tank through the feeding pipe, the first valve is closed, and the gas conveying device is used to continuously maintain the negative pressure state in the containing tank, so that the bubbles in the prepared resin solution in the containing tank are removed.

[0014] In some embodiments, in step S1, the resin liquid is mixed with the curing agent at a preset ratio to obtain a mixed solution, and after adjusting the solution viscosity of the mixed solution, the prepared resin solution is obtained. Preferably, the ratio between the resin liquid and the curing agent is 30:1 to 10:1, and the viscosity of the prepared resin solution is 80 to 150 mPa·s.

[0015] The technical solutions provided in the present application can have the following beneficial effects: By rotating the sample loading device, multiple samples can be hung with beads synchronously, and compared with the traditional manual sample preparation, the sample preparation time is greatly shortened, and the problem of early reaction of the resin with fast curing speed during sample preparation is avoided. The inlet and outlet devices can effectively remove the bubbles in the prepared resin solution in the extrusion device by adjusting the gas pressure in the extrusion device, so that the size of the extruded resin beads is uniform, which is beneficial to obtain effective test samples with good stability, thereby efficiently and high-quality completing sample preparation.

[0016] It should be understood that the above general description and the following detailed description are only exemplary and explanatory, and cannot limit the present application. BRIEF DESCRIPTION OF DRAWINGS

[0017] The accompanying drawings, which are incorporated into and form part of the specification, illustrate embodiments consistent with the present application and, together with the specification, serve to explain the principles of the present application.

[0018] Figure 1 is a front view of a microbead debonding sample preparation device according to an exemplary embodiment.

[0019] Figure 2 is a side view of a microbead debonding sample preparation device according to an exemplary embodiment.

[0020] Figure 3 is a schematic view of an extrusion device according to an exemplary embodiment.

[0021] Figure 4 is a schematic view of a sample according to an exemplary embodiment.

[0022] Figure 5 is a flowchart of a microbead debonding sample preparation method according to an exemplary embodiment.

[0023] Reference signs: 1, support; 2, rotating sample loading device; 21, rotating shaft; 22, disc; 23, driving part; 3, sample; 31, sample paperboard; 32, fiber filament; 33, groove; 34, mark; 4, extrusion device; 41, containing tank; 42, extrusion needle; 43, needle cap; 51, feeding tube; 52, liquid storage part; 53, gas tube; 54, gas delivery device; 55, first valve; 56, second valve; 6, air pressure detection part. DETAILED DESCRIPTION

[0024] In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be described clearly and completely below with reference to the drawings in the embodiments of the present application. Obviously, the described embodiments are only some of the embodiments of the present application, rather than all the embodiments of the present application. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative work fall within the protection scope of the present application. It should be noted that, in the case of no conflict, the embodiments in the present application and the features in the embodiments can be combined with each other at will.

[0025] The micro bead debonding test method has been maturely used for evaluating the interfacial debonding strength of thermosetting resin and fiber, but the interfacial debonding strength value of the composite material tested by the micro bead debonding method has great fluctuation and error, which has great relation with the resin micro bead on the fiber filament. The traditional manual sample preparation method is too slow for some resins with fast curing speed, which leads to that the resin inside has begun to react but the sample preparation has not been completed, and the manual single sample preparation cannot control the size of the resin micro bead on the fiber, and it is difficult to meet the testing requirements in the experiment, and there is an urgent need for a sample preparation device and method which can meet the experimental requirements and can be efficiently prepared.

