Preparation method of high-performance carbon fiber multifilament tensile mechanical property test sample

By spraying glue liquid and curing with a wire wrap rod with heating function, combined with the use of a force control frame and a force measuring instrument, the problems of damage and unadjustment of tension in the tensile mechanical properties test of fiber multifilament are solved, significantly improving the accuracy and stability of the test results.

CN119958923APending Publication Date: 2025-05-09BAOWU CHARCOAL MATERIAL TECH CO LTD
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Patent Information

Application Number
CN202311469142.8
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2023-11-07
Publication Date
2025-05-09

AI Technical Summary

Technical Problem

In the preparation of intermediate phase asphalt-based carbon fiber multifilament tensile mechanical properties test samples, there are problems such as fiber damage, low glue impregnation efficiency, difficult glue content, and unadjustable fiber multifilament tension, resulting in low tensile strength value, large discreteness and poor reproducibility.

Method used

The glue liquid is sprayed evenly on the fiber multifilament, and cured by a wire wrapping rod with heating function. Combined with the use of a power control frame and a force measuring instrument, we ensure the full tension of the fiber multifilament and the uniform curing of the glue liquid.

Benefits of technology

The accuracy and stability of the tensile mechanical properties test results of fiber multifilament are improved, the fiber damage and uneven glue solution problems are reduced, and the repetition and reproducibility of the test results are significantly improved.

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Abstract

The invention relates to a preparation method and device of a high-performance carbon fiber multifilament tensile mechanical property test sample, which adopts a detachable filament winding rod with a heating function and integrates the use of a glue spraying process. The problems of low tensile strength value, large result discreteness, poor reproducibility and the like caused by low glue solution utilization rate, serious fiber damage and the like in the existing sample preparation process are effectively solved, the tension force of fiber samples of different sample preparation batches is the same in combination with the use of a tensiometer, and the stability, the comparability and the reproducibility of test results are ensured; meanwhile, due to the fact that the tension is adjustable and controllable, the device can be widely applied to carbon fibers with various tow specifications and has applicability to samples such as PAN-based carbon fibers.
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Description

Technical Field

[0001] The invention relates to the technical field of analysis and detection sample preparation, and in particular to a method for preparing a high-performance carbon fiber multifilament tensile mechanical property test sample. Background Art

[0002] Mesophase pitch-based carbon fiber is widely used in aerospace, new energy, rail transportation, integrated circuits, electronic instruments, high-pressure storage tanks, nuclear industry and many other fields due to its low density, high modulus, high thermal conductivity, corrosion resistance, creep resistance and electromagnetic shielding. However, when characterizing the tensile mechanical properties of mesophase pitch-based carbon fiber, its extremely high modulus and brittleness make it more difficult to prepare test samples, the success rate of sample preparation is low, and the repeatability and reproducibility are poor, making it impossible to objectively and accurately evaluate the tensile mechanical properties and stability of carbon fiber multifilaments.

[0003] Chinese patent CN110763534A discloses "an ultra-high modulus carbon fiber multifilament tensile performance sample preparation device and sample preparation method", which uses a precise control system to vertically drip the impregnation liquid to the ultra-high modulus carbon fiber multifilament, and controls the amount and speed of the glue liquid dripping to keep consistent through the electronic control system, ensuring the consistency of the glue content of the tensile sample, ensuring the low damage and full impregnation of the ultra-high modulus carbon fiber and the consistency of the glue content of the tensile sample, improving the accuracy of the ultra-high modulus carbon fiber tensile performance test and reducing the test cost. It mainly solves the problems of low efficiency, uneven impregnation and difficulty in controlling the manual impregnation method, but has not effectively solved the problems of low tensile strength test values, large discrete results and poor reproducibility caused by inconsistent tension of the fiber multifilament after impregnation.

