JP2018100885A - Method for measuring strength of regenerated carbon fiber - Google Patents
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本発明は、再生炭素繊維の強度の測定方法に関する。 The present invention relates to a method for measuring the strength of regenerated carbon fiber.
近年、航空機、自動車、タンク等の材料として、軽量で強度の高い炭素繊維強化プラスチック（ＣＦＲＰ）が普及している。用途の拡大に伴って、製造工程で生じる端材や、一度使用された炭素繊維強化プラスチックの廃材の相当量が、焼却されたり、埋め立てられている。しかし、炭素繊維強化プラスチックの端材や廃材から回収した炭素繊維の中には、十分な強度を有していて再利用が可能なものが存在すると考えられている。このため、一旦加工したり使用したあと再生処理を行って取り出した炭素繊維（以下、再生炭素繊維またはリサイクル炭素繊維とも言う）の強度を解析して、十分な強度を有する再生炭素繊維を再利用したいという要求がある。 In recent years, carbon fiber reinforced plastic (CFRP), which is lightweight and high in strength, has become widespread as a material for aircraft, automobiles, tanks and the like. With the expansion of applications, a considerable amount of scrap materials generated in the manufacturing process and carbon fiber reinforced plastic waste materials once used are incinerated or landfilled. However, it is considered that some carbon fibers recovered from the end materials and waste materials of carbon fiber reinforced plastic have sufficient strength and can be reused. For this reason, the strength of carbon fiber (hereinafter also referred to as regenerated carbon fiber or recycled carbon fiber) that has been processed and used and then reprocessed and taken out is analyzed, and recycled carbon fiber having sufficient strength is reused. There is a demand to do.
例えば、炭素繊維強化プラスチック（以下、ＣＦＲＰとも言う）に適用された炭素繊維は、加工の工程と使用によって、強度が部分的に変化している可能性がある。さらに、炭素繊維強化プラスチックから炭素繊維を回収して再生する方法として、熱分解法、常圧溶解法、超臨界流体法、亜臨界流体法、触媒分解法などが知られているが、これらの方法は熱又は薬品で樹脂を除去して炭素繊維を取り出す方法であるので、さらに一部の炭素繊維の強度が変化していると考えられる。このため、図７に示すように、再生炭素繊維は、たとえ同一の製品から再生されたものであっても、繊維ごとに強度のばらつきが大きい。 For example, the strength of carbon fibers applied to carbon fiber reinforced plastic (hereinafter also referred to as CFRP) may vary partially depending on the process and use. Furthermore, as a method for recovering and recovering carbon fiber from carbon fiber reinforced plastic, a thermal decomposition method, a normal pressure dissolution method, a supercritical fluid method, a subcritical fluid method, a catalytic decomposition method, etc. are known. Since the method is a method in which the resin is removed by heat or chemicals and the carbon fiber is taken out, it is considered that the strength of some of the carbon fibers is further changed. For this reason, as shown in FIG. 7, even if the regenerated carbon fiber is regenerated from the same product, there is a large variation in strength for each fiber.
炭素繊維の繊維強度の試験方法に関して、ＪＩＳ Ｒ７６０６「炭素繊維−単繊維の引張特性の試験方法」が定められている。ＪＩＳ Ｒ７６０６の試験方法は、単繊維の試験片を、繊維が破断するまで一定の速度で引張り、引張荷重と伸びの関係を記録する方法である。また、特許文献１では、炭素繊維束に対して、ＪＩＳ Ｒ７６０２の炭素繊維織物試験方法を適用して、強度を測定している。 JIS R7606 “Testing Method for Tensile Properties of Carbon Fiber-Single Fiber” is defined as a test method for fiber strength of carbon fibers. The test method of JIS R7606 is a method in which a single fiber test piece is pulled at a constant speed until the fiber breaks, and the relationship between tensile load and elongation is recorded. Moreover, in patent document 1, the carbon fiber fabric test method of JIS R7602 is applied with respect to a carbon fiber bundle, and the intensity | strength is measured.