[0026] To solve the technical problems in the related art, the present application provides a microsphere debonding sample preparation device, which comprises a support, a rotating sample loading device, a plurality of samples, an extrusion device and an in-out material device. The rotating sample loading device is rotatably arranged on the support, the plurality of samples are detachably arranged on the rotating sample loading device, and the plurality of samples are spaced apart along the circumferential direction of the rotating sample loading device. The sample comprises a sample paperboard and a fiber monofilament arranged on the sample paperboard. The extending directions of the fiber monofilaments on each sample paperboard located on the rotating sample loading device are parallel. The extrusion device is arranged on the support and located above the rotating sample loading device. The extrusion device is used to contain a pre-prepared resin solution. The bottom of the extrusion device is provided with a plurality of liquid outlets. The plurality of liquid outlets are spaced apart along the extending direction of the fiber monofilament located on the rotating sample loading device. The in-out material device is connected with the extrusion device. The in-out material device is used to adjust the air pressure in the extrusion device, so that the pre-prepared resin solution in the extrusion device can enter and exit the extrusion device, and the air bubbles in the pre-prepared resin solution in the extrusion device can be removed. The in-out material device cooperates with the rotating sample loading device, so that the pre-prepared resin solution extruded from the liquid outlet can be transferred to the fiber monofilament located below the extrusion device. The present application also provides a microsphere debonding sample preparation method, which is prepared by using the microsphere debonding sample preparation device. By using the rotating sample loading device, the present application realizes the synchronous bead hanging of the plurality of samples. In cooperation with the resin extrusion mode controlled by the air pressure, compared with the traditional manual sample preparation, the sample preparation time is greatly shortened, and the problem of early reaction of the resin with fast curing speed during the sample preparation process is avoided. By adjusting the air pressure in the extrusion device, the in-out material device can effectively remove the air bubbles in the pre-prepared resin solution in the extrusion device, so that the size of the extruded resin microspheres is uniform, which is beneficial to obtain an effective sample with good test stability, thereby efficiently and high-quality completing the sample preparation.

[0027] The microsphere debonding sample preparation device and method provided by the present application will be described in detail below with reference to the accompanying drawings.

[0028] An example embodiment of the present application provides a microsphere debonding sample preparation device, as shown in Figures 1-4As shown, the preparation device comprises a support 1, a rotating sample loading device 2, a plurality of samples 3, an extrusion device 4 and an in-out material device. The support 1 serves as the supporting base of the entire preparation device, and is used to mount and fix the rotating sample loading device 2, the extrusion device 4 and the in-out material device, so as to ensure the positional stability and relative accuracy of each component during the working process. The rotating sample loading device 2 is rotatably arranged on the support 1, and the plurality of samples 3 are detachably arranged on the rotating sample loading device 2 and are spaced apart along the circumference of the rotating sample loading device 2, so as to facilitate batch bead hanging operation. The sample 3 comprises a sample paperboard 31 and a fiber filament 32 arranged on the sample paperboard 31, and the extending directions of the fiber filaments 32 on each sample paperboard 31 located on the rotating sample loading device 2 are parallel, so as to ensure the consistency of the relative positions of the fiber filaments 32 and the liquid outlet of the extrusion device 4 during the bead hanging process. The extrusion device 4 is arranged on the support 1 and located above the rotating sample loading device 2, and is used to accommodate a pre-prepared resin solution. The bottom of the extrusion device 4 is provided with a plurality of liquid outlets, which are spaced apart along the extending direction of the fiber filaments 32 located on the rotating sample loading device 2, so that the microbeads are arranged on each fiber filament 32. The in-out material device is connected with the extrusion device 4, and is used to adjust the air pressure in the extrusion device 4, so that the pre-prepared resin solution in the extrusion device 4 can enter and exit the extrusion device 4, and the air bubbles in the pre-prepared resin solution in the extrusion device 4 can be removed. The in-out material device cooperates with the rotating sample loading device 2, so that the pre-prepared resin solution extruded from the liquid outlet can be transferred to the fiber filament 32 located below the extrusion device 4. The present application realizes the synchronous bead hanging of the plurality of samples 3 through the rotating sample loading device 2, and cooperates with the resin extrusion mode controlled by air pressure, so that the sample preparation time is greatly shortened compared with the traditional manual sample preparation, and the problem of early reaction of the resin with fast curing speed during the sample preparation process is avoided. The in-out material device can effectively remove the air bubbles in the pre-prepared resin solution in the extrusion device 4 by adjusting the air pressure in the extrusion device 4, so that the size of the extruded resin microbeads is uniform, which is beneficial to obtain effective samples with good test stability, so as to efficiently and high-quality complete the sample 3 preparation.