[0004] Chinese patent CN102809499A discloses "a method for preparing samples for testing the tensile properties of carbon fibers". The number of the same samples to be tested can be set by the number of turns of the wire winding frame; and the number of groups of samples to be tested can be set by setting the length of the wire winding rod in the wire winding frame. Compared with manual sample preparation, its efficiency is greatly improved. At the same time, combined with the mass ratio of epoxy resin, curing agent and acetone and the drying conditions in the preparation method, the curing performance is improved, and the tension of the carbon fiber multifilament after dipping can be controlled by adjusting the telescopic rod to adjust the carbon fiber multifilament to be straight, thereby ensuring the accuracy and stability of the test data.

[0005] Chinese patent CN116148006A discloses "Carbon fiber multifilament tensile performance test sample preparation device and its use method", which can realize automatic sample preparation to improve sample preparation efficiency and sample quality, and can also control the tension of the filament bundle to ensure the consistency and stability of the test results; and monitor the concentration of the glue solution online and adjust the unqualified glue solution so that the glue solution concentration reaches the sample preparation standard to further improve the sample quality.

[0006] Therefore, it is necessary to develop a sample preparation method that has efficient and uniform impregnation, adjustable and controllable tension, basically no fiber damage, and is suitable for high modulus carbon fiber. Summary of the invention

[0007] The purpose of the present invention is to provide a method for preparing a high-performance carbon fiber multifilament tensile mechanical property test sample. The invention can effectively solve the problems of low tensile strength value, large discreteness of results and poor reproducibility caused by fiber damage in the existing sample preparation process, low impregnation efficiency, difficult to control glue content, and unadjustable tension of fiber multifilaments. At the same time, because the tension is adjustable and controllable, the invention can also be widely used in carbon fibers of various tow specifications, and is also applicable to samples such as PAN-based carbon fibers.

[0008] To achieve the above object, the technical solution of the present invention is:

[0009] A method for preparing a high-performance carbon fiber multifilament tensile mechanical property test sample comprises the following steps:

[0010] 1) Silk wrapping

[0011] Winding the fiber multifilaments on a heating winding rod in sequence, and adjusting the tension value of the fiber multifilaments to pre-tension the fiber multifilaments;

[0012] 2) Glue spraying

[0013] Spray the glue evenly on the fiber multifilaments, then adjust the tension value of the fiber multifilaments to ensure that the glue-carrying fiber multifilaments are fully tensioned, and let it stand until there is no obvious glue hanging or dripping on the fiber multifilaments;

[0014] 3) Heating

[0015] Turn on the electric heating rod in the winding rod for heating, and turn off the electric heating rod when the glue on the fiber multifilament is completely solidified;

[0016] 4) Sampling

[0017] At the same time, the fiber multifilaments are cut off from both ends of the winding rod to take out the fiber multifilament samples.

[0018] Preferably, the glue liquid comprises epoxy resin, curing agent and acetone, and the mass ratio is epoxy resin: curing agent: acetone = 1:0.1-0.8:1-2, the glue liquid temperature is 35±5°C, and the glue liquid viscosity is 400-800mPa·s.

[0019] Preferably, in the step 1), when the fiber multifilament bundle specification is 1K-3K, the pre-tensioning force is 80-150 cN, when the fiber multifilament bundle specification is 3K-6K, the pre-tensioning force is 150-300 cN, and when the fiber multifilament bundle specification is 6K-12K, the pre-tensioning force is 300-800 cN.

[0020] Preferably, in the step 2), the glue spraying rate ranges from 5 to 100 ml / min, preferably, the glue spraying rate is set to 15 to 20 ml / min; when the fiber multifilament tow specification is 1K to 3K, the glue spraying time is 10 to 15 min, when the fiber multifilament tow specification is 3K to 6K, the glue spraying time is 15 to 20 min, and when the fiber multifilament tow specification is 6K to 12K, the glue spraying time is 20 to 25 min.