しかし、強度のばらつきが大きい再生炭素繊維束について、単繊維の抜き取り試験で繊維束全体の強度を知るためには、極めて多くの試験回数が必要となる。また、再生炭素繊維束から単繊維を抜き出して試験機にセットする工程で、強度の弱い繊維は切れてしまっていることがあり、引張り試験のデータが得られた繊維は一定の強度を有する繊維に片寄っている可能性がある。抜き出し段階で切れなかった繊維だけで測定した結果は、実際の再生炭素繊維よりも高い強度を示している可能性がある。また、繊維束として強度を測定する場合、束を構成する繊維の本数を１本ずつ数えて確認してから測定することは非常に手間がかかり、現実的ではない。 However, in order to know the strength of the entire fiber bundle in a single fiber sampling test for a regenerated carbon fiber bundle with a large variation in strength, a very large number of tests are required. Also, in the process of extracting a single fiber from a recycled carbon fiber bundle and setting it in a testing machine, a weak fiber may be cut off, and a fiber from which tensile test data is obtained is a fiber having a certain strength There is a possibility that it is offset. The result of measuring only the fibers that were not cut at the extraction stage may indicate a higher strength than the actual recycled carbon fiber. Moreover, when measuring the strength as a fiber bundle, it is very time-consuming and time-consuming to measure after confirming the number of fibers constituting the bundle one by one.
再生炭素繊維の引張強度を測定する方法として、短繊維を対象とした従来のＪＩＳ Ｒ７６０６の試験方法よりも効率の良い方法が求められている。また、単繊維を対象とした試験では、抜き出し工程で切れなかった繊維を対象とした測定が行われており、実際よりも引張強度が高く示される可能性がある。このため、簡易で効率の良い測定が可能で、且つ実際の再生炭素繊維の強度を反映した、精度の高い再生炭素繊維の強度測定方法が求められている。 As a method for measuring the tensile strength of regenerated carbon fiber, a method that is more efficient than the conventional JIS R7606 test method for short fibers is required. Moreover, in the test for the single fiber, the measurement for the fiber that was not cut in the extraction process is performed, and the tensile strength may be higher than the actual one. For this reason, there is a need for a highly accurate method for measuring the strength of regenerated carbon fiber that allows simple and efficient measurement and reflects the strength of the actual regenerated carbon fiber.
本発明の再生炭素繊維の強度測定方法は、再生炭素繊維の強度測定方法であって、再生炭素繊維の束の繊維長を測定する工程と、再生炭素繊維の束の重量を測定する工程と、再生炭素繊維の束の断面積を式１を用いて決定する工程と、再生炭素繊維の束の破断荷重を決定する工程と、再生炭素繊維の強度を式２を用いて決定する工程と、を備えている。 The strength measurement method of the regenerated carbon fiber of the present invention is a strength measurement method of the regenerated carbon fiber, the step of measuring the fiber length of the bundle of the regenerated carbon fiber, the step of measuring the weight of the bundle of the regenerated carbon fiber, A step of determining a cross-sectional area of the bundle of regenerated carbon fibers using Equation 1, a step of determining a breaking load of the bundle of regenerated carbon fibers, and a step of determining the strength of the regenerated carbon fibers using Equation 2. I have.
ここで再生炭素繊維の束の断面積Ｓ（ｍ２）を決定する式１は、
であり、Ｗが再生炭素繊維の束の重量（g）であり、ρが再生炭素繊維の密度（ｇ／ｃｍ３）であり、lが再生炭素繊維の束の繊維長（ｍｍ）である。
Here, Equation 1 for determining the cross-sectional area S (m 2 ) of the bundle of regenerated carbon fibers is
Where W is the weight (g) of the bundle of regenerated carbon fibers, ρ is the density of the regenerated carbon fibers (g / cm 3 ), and l is the fiber length (mm) of the bundle of regenerated carbon fibers.