[0029] Referring to Figure 1 and Figure 2In some embodiments, the rotating loading device 2 comprises a rotating shaft 21, at least two discs 22 and a driving part 23. The two ends of the rotating shaft 21 are rotatably connected to the support 1 to provide support and transmission basis for the rotating movement. The discs 22 are arranged on the rotating shaft 21 and are spaced apart along the axial direction of the rotating shaft 21. The radial direction of each disc 22 is perpendicular to the axial direction of the rotating shaft 21. The outer circumferential surface of each disc 22 is provided with a plurality of clamping grooves, and the clamping grooves on at least two adjacent discs 22 correspond to each other. The sample paperboard 31 is fixed in the corresponding clamping grooves. The driving part 23 is connected to one of the two ends of the rotating shaft 21. The driving part 23 is used to drive the rotating shaft 21 to rotate, thereby driving the discs 22 and the sample 3 to rotate synchronously. The driving part 23 can adopt a knob structure to realize precise speed control by manual rotation, or can adopt a motor driving mode to further improve the degree of automation. In an exemplary embodiment, the discs 22 are two and are located at the two ends of the rotating shaft 21. The sample paperboard 31 is arranged between the two discs 22, which is conducive to ensuring batch bead hanging operation and forming continuous microbeads. The number of clamping grooves arranged on the two discs 22 is 4-10. The size of the clamping grooves is only for the sample paperboard 31 to pass through, so as to ensure the stable installation of the sample paperboard 31.

[0030] Referring to Figure 1 and Figure 4 In some embodiments, the sample paperboard 31 is provided with a groove 33, and the fiber monofilament 32 is located in the groove 33. The two ends of the fiber monofilament 32 are fixed to the two opposite groove side walls of the groove 33, respectively. In an exemplary embodiment, the two groove side walls are provided with a mark 34 at a position about 1 cm away from the groove opening. The two ends of the fiber monofilament 32 are fixed to the mark 34 through rosin, respectively, so as to ensure the consistency of the fixed position of each fiber monofilament 32, thereby ensuring the uniformity of the beads.

[0031] Referring to Figure 1 and Figure 3In some embodiments, the extrusion device 4 comprises a containing tank 41 fixed to the support 1 for storing the pre-prepared resin solution, a plurality of extrusion needles 42 arranged at the bottom of the containing tank 41 and in communication with the containing tank 41, and a plurality of needle caps 43 corresponding to the plurality of extrusion needles 42. The plurality of needle caps 43 are detachably arranged at the ends of the plurality of extrusion needles 42 away from the containing tank 41 for sealing the extrusion needles 42 in a non-working state to prevent the pre-prepared resin solution from being contaminated or solidified. The plurality of needle caps 43 can be fixedly connected side by side, so that when the needle caps 43 are removed in the working state, they do not need to be removed one by one, but can be removed at one time, saving time and effort. In an exemplary embodiment, the vertical distance between the extrusion needles 42 and the fiber filaments 32 on the rotating sample loading device 2 is set to 2 mm, ensuring that the fiber filaments 32 can just pass through the center of the resin droplets, thereby forming resin microbeads of uniform size on the fiber filaments 32.