[0021] Preferably, in the step 2), when the specification of the fiber multifilament bundle is 1K to 3K, the tension force of the rubber-carrying fiber is 150 to 300 cN, when the specification of the fiber multifilament bundle is 3K to 6K, the tension force of the rubber-carrying fiber is 300 to 600 cN, and when the specification of the fiber multifilament bundle is 6K to 12K, the tension force of the rubber-carrying fiber is 600 to 1500 cN.

[0022] Preferably, in step 3), the heating temperature is 60-200°C.

[0023] Wind the fiber multifilament on the winding rod, slide the force adjustment frame, and observe the tension value to ensure that the fiber multifilament is in a straightened and pre-tightened state, and then evenly and quantitatively spray the glue on the fiber. The present invention uses a spraying method to spray the glue on the fiber multifilament, which can better ensure the integrity of the fiber multifilament. Further, the glue spraying rate is set to 15-20ml / min; when the fiber multifilament bundle specification is 1K-3K, the glue spraying time is 10-15min, when the fiber multifilament bundle specification is 3K-6K, the glue spraying time is 15-20min, and when the fiber multifilament bundle specification is 6K-12K, the glue spraying time is 20-25min. The glue spraying amount is controlled by combining the glue spraying rate with the mode of controlling the time of the fiber bundle size, and the fiber can be quantitatively sprayed with glue, and the glue utilization rate is high, avoiding the problems of uneven glue spraying amount and insufficient fiber wettability.

[0024] Then adjust the fiber multifilament tension value to ensure that the adhesive fiber is fully straightened and tensioned, and after waiting for a certain period of time, turn on the heating function on the winding rod to heat and solidify the adhesive fiber. In the adhesive liquid solidification stage, since the present invention uses a winding rod with a heating function, the temperature of the winding rod can be directly adjusted to the required temperature to solidify the adhesive liquid, thereby avoiding the need to transport the device to an oven for adhesive liquid solidification to cause fiber damage, and can also reduce equipment and space requirements.

[0025] Finally, after the solidification is completed, the fiber multifilaments are cut off from the bottom of the winding rod at the same time to remove the fiber samples. On the one hand, removing them at the same time can improve the operation efficiency without cutting them one end at a time; on the other hand, it can reduce the damage to the sample. When cutting one end at a time, first cut off one end and then cut off the other end. In the process, the sample is similar to the structure of a cantilever beam, with bending moment, and is easy to be damaged.

[0026] The present invention also provides a device for preparing a sample for testing the tensile mechanical properties of high-performance carbon fiber multifilaments, comprising:

[0027] Fixed frame;

[0028] Two parallel sliding rails, one end of which is fixed on a fixed frame;

[0029] A force regulating frame is slidably mounted on two sliding rails; a force measuring instrument is mounted on the force regulating frame; and a driving device is mounted on the force regulating frame;

[0030] A plurality of wire winding rods are respectively arranged on the fixing frame and the force adjusting frame; a heating device is arranged on the wire winding rods;

[0031] A plurality of cutting pieces, respectively arranged on one side of each wire winding rod, preferably spring blades;

[0032] A glue spraying device, arranged outside the sliding track;

[0033] The controller is electrically connected to the driving device, the dynamometer, the heating device and the glue spraying device.

[0034] Preferably, there are two glue spraying devices, which are respectively arranged on the outer sides of the two sliding rails.

[0035] Preferably, the glue spraying device includes a support frame, a heated glue storage tank installed at the bottom of the support frame, and a spray head installed at the top of the support frame and rotatable 360 ​​degrees; the glue storage tank and the spray head are connected through a suction pipe, and a viscometer is installed in the glue storage tank.

[0036] Preferably, the wire winding rod is connected to the fixing frame and the force adjusting frame by threads.

[0037] The force frame can slide freely on the sliding track to ensure that the fiber multifilament can be fully tensioned, thereby greatly improving the accuracy of the tensile mechanical properties test results; the force frame is equipped with a dynamometer to achieve quantitative control of the fiber tension force, ensuring that the tension force of fiber samples from different sample preparation batches is the same, thereby ensuring the stability, comparability and reproducibility of the test results.