再生炭素繊維の強度σ（ＭＰａ）を決定する式２は、
であり、Ｆが破断荷重（Ｎ）であり、Ｓが式１によって求めた再生炭素繊維の断面積（ｍ２）である。
Formula 2, which determines the strength σ (MPa) of the regenerated carbon fiber,
Where F is the breaking load (N), and S is the cross-sectional area (m 2 ) of the regenerated carbon fiber determined by Equation 1.
発明者は、再生炭素繊維の束に含まれる本数と、その重量との間に高い相関関係があり、さらに、再生炭素繊維の重量と破断強度との間に高い相関関係があることを見いだして、本発明をなすに至った。再生炭素繊維は、バージン炭素繊維の使用状態を反映して、多数の単繊維で構成された繊維束（フィラメント）あるいは１，０００本から数万本のフィラメント束（トウ）の形状を残していることが多い。このフィラメント束（トウ）を用いて引張試験を行うことにより、抜き出し段階で切れる繊維も含めて強度を測定することができる。そして、測定された破断強度から、炭素繊維の強度を決定することができる。 The inventor has found that there is a high correlation between the number of regenerated carbon fibers contained in the bundle and the weight thereof, and that there is a high correlation between the weight of the regenerated carbon fibers and the breaking strength. The present invention has been made. Recycled carbon fiber reflects the state of use of virgin carbon fiber, leaving the shape of a fiber bundle (filament) composed of a large number of single fibers or 1,000 to tens of thousands of filament bundles (tow). There are many cases. By carrying out a tensile test using this filament bundle (tow), the strength can be measured including fibers that are cut in the extraction stage. Then, the strength of the carbon fiber can be determined from the measured breaking strength.
本発明の強度測定方法は、再生炭素繊維の引張特性を精度高く評価することができる。しかも、試験に供する再生炭素繊維の束に含まれる本数を数える代わりに、再生炭素繊維束の重量を測定し、その破断荷重を測定することで再生炭素繊維の実質的な強度を知ることができるので、短繊維の測定と比較すると、非常に効率よく迅速に炭素繊維の強度を知ることができる。 The strength measurement method of the present invention can accurately evaluate the tensile properties of the regenerated carbon fiber. Moreover, instead of counting the number of regenerated carbon fiber bundles used in the test, the weight of the regenerated carbon fiber bundle is measured, and the substantial strength of the regenerated carbon fiber can be determined by measuring the breaking load. Therefore, compared with the measurement of short fibers, the strength of carbon fibers can be known very efficiently and quickly.
種々の検討の結果、再生炭素繊維は、繊維長が一定の場合、本数と重量との間に正の相関関係を有していることが明らかとなっている。同時に、再生炭素繊維は、本数と破断強度との間に正の相関関係を有していることが明らかとなっている。図２は、一例として温度５００oＣで焼成処理を行った、繊維長が９０ｍｍの再生炭素繊維の本数Ｎと重量Ｗ（ｍｇ）との関係を示している。図３は、同一条件である５００oＣの焼成処理を行った、繊維長が９０ｍｍの同一種類の再生炭素繊維における、再生炭素繊維の束の本数Ｎと、この束を用いて引張り試験を行った場合の破断強度Ｆ（Ｎ）との関係を示している。これらを含めた多くの測定結果から、再生炭素繊維の本数と重量との間に正の相関関係があり、同時に、再生炭素繊維の本数と破断強度との間に正の相関関係がある事が確認された。その結果として、再生炭素繊維には、重量と破断強度との間に正の相関関係を有していることが確認された。 As a result of various studies, it has been clarified that the regenerated carbon fiber has a positive correlation between the number and the weight when the fiber length is constant. At the same time, it is clear that the regenerated carbon fiber has a positive correlation between the number and the breaking strength. FIG. 2 shows the relationship between the number N of regenerated carbon fibers having a fiber length of 90 mm and the weight W (mg), which was baked at a temperature of 500 ° C. as an example. FIG. 3 shows a case in which the number N of regenerated carbon fiber bundles in the same type of regenerated carbon fiber having a fiber length of 90 mm subjected to a firing process of 500 ° C. under the same conditions and a tensile test using this bundle. Shows the relationship with the breaking strength F (N). From many measurement results including these, there is a positive correlation between the number of regenerated carbon fibers and the weight, and at the same time, there is a positive correlation between the number of regenerated carbon fibers and the breaking strength. confirmed. As a result, it was confirmed that the regenerated carbon fiber has a positive correlation between the weight and the breaking strength.