[0032] Referring to Figure 1 and Figure 3 In some embodiments, the feeding and discharging device comprises a feeding pipe 51, a liquid storage part 52, a gas pipe 53, and a gas delivery device 54. The first end of the feeding pipe 51 is in communication with the containing tank 41, and the feeding pipe 51 is used to deliver the pre-prepared resin solution to the containing tank 41. The liquid storage part 52 is arranged on the support 1 and in communication with the second end of the feeding pipe 51. The liquid storage part 52 is used to store the pre-prepared resin solution, and can be a beaker or other container. The first end of the gas pipe 53 is in communication with the top of the containing tank 41, and the gas delivery device 54 is in communication with the second end of the gas pipe 53. The gas delivery device 54 is used to adjust the gas pressure in the extrusion device 4 through the gas pipe 53. The gas delivery device 54 is preferably a gas pump, which can extract the gas in the containing tank 41 to form a negative pressure in the tank, or can inject gas into the containing tank 41 to form a positive pressure in the tank, thereby achieving the function of adjusting the gas pressure. In this embodiment, a first valve 55 is arranged on the feeding pipe 51 to control the opening and closing of the feeding pipe 51, and a second valve 56 is arranged on the gas pipe 53 to control the opening and closing of the gas pipe 53. The height of the inlet end of the feeding pipe 51 is lower than the height of the inlet end of the gas pipe 53, and the inlet end of the gas pipe 53 is always above the liquid level of the containing tank 41, so as to avoid the pre-prepared resin solution in the containing tank 41 affecting the delivery and extraction of the gas.

[0033] Referring to Figure 1 and Figure 3In some embodiments, the microbead debonding sample preparation device further comprises a gas pressure detection unit 6, the detection end of which extends into the containing tank 41 for detecting the gas pressure of the containing tank 41. The gas pressure detection unit 6 is preferably a gas pressure monitoring table for detecting the gas pressure in the containing tank 41 in real time, facilitating the accurate control of the gas pressure adjustment process by the operator.

[0034] The present disclosure also provides a microbead debonding sample preparation method, as shown in the accompanying drawings, which is prepared by using the microbead debonding sample preparation device, and comprises the following steps: Figure 5 The present disclosure also provides a microbead debonding sample preparation method, as shown in the accompanying drawings, which is prepared by using the microbead debonding sample preparation device, and comprises the following steps: S1, preparing a pre-prepared resin solution and a plurality of samples, the samples comprising sample paperboards and fiber filaments arranged on the sample paperboards, and assembling the plurality of samples on the rotating sample loading device.

[0035] In this step, when preparing the pre-prepared resin solution, the resin liquid is mixed with the curing agent at a predetermined ratio to obtain a mixed solution, and after adjusting the solution viscosity of the mixed solution, the pre-prepared resin solution is obtained.

[0036] In the preparation of the sample 3, the fiber filament 32 is first fixed in the groove 33 of the sample paperboard 31 by rosin to form the sample 3 comprising the sample paperboard 31 and the fiber filament 32, and then a plurality of samples 3 are detachably installed in the clamping groove of the rotating sample loading device 2, ensuring that the fiber filaments 32 of the samples 3 are parallel to each other and correspond to the liquid outlet end of the extrusion device 4.

[0037] S2, forming a negative pressure state in the containing tank of the extrusion device by the feeding and discharging device, the negative pressure state being capable of transporting the pre-prepared resin solution into the containing tank, and continuously maintaining the negative pressure state in the containing tank by the feeding and discharging device to remove the gas bubbles in the pre-prepared resin solution.

[0038] In this step, a negative pressure state is formed in the containing tank 41 of the extrusion device 4 by the feeding and discharging device. Specifically, the first valve 55 on the feeding pipe 51 and the second valve 56 on the gas pipe 53 are opened, and the gas conveying equipment 54 is started to extract the gas in the containing tank 41, so that a negative pressure state is formed in the containing tank 41. Under the negative pressure state, the pre-prepared resin solution in the liquid storage part 52 is sucked into the containing tank 41 through the feeding pipe 51, and when the volume of the pre-prepared resin solution entering the containing tank 41 reaches 25-50% of the container capacity, the first valve 55 is closed. The gas conveying equipment 54 is kept running to continuously maintain the negative pressure state in the containing tank 41, so as to sufficiently remove the gas bubbles in the pre-prepared resin solution. The negative pressure maintenance time is preferably about 3 minutes to ensure complete removal of the gas bubbles.