[0038] The connection between the winding rod and the fixed frame and the force adjusting frame is threaded, which is convenient for selectively replacing winding rods of different diameters and lengths according to the fragility of different fibers and different yarn bundle specifications. Large-diameter winding rods are used for fibers with high brittleness to alleviate the problem of brittle fiber breaking due to excessive bending. Long-length winding rods are used for fibers with large yarn bundles to avoid entanglement and adhesion between fiber multifilament bundles.

[0039] Each winding rod has a separate temperature control function, which can achieve rapid drying and curing of the adhesive fiber multifilament, avoiding the traditional frequent operation of moving the adhesive fiber multifilament into the oven for curing, which causes random fiber breakage, low sample preparation success rate, discrete and unstable measurement data, etc. In addition, a cutting piece (spring blade) is installed next to each winding rod to facilitate the rapid removal of the fiber multifilament sample from the winding rod after the adhesive is cured.

[0040] The glue spraying devices symmetrically distributed on both sides of the sliding track can realize uniform, quantitative and timed glue spraying on the fiber multifilament. The glue spraying device consists of a spray head that can rotate 360 ​​degrees, a support frame and a heated glue storage tank. The suction pipe is installed in the center of the support frame and connected to the glue storage tank and the spray head. The heating temperature of the glue storage tank is adjustable from 20 to 100 degrees. Different types of dipping glue can be selected according to actual needs. The heating function of the glue storage tank can avoid the problem of high viscosity and poor fluidity of the glue at room temperature, which makes glue spraying difficult; at the same time, the glue storage tank is connected with a viscometer to observe the viscosity changes of the glue in real time.

[0041] The glue tank temperature, glue viscosity, glue spraying, force frame sliding distance and dynamometer in the entire device are all controlled by the controller, realizing highly sensitive automatic display and control, which can avoid the differentiation of sample preparation conditions caused by inconsistent human operation, and ultimately affect the accuracy of the measurement results.

[0042] Compared with the prior art, the present invention has the following advantages:

[0043] The present invention uses a spraying method to spray the glue on the fiber multifilaments, which can better ensure the integrity of the fiber multifilaments. However, the traditional glue tank dipping process requires operations such as shaking the glue, rubbing the glue or squeezing the glue, which is easy to damage the fiber; the fiber needs to be immersed in the glue tank for dipping, and the fallen fiber fragments will contaminate the glue, reducing the workability of the glue, and the residual fiber fragments in the glue are easy to adhere to the subsequent glue-dipped fiber bundles together with the glue, affecting the integrity and surface smoothness of the sample. In combination with the curing stage, a wire winding rod with a heating function is used to cure the glue-carrying fiber, further avoiding the need to move the device to an oven for glue curing, which causes fiber damage.

[0044] In the device described in the present invention, a detachable winding rod with a heating function is used, and winding rods of different diameters and lengths can be selectively replaced according to the fragility of different fibers and different yarn bundle specifications, which can not only alleviate the problem of brittle fiber breaking due to excessive bending, but also avoid the entanglement and adhesion between fiber multifilament bundles. At the same time, in the curing stage of the adhesive fiber, the heating function of the winding rod is directly turned on to quickly dry and cure the adhesive fiber multifilament, avoiding the traditional need to move the adhesive fiber multifilament into the oven for curing and frequent operations, which may cause random fiber breakage. The force adjustment frame is equipped with a dynamometer to accurately measure the tension value of the fiber multifilament before and after spraying, ensuring that the tension of fiber samples from different sample preparation batches is the same, and ensuring the stability, comparability and reproducibility of the test results. BRIEF DESCRIPTION OF THE DRAWINGS

[0045] Figure 1 Schematic diagram of the structure of the device according to the embodiment of the present invention. DETAILED DESCRIPTION

[0046] The present invention will be further described below in conjunction with the embodiments and drawings.