図４に、炭素繊維を４６０oＣで焼成処理して得た再生炭素繊維の重量Ｗ（ｍｇ）と破断強度Ｆ（Ｎ）との関係を示す。図５に、炭素繊維を４８０oＣで焼成処理して得た再生炭素繊維の重量Ｗ（ｍｇ）と破断強度Ｆ（Ｎ）との関係を示す。図６に、炭素繊維を５００oＣで焼成処理して得た再生炭素繊維の重量Ｗ（ｍｇ）と破断強度Ｆ（Ｎ）との関係との関係を示す。測定を行った再生炭素繊維の束は、いずれも繊維長が９０ｍｍである。再生炭素繊維は、引張り試験時の保持具（クランプ装置）間の距離（ｈ）を２５ｍｍとして、引っ張り試験を行っている。焼成温度を変更して得たこれらの再生炭素繊維の強度試験の測定結果からもまた、再生炭素繊維の重量と破断強度との間には正の強い相関関係があることが確認された。このことから、再生炭素繊維の繊維長および重量を測定し、さらにその破断強度を特定することで、再生炭素繊維の強度を特定できることが明らかとなった。 FIG. 4 shows the relationship between the weight W (mg) and the breaking strength F (N) of the regenerated carbon fiber obtained by firing the carbon fiber at 460 ° C. FIG. 5 shows the relationship between the weight W (mg) and the breaking strength F (N) of the regenerated carbon fiber obtained by firing the carbon fiber at 480 ° C. FIG. 6 shows the relationship between the weight W (mg) of the regenerated carbon fiber obtained by firing the carbon fiber at 500 ° C. and the relationship between the breaking strength F (N). All of the bundles of regenerated carbon fibers subjected to the measurement have a fiber length of 90 mm. The recycled carbon fiber is subjected to a tensile test with a distance (h) between holders (clamp devices) at the time of a tensile test of 25 mm. Also from the measurement results of the strength tests of these regenerated carbon fibers obtained by changing the firing temperature, it was confirmed that there was a strong positive correlation between the weight of the regenerated carbon fibers and the breaking strength. From this, it became clear that the strength of the regenerated carbon fiber can be specified by measuring the fiber length and weight of the regenerated carbon fiber and further specifying its breaking strength.
本発明の破断強度の測定に適用可能な、強度試験機１の一例を図１に挙げる。たとえば、（株）エー・アンド・デイ製、ＴＥＮＳＩＲＯＮ万能試験機ＲＴＦ−１３５０が使用可能であり、試験方法は、用いる繊維の本数以外、ＪＩＳ Ｒ７６０６に規定される試験方法と実質的に同一である。再生炭素繊維の束１０は、所定の間隔（ｈ）で上下の保持具２，２によって固定されており、保持具２，２が所定の速度で離間していくことで再生炭素繊維の束に加わる荷重が増大する。試料である再生炭素繊維の束１０に加えた荷重は、検出器であるロードセル３で測定して出力し、応力−歪み曲線や破断強度の値として表示することができる。 An example of a strength tester 1 applicable to the measurement of the breaking strength of the present invention is shown in FIG. For example, A & D Co., Ltd., TENSIRON universal testing machine RTF-1350 can be used, and the test method is substantially the same as the test method defined in JIS R7606, except for the number of fibers used. . The bundle 10 of the regenerated carbon fibers is fixed by the upper and lower holders 2 and 2 at a predetermined interval (h), and the holders 2 and 2 are separated at a predetermined speed to form a bundle of regenerated carbon fibers. The applied load increases. The load applied to the bundle 10 of the regenerated carbon fiber that is a sample can be measured and output by the load cell 3 that is a detector, and can be displayed as a value of a stress-strain curve or a breaking strength.