[0039] S3, injecting gas into the containing tank through the inlet and outlet device to extrude the prefabricated resin solution in the containing tank from the multiple liquid outlet ends of the containing tank bottom, and forming resin droplets at the liquid outlet ends from the prefabricated resin solution extruded from the liquid outlet ends.

[0040] In this step, after the bubble removal is completed, the second valve 56 is closed, the air extraction operation of the gas delivery device 54 is stopped, and the containing tank 41 returns to normal pressure. The needle cap 43 on the extrusion needle 42 is removed, and the gas delivery device 54 is started again to inject gas into the containing tank 41 through the air pipe 53 to form a positive pressure in the containing tank 41. Under the action of the positive pressure, the prefabricated resin solution in the containing tank 41 is extruded from the liquid outlet ends of the multiple extrusion needles 42, and after forming tiny resin droplets at the liquid outlet ends, the air filling operation of the gas delivery device 54 is stopped.

[0041] S4, rotating the rotating sample loading device to make the multiple sample fiber filaments pass through the bottom of the containing tank in turn, so that the multiple resin droplets are transferred to the fiber filaments to form multiple resin microbeads, and a sample intermediate is obtained.

[0042] In this step, the rotating shaft 21 of the rotating sample loading device 2 is uniformly rotated by the driving part 23 to drive the disc 22 and the sample 3 to rotate synchronously. During the rotation of the sample 3, the fiber filaments 32 of each sample 3 pass through the liquid outlet ends of the containing tank 41 bottom in turn, the fiber filaments 32 sweep through the resin droplets, and the resin droplets are transferred to the fiber filaments 32 to form multiple equidistantly distributed resin microbeads. The rotating sample loading device 2 is continuously rotated until the fiber filaments 32 of all samples 3 complete the bead hanging operation, and a sample intermediate is obtained.

[0043] S5, performing solidification and cooling treatment on the sample intermediate to obtain a microbead debonding test sample.

[0044] In this step, the sample intermediate is subjected to solidification and cooling treatment to obtain a microbead debonding test sample. Specifically, the sample intermediate after completing the bead hanging is removed and placed in a vacuum oven for solidification treatment. The solidification temperature is preferably about 120°C, and the solidification time is preferably about 60 minutes. After solidification is completed, the test sample is cooled to room temperature, and then taken out for subsequent microbead debonding test.

[0045] In this embodiment, batch bead hanging of multiple samples can be realized by the rotating sample loading device. Compared with traditional manual single sample preparation, the sample preparation time is greatly shortened, and the problem of affecting the accuracy of test data due to changes in resin inside caused by long sample preparation process is avoided, which is especially suitable for sample preparation of resin with fast curing speed. By precisely controlling the viscosity of the prefabricated resin solution, the ratio of resin to curing agent and other parameters, and combining with the negative pressure bubble removal operation, the size of the prepared resin microbeads is uniform, the spacing is consistent, and the stability and reliability of the test data are improved.

[0046] In some embodiments, the feeding and discharging device comprises a feeding pipe, a gas pipe, a liquid storage part, and a first valve arranged on the feeding pipe, one end of the feeding pipe is communicated with the containing tank, the other end of the feeding pipe is communicated with the liquid storage part, one end of the gas pipe is communicated with the top of the containing tank, the other end of the gas pipe is connected with a gas conveying device, The step S2 specifically comprises the following steps: The gas conveying device is used to form a negative pressure state in the containing tank, so that the prefabricated resin solution enters the containing tank through the feeding pipe, the first valve is closed, and the gas conveying device is continuously used to keep the negative pressure state in the containing tank, so as to remove the gas bubbles in the prefabricated resin solution in the containing tank.

[0047] This step can remove the gas bubbles in the solution, so as to realize the purpose of preparing the resin microbeads with uniform size and dense structure, and guarantee the accuracy of test data.