[0047] See also Figure 1 The device for preparing a sample for testing the tensile mechanical properties of high-performance carbon fiber multifilaments of the present invention comprises:

[0048] Fixed frame 1;

[0049] Two parallel sliding rails 2, 2', one end of which is fixed on the fixed frame 1;

[0050] The force adjusting frame 3 is slidably mounted on the two sliding rails 2 and 2'; a force measuring instrument 4 is mounted on the force adjusting frame 3; and a driving device is mounted on the force adjusting frame 3;

[0051] A plurality of wire winding rods 5, 5' are respectively arranged on the fixing frame 1 and the force adjusting frame 3; the wire winding rods 5, 5' are provided with heating devices; in this embodiment, the wire winding rods 5, 5' are connected to the fixing frame 1 and the force adjusting frame 3 by threads;

[0052] A plurality of cutting members 6, 6' are respectively arranged on one side of each wire winding rod 5, 5'; the cutting members are preferably spring blades;

[0053] Glue spraying devices 7, 7' are arranged outside the sliding rails 2, 2';

[0054] The controller 8 is electrically connected to the driving device, the dynamometer, the heating device and the glue spraying device.

[0055] Preferably, the glue spraying device 7 includes a support frame 71, a heated glue storage tank 72 installed at the bottom of the support frame 71, and a spray head 73 installed at the top of the support frame 71 and rotatable 360 ​​degrees; the glue storage tank 73 and the spray head 73 are connected through a suction pipe, and a viscometer is installed in the glue storage tank 72.

[0056] Example 1

[0057] A method for preparing a high-performance carbon fiber multifilament tensile mechanical property test sample comprises the following steps:

[0058] 1) Silk wrapping

[0059] Install winding rods of appropriate sizes on the fixed frame and the force adjusting frame, adjust the sliding distance of the force adjusting frame on the sliding track through the controller, so that the distance between the force adjusting frame and the fixed frame reaches 1.3m, wind the fiber multifilaments on the winding rods in sequence, slide the force adjusting frame and control the tension value on the force gauge to 80-100cN, and pre-tension the fiber multifilaments;

[0060] 2) Glue spraying

[0061] Turn on the glue spraying device, set the glue spraying rate to 18 ml / min, let the spray head spray glue evenly on the fiber multifilament for 10 to 15 minutes, slide the force adjustment frame after the glue spraying to control the tension value on the dynamometer to 200 to 250 cN, so that the fiber multifilament is fully tensioned, and let it stand until there is no obvious glue hanging or dripping on the fiber multifilament; the glue includes epoxy resin, curing agent and acetone, in a mass ratio of epoxy resin: curing agent: acetone = 1:0.34:1, the temperature is 35±5°C, and the glue viscosity is 400 to 800 mPa·s;

[0062] 3) Heating

[0063] Turn on the heating function of the winding rod, adjust the temperature to 120°C, maintain it for 120 minutes, and turn off the heating when the glue on the fiber multifilament is completely solidified;

[0064] 4) Sampling

[0065] Start the spring blade next to the winding rod, take out the fiber multifilament sample and cut it into a standard length of 250mm, paste the paper reinforcement sheet and perform the tensile test.

[0066] The self-produced mesophase pitch-based graphite fibers (tow specification 1K) were sampled and tested by the scheme described in Example 1 and the traditional method, and the results of the tensile test are shown in Table 1. The outer diameter of the winding rod is 20 mm and the length is 5 cm.