[0048] In some embodiments, in the step S1, the resin liquid and the curing agent are mixed in a preset ratio to obtain a mixed solution, and after adjusting the solution viscosity of the mixed solution, a prefabricated resin solution is obtained. The ratio between the resin liquid and the curing agent is 30:1 to 10:1, and the viscosity of the prefabricated resin solution is 80 to 150 mPa·s. The ratio and viscosity range can ensure that the flowability of the prefabricated resin solution is appropriate, which is convenient for forming microbeads with uniform size, and at the same time guarantees the subsequent curing effect.

[0049] In order to explain the technical solutions of the present disclosure, examples 1, comparative examples 1, comparative examples 2 and comparative examples 3 are listed.

[0050] Example 1 The carbon fiber monofilament 32 is fixed at the mark 34 of the sample paperboard 31 by rosin to form a plurality of samples 3, and the samples 3 are installed in the clamping groove of the rotating sample loading device 2. The E51 resin (a bisphenol A type epoxy resin with model number E51) is uniformly mixed with triethylene tetramine at a ratio of 15:1, and the solution viscosity is adjusted to 100 mPa s by adding acetone to obtain a prefabricated resin solution, and the prefabricated resin solution is introduced into the liquid storage part 52. The first valve 55 and the second valve 56 are opened, the gas conveying device 54 is started to extract the gas in the containing tank 41 to form a negative pressure in the containing tank 41, the prefabricated resin solution in the liquid storage part 52 is sucked into the containing tank 41 through the feeding pipe 51, the first valve 55 is closed after reaching a preset amount, and the negative pressure is maintained for 3 min to remove the gas bubbles. The second valve 56 is closed, the gas extraction is stopped, the containing tank 41 returns to normal pressure, the needle cap 43 is removed, the gas conveying device 54 is started to inject gas into the containing tank 41, and the prefabricated resin solution is extruded from the extrusion needle 42 to form droplets, and then the gas injection is stopped. The knob is manually rotated at a constant speed to drive the sample 3 to rotate, the fiber monofilament 32 sweeps across the droplets to form equidistantly distributed microbeads, and all the samples 3 are completed.

[0051] Comparative Example 1 Comparative Example 1 differs from Example 1 in that the extrusion device 4 does not continuously apply negative pressure for 3 minutes to remove air bubbles before and after the predetermined amount of pre-prepared resin solution is sucked into the holding tank 41. The rest of the operations are the same.

[0052] Comparative Example 2 Comparative Example 2 differs from Example 1 in that after the E51 resin and triethylene tetramine are mixed at a ratio of 15:1, acetone is added to adjust the viscosity of the mixed solution to 200 mPa·s to form the pre-prepared resin solution. The rest of the operations are the same.

[0053] Comparative Example 3 Comparative Example 3 differs from Example 1 in that after the pre-prepared resin solution is prepared according to the ratio of Example 1, a manual sampling method is used, in which a glass rod is dipped into the pre-prepared resin solution and then contacts the fiber filament 32 to complete the beading.

[0054] The four groups of sample paperboards 31 in Example 1 and Comparative Examples 1, 2, and 3 are placed in a vacuum oven at 120°C for 60 minutes, and then taken out to test the diameter and breakage strength of the resin microspheres and calculate the coefficient of variation (CV value), with the results as follows:

[0055] The preparation method of the microbead debonding sample of Example 1 forms resin microspheres with similar size, small CV value of microsphere diameter, and small CV value of breakage strength, indicating stable data and reference value.

[0056] The preparation method of the microbead debonding sample of Comparative Example 1 results in residual gas voids in the extrusion needle of the extrusion device due to the lack of continuous negative pressure for 3 minutes to remove air bubbles before and after the predetermined amount of pre-prepared resin solution is sucked into the holding tank, leading to inconsistent resin volume extruded by different extrusion needles, non-uniform size of the prepared resin microspheres, large CV value, low breakage strength of the small volume resin microspheres tested, low average breakage strength and large CV value, and low data reference value.

[0057] The preparation method of the microbead debonding sample in Comparative Example 2 involves mixing E51 resin and triethylenetetraammonium in a 15:1 ratio, followed by adding acetone to adjust the viscosity of the mixed solution to 200 mPa·s to form a pre-prepared resin solution. Due to the small amount of solvent added, the pre-prepared resin solution has a high viscosity, increasing the time required for injection into the extrusion device container. Furthermore, the smaller amount of solvent increases the resin content in the pre-prepared resin solution, leading to an increase in the size of the microbeads on the fibers. This increases the contact area between the larger resin microbeads and the fibers, increasing the breaking force required for debonding. If the breaking force exceeds the tensile strength of the fiber monofilament, it will cause the fiber monofilament to break. This method yields too little data; most microbead tests directly break the fiber monofilament, resulting in low data reference value.

[0058] The preparation method of the microbead debonding sample in Comparative Example 3, which uses manual bead hanging, takes much longer than the preparation method in Example 1 which uses a microbead debonding sample preparation device. Manual sample preparation cannot guarantee the size of each microbead, resulting in a large CV value. Furthermore, out of 40 microbeads, some are too large or too small, resulting in only 32 valid test data. The large fluctuation in microbead size leads to large fluctuations in its breaking strength, resulting in low data reference value.

[0059] In summary, the microbead debonding sample preparation device and method provided by the present invention have high sample preparation efficiency and good sample consistency, which can meet the testing requirements in experiments.

[0060] Other embodiments of this application will readily occur to those skilled in the art upon consideration of the specification and practice of the disclosure herein. This application is intended to cover any variations, uses, or adaptations of this application that follow the general principles of this application and include common knowledge or customary techniques in the art not disclosed herein. The specification and examples are to be considered exemplary only, and the true scope and spirit of this application are indicated by the following claims.

[0061] It should be understood that this application is not limited to the precise structure described above and shown in the accompanying drawings, and various modifications and changes can be made without departing from its scope. The scope of this application is limited only by the appended claims.

Claims

1. An apparatus for preparing microbead debonding samples, characterized in that, include: support; A rotating sample loading device, which is rotatably mounted on the support; Multiple samples are detachably mounted on the rotary sample loading device. The multiple samples are distributed circumferentially along the rotary sample loading device. Each sample includes a sample paperboard and a fiber monofilament mounted on the sample paperboard. The extension directions of the fiber monofilaments on each sample paperboard on the rotary sample loading device are parallel. An extrusion device is provided on the support and located above the rotary sample loading device. The extrusion device is used to contain a pre-prepared resin solution. The bottom of the extrusion device is provided with multiple liquid outlets, which are spaced apart along the extension direction of the fiber monofilaments located on the rotary sample loading device. The feeding and discharging device is connected to the extrusion device. The feeding and discharging device is used to adjust the air pressure in the extrusion device so that the pre-prepared resin solution in the extrusion device can enter and exit the extrusion device and remove air bubbles in the pre-prepared resin solution in the extrusion device. The feeding and discharging device cooperates with the rotary sample loading device so that the pre-prepared resin solution extruded from the liquid outlet end can be transferred to the fiber monofilament located below the extrusion device.

2. The apparatus for preparing microbead debonding samples according to claim 1, characterized in that, The extrusion apparatus includes: A container, the container being fixed to the bracket; Multiple extrusion needles are disposed at the bottom of the container and communicate with the container. The multiple extrusion needles are spaced apart along the extension direction of the fiber monofilament, and the end of the extrusion needle facing away from the container constitutes the liquid outlet end. Multiple needle caps correspond one-to-one with multiple extrusion needles, and the needle caps are detachably attached to the end of the corresponding extrusion needle opposite to the receiving container.