[0067] Table 1

[0068]

[0069] Example 2

[0070] A method for preparing a high-performance carbon fiber multifilament tensile mechanical property test sample comprises the following steps:

[0071] 1) Silk wrapping

[0072] Install winding rods of suitable sizes on the fixed frame and the force adjusting frame, adjust the sliding distance of the force adjusting frame on the sliding track through the controller, so that the distance between the force adjusting frame and the fixed frame reaches 1.3m, wind the fiber multifilaments on the winding rods in sequence, slide the force adjusting frame and control the tension value on the force gauge to 100-120cN, and pre-tension the fiber multifilaments;

[0073] 2) Glue spraying

[0074] Turn on the glue spraying device, set the glue spraying rate to 17 ml / min, let the spray head spray glue evenly on the fiber multifilament for 10 to 15 minutes, slide the force adjustment frame after the glue spraying to control the tension value on the dynamometer to 220 to 250 cN, so that the fiber multifilament is fully tensioned, and let it stand until there is no obvious glue hanging or dripping on the fiber multifilament; the glue includes epoxy resin, curing agent and acetone, in a mass ratio of epoxy resin: curing agent: acetone = 1:0.1:1, the temperature is 35±5°C, and the glue viscosity is 400 to 800 mPa·s;

[0075] 3) Heating

[0076] Turn on the heating function of the winding rod, adjust the temperature to 120°C, maintain it for 120 minutes, and turn off the heating when the glue on the fiber multifilament is completely solidified;

[0077] 4) Sampling

[0078] Start the spring blade next to the winding rod, take out the fiber multifilament sample and cut it into a standard length of 250mm, paste the paper reinforcement sheet and perform the tensile test.

[0079] The high modulus asphalt-based carbon fiber K13D2U (tow specification 2K) of Mitsubishi Corporation of Japan was sampled and tensile tested using the scheme described in Example 2 and the traditional method, and the results are shown in Table 2: the outer diameter of the winding rod is 20 mm and the length is 5 cm.

[0080] Table 2

[0081]

[0082] Example 3

[0083] A method for preparing a high-performance carbon fiber multifilament tensile mechanical property test sample comprises the following steps:

[0084] 1) Silk wrapping

[0085] Install winding rods of appropriate sizes on the fixed frame and the force adjusting frame, adjust the sliding distance of the force adjusting frame on the sliding track through the controller, so that the distance between the force adjusting frame and the fixed frame reaches 1.3m, wind the fiber multifilaments on the winding rods in sequence, slide the force adjusting frame and control the tension value on the force gauge to 250-280cN, and pre-tension the fiber multifilaments;

[0086] 2) Glue spraying

[0087] Turn on the glue spraying device, set the glue spraying rate to 15 ml / min, let the spray head spray glue evenly on the fiber multifilament for 15 to 20 minutes, slide the force adjustment frame after the glue spraying to control the tension value on the dynamometer to 500 to 600 cN, so that the fiber multifilament is fully tensioned, and let it stand until there is no obvious glue hanging or dripping on the fiber multifilament; the glue includes epoxy resin, curing agent and acetone, in a mass ratio of epoxy resin: curing agent: acetone = 1:0.5:2, the temperature is 35±5°C, and the glue viscosity is 400 to 800 mPa·s;

[0088] 3) Heating

[0089] Turn on the heating function of the winding rod, adjust the temperature to 120℃, maintain it for 150 minutes, and turn off the heating when the glue on the fiber multifilament is completely solidified;

[0090] 4) Sampling

[0091] Start the spring blade next to the winding rod, take out the fiber multifilament sample and cut it into a standard length of 250mm, paste the paper reinforcement sheet and perform the tensile test.

[0092] The high modulus PAN-based carbon fiber M55JB (tow specification 6K) produced by Toray Industries, Japan, was sampled and tensile tested using the scheme described in Example 3 and the traditional method, respectively. The results are shown in Table 3 below. The outer diameter of the winding rod is 17 mm and the length is 7 cm.