3. The apparatus for preparing microbead debonding samples according to claim 2, characterized in that, The feeding and discharging device includes: A feed pipe, the first end of which is connected to the container tank, is used to feed a pre-prepared resin solution into the container tank; A liquid storage section is disposed on the bracket and connected to the second end of the feed pipe. The liquid storage section is used to store the pre-prepared resin solution. A trachea, the first end of which is connected to the top of the container; A gas delivery device is connected to the second end of the gas pipe, and the gas delivery device is used to regulate the gas pressure in the extrusion device through the gas pipe.

4. The apparatus for preparing microbead debonding samples according to claim 3, characterized in that, The feeding and discharging device further includes: A first valve is installed in the feed pipe; The second valve is located in the gas pipe.

5. The apparatus for preparing microbead debonding samples according to claim 2, characterized in that, The apparatus for preparing the microbead debonding sample further includes: A pressure detection unit is used to detect the pressure of the container.

6. The apparatus for preparing microbead debonding samples according to claim 1, characterized in that, The rotating sample loading device includes: A rotating shaft, the two ends of which are rotatably connected to the bracket; At least two disks are disposed on the rotating shaft, and the at least two disks are spaced apart along the axial direction of the rotating shaft. The radial direction of each disk is perpendicular to the axial direction of the rotating shaft. The outer circumferential surface of the disks is provided with a plurality of slots at intervals, and the plurality of slots on at least adjacent disks correspond one-to-one. The sample paperboard is fixed in the corresponding at least two slots. A drive unit is connected to one of the two ends of the rotating shaft, and the drive unit is used to drive the rotating shaft to rotate.

7. The apparatus for preparing microbead debonding samples according to any one of claims 1-6, characterized in that, The sample paperboard is provided with a groove, the fiber monofilament is located in the groove, and the two ends of the fiber monofilament are respectively fixed to two opposite sidewalls of the groove.

8. A method for preparing a microbead debonding sample, characterized in that, The preparation is carried out using the apparatus for preparing microbead debonding samples as described in any one of claims 1-7, and the preparation method includes the following steps: S1. Prepare a pre-made resin solution and multiple samples, wherein the samples include a sample paperboard and fiber monofilaments disposed on the sample paperboard, and assemble multiple samples into a rotary sample loading device; S2. A negative pressure state is formed in the container of the extrusion device through the feeding and discharging device. The negative pressure state can transport the pre-made resin solution into the container and continuously maintain the negative pressure state in the container through the feeding and discharging device to remove air bubbles in the pre-made resin solution. S3. Gas is injected into the container through the feeding and discharging device to squeeze the pre-prepared resin solution in the container from multiple outlets at the bottom of the container, and the pre-prepared resin solution squeezed out from the outlets forms resin droplets at the outlets. S4. Rotate the rotary sample loading device so that the fiber monofilaments of the multiple samples pass through the bottom of the container in sequence, so that the multiple resin droplets are transferred onto the fiber monofilaments to form multiple resin microbeads, thereby obtaining the sample intermediate. S5. The intermediate sample is solidified and cooled to obtain a microbead debonding sample.

9. The method for preparing the microbead debonding sample according to claim 8, characterized in that, The feeding and discharging device includes a feed pipe, an air pipe, a liquid storage section, and a first valve disposed on the feed pipe. One end of the feed pipe is connected to the container tank, and the other end of the feed pipe is connected to the liquid storage section. One end of the air pipe is connected to the top of the container tank, and the other end of the air pipe is connected to a gas conveying device. In step S2... The gas delivery device creates a negative pressure state inside the container to allow the pre-prepared resin solution to enter the container through the feed pipe. The first valve is closed, and the gas delivery device continuously maintains the negative pressure state inside the container to remove air bubbles from the pre-prepared resin solution inside the container.

10. The method for preparing the microbead debonding sample according to claim 8, characterized in that, In step S1, the resin liquid and the curing agent are mixed in a preset ratio to obtain a mixed solution. After adjusting the viscosity of the mixed solution, the pre-made resin solution is obtained. The ratio of resin liquid to curing agent is 30:1 to 10:1, and the viscosity of the pre-prepared resin solution is 80 to 150 mPa·s.

Images