[0093] Table 3

[0094]

[0095] Example 4

[0096] A method for preparing a high-performance carbon fiber multifilament tensile mechanical property test sample comprises the following steps:

[0097] 1) Silk wrapping

[0098] Install winding rods of suitable sizes on the fixed frame and the force adjusting frame, adjust the sliding distance of the force adjusting frame on the sliding track through the controller, so that the distance between the force adjusting frame and the fixed frame reaches 1.3m, wind the fiber multifilaments on the winding rods in sequence, slide the force adjusting frame and control the tension value on the force gauge to 700-750cN, and pre-tension the fiber multifilaments;

[0099] 2) Glue spraying

[0100] Turn on the glue spraying device, set the glue spraying rate to 20 ml / min, let the spray head spray glue evenly on the fiber multifilament for 20 to 25 minutes, slide the force adjustment frame after the glue spraying to control the tension value on the dynamometer to 1100 to 1300 cN, so that the fiber multifilament is fully tensioned, and let it stand until there is no obvious glue hanging or dripping on the fiber multifilament; the glue includes epoxy resin, curing agent and acetone, in a mass ratio of epoxy resin: curing agent: acetone = 1:0.8:1.5, the temperature is 35±5°C, and the glue viscosity is 400 to 800 mPa·s;

[0101] 3) Heating

[0102] Turn on the heating function of the winding rod, adjust the temperature to 120°C, maintain it for 180 minutes, and turn off the heating when the glue on the fiber multifilament is completely solidified;

[0103] 4) Sampling

[0104] Start the spring blade next to the winding rod, take out the fiber multifilament sample and cut it into a standard length of 250mm, paste the paper reinforcement sheet and perform the tensile test.

[0105] The high-performance PAN-based carbon fiber ZJBJ4022 (tow specification 12K) of Zhejiang Baojing Carbon Materials Co., Ltd. was sampled and tensile tested using the scheme described in Example 4 and the traditional method. The results are shown in Table 4 below. The outer diameter of the winding rod is 15 mm and the length is 12 cm.

[0106] Table 4

[0107]

[0108] The traditional method mentioned above refers to the manual dipping method. The fiber tension and other factors are random and have not been systematically standardized. Please refer to Appendix A of GB / T 3362-2017.

[0109] It can be seen from the data in Tables 1 to 4 that, compared with the traditional sample preparation method, the present invention has a more controllable glue content and lower discreteness; and the test values ​​of tensile strength and tensile modulus are higher than those of the traditional sample preparation method, with a smaller discrete coefficient and good repeatability. If the glue is not uniform, it will preferentially damage the glue-deficient or glue-rich areas during testing; if the fibers are not fully tensioned, many fibers will not function during testing, and it is mainly the glue that is carrying the load; if the fiber filaments are damaged, it is equivalent to a reduction in the number of fibers carried in the test sample and a decrease in the load-bearing capacity. Therefore, uniform glue, fully tensioned fibers, and minimal fiber filament damage can greatly improve the test results.

[0110] In addition, compared with the reported values, the test results of the sample preparation method of the present invention can basically reach or even exceed the reported values. The preparation of carbon fiber multifilament tensile samples is a major problem in the industry. The reported values ​​are reference values ​​provided by manufacturers based on their test results, and are not the true performance of the fiber. The test results of the present invention can exceed the values ​​reported by some manufacturers, indicating that the test results of the present invention are closer to the true performance of the fiber, with less fiber damage and higher reliability.

Claims

1. A method for preparing a high-performance carbon fiber multifilament tensile mechanical properties test sample, characterized in that: The steps include: 1) Silk wrapping Winding the fiber multifilaments on a heating winding rod in sequence, and adjusting the tension value of the fiber multifilaments to pre-tension the fiber multifilaments; 2) Glue spraying Spray the glue evenly on the fiber multifilaments, then adjust the tension value of the fiber multifilaments to ensure that the glue-carrying fiber multifilaments are fully tensioned, and let it stand until there is no obvious glue hanging or dripping on the fiber multifilaments; 3) Curing Turn on the heating function on the winding rod, and turn off the heating after the glue on the fiber multifilament is completely solidified; 4) Sampling At the same time, the fiber multifilaments are cut off from both ends of the winding rod to take out the fiber multifilament samples.

2. The method for preparing a high-performance carbon fiber multifilament tensile mechanical properties test sample according to claim 1, characterized in that: The glue in step 2) comprises epoxy resin, curing agent and acetone; in terms of mass ratio, epoxy resin: curing agent: acetone = 1: 0.1-0.8: 1-2, the glue temperature is 35±5°C, and the glue viscosity is 400-800mPa·s.

3. The method for preparing a high-performance carbon fiber multifilament tensile mechanical properties test sample according to claim 1 or 2, characterized in that: In the step 1), when the fiber multifilament bundle specification is 1K-3K, the pre-tensioning force is 80-150 cN; when the fiber multifilament bundle specification is 3K-6K, the pre-tensioning force is 150-300 cN; when the fiber multifilament bundle specification is 6K-12K, the pre-tensioning force is 300-800 cN.

4. The method for preparing a high-performance carbon fiber multifilament tensile mechanical property test sample according to claim 1, 2 or 3, characterized in that: In the step 2), the glue spraying rate ranges from 5 to 100 ml / min, preferably, the glue spraying rate is set to 15 to 20 ml / min; when the fiber multifilament bundle specification is 1K to 3K, the glue spraying time is 10 to 15 min; when the fiber multifilament bundle specification is 3K to 6K, the glue spraying time is 15 to 20 min; when the fiber multifilament bundle specification is 6K to 12K, the glue spraying time is 20 to 25 min.

5. The method for preparing a high-performance carbon fiber multifilament tensile mechanical property test sample according to claim 1, 3 or 4, characterized in that: In the step 2), when the specification of the fiber multifilament bundle is 1K-3K, the tension force of the rubber-attached fiber is 150-300 cN; when the specification of the fiber multifilament bundle is 3K-6K, the tension force of the rubber-attached fiber is 300-600 cN; when the specification of the fiber multifilament bundle is 6K-12K, the tension force of the rubber-attached fiber is 600-1500 cN.

6. The method for preparing a high-performance carbon fiber multifilament tensile mechanical property test sample according to claim 1 or 5, characterized in that: In the step 3), the heating temperature is 60-200°C.

7. A device for preparing samples for the method for testing tensile mechanical properties of high-performance carbon fiber multifilaments according to claims 1 to 6, characterized in that: include: Fixed frame; Two parallel sliding rails, one end of which is fixed on a fixed frame; A force regulating frame is slidably mounted on two sliding rails; a force measuring instrument is mounted on the force regulating frame; and a driving device is mounted on the force regulating frame; A plurality of wire winding rods are respectively arranged on the fixing frame and the force adjusting frame; a heating device is arranged on the wire winding rods; A plurality of cutting pieces, respectively arranged on one side of each wire winding rod, preferably spring blades; A glue spraying device, arranged outside the sliding track; The controller is electrically connected to the driving device, the dynamometer, the heating device and the glue spraying device.

8. The device according to claim 7, characterized in that: The glue spraying device includes a support frame, a heated glue storage tank installed at the bottom of the support frame, and a spray head installed at the top of the support frame and rotatable 360 ​​degrees; the glue storage tank and the spray head are connected through a suction pipe, and a viscometer is installed in the glue storage tank.

9. The device according to claim 7 or 8, characterized in that: There are two glue spraying devices, which are respectively arranged on the outer sides of the two sliding rails.

10. The device according to claim 7, characterized in that: The wire winding rod is connected with the fixing frame and the force adjusting frame by threaded connection.

Citation Information

Patent Citations

  • Sample preparation method for carbon fiber tensile property test

    CN102809499A

  • Tensile property sample preparation device of ultra-high modulus carbon fiber multifilament and sample preparation method

    CN110763534A

  • Sample preparation device for tensile property test of carbon fiber multifilament and use method of sample preparation device

    CN116148006A