本発明の再生炭素繊維の強度測定方法の各工程について、以下に説明する。図８に、再生炭素繊維の強度測定方法のフローチャートを示す。再生炭素繊維の強度測定方法は、再生炭素繊維の束の繊維長ｌ（ｍｍ）を測定する工程（ステップ１）と、再生炭素繊維の束の重量を測定する工程（ステップ２）と、再生炭素繊維の束の断面積を式１を用いて決定する工程（ステップ３）と、再生炭素繊維の束の破断荷重を決定する工程（ステップ４）と、再生炭素繊維の強度を式２を用いて決定する工程（ステップ５）と、を備えている。 Each step of the method for measuring the strength of the regenerated carbon fiber of the present invention will be described below. FIG. 8 shows a flowchart of a method for measuring the strength of the regenerated carbon fiber. The strength measurement method of the regenerated carbon fiber includes a step of measuring the fiber length l (mm) of the bundle of regenerated carbon fibers (step 1), a step of measuring the weight of the bundle of regenerated carbon fibers (step 2), and the regenerated carbon. The step of determining the cross-sectional area of the bundle of fibers using Equation 1 (Step 3), the step of determining the breaking load of the bundle of recycled carbon fibers (Step 4), and the strength of the recycled carbon fibers using Equation 2. And a step of determining (step 5).
再生炭素繊維の束の繊維長ｌ（ｍｍ）を測定する工程は、たとえばノギスや顕微鏡等の距離測定手段を用いて行うことができる。再生炭素繊維の束の重量Ｗ（ｇ）を測定する工程は、たとえば電子天秤等の重量測定手段を用いて測定する行うことができる。 The step of measuring the fiber length l (mm) of the bundle of regenerated carbon fibers can be performed using a distance measuring means such as a caliper or a microscope. The step of measuring the weight W (g) of the bundle of regenerated carbon fibers can be performed using a weight measuring means such as an electronic balance.
ステップ３の再生炭素繊維の束の断面積Ｓ（ｍ２）の決定は、以下の式１を用いて行われる。
ここで、ρは再生炭素繊維の密度（ｇ／ｃｍ３）であり、lは、測定を行う再生炭素繊維の束の繊維長（ｍｍ）である。ρは原料であるバージン炭素繊維の密度の値と同一とすることができる。または、密度の値は、一旦測定を行えば、その後は、同一の種類の炭素繊維について、同一の値を使用することができる。
The determination of the cross-sectional area S (m 2 ) of the bundle of regenerated carbon fibers in Step 3 is performed using the following Equation 1.
Here, ρ is the density (g / cm 3 ) of the regenerated carbon fiber, and l is the fiber length (mm) of the bundle of regenerated carbon fiber to be measured. ρ can be the same as the density value of the virgin carbon fiber as a raw material. Or once the density value is measured, the same value can be used for the same type of carbon fiber.
再生炭素繊維の束の断面積Ｓ（ｍ２）を決定するもう一つの方法として、炭素繊維についての線密度の値ｔｅｘ（ｇ／１０００ｍ）の値が既知であれば、
Ｓ ＝ ｔｅｘ／（ρ×１０９） （式３）
から、断面積を計算により決定することができる。
As another method for determining the cross-sectional area S (m 2 ) of the bundle of regenerated carbon fibers, if the value of the linear density value tex (g / 1000 m) for the carbon fibers is known,
S = tex / (ρ × 10 9 ) (Formula 3)
From this, the cross-sectional area can be determined by calculation.
ステップ４の破断強度の決定工程は、強度試験機１を用いて、所定の間隔（ｈ）で把持した再生炭素繊維の束の引張り試験を行い、破断強度を測定することで行われる。 The step 4 for determining the breaking strength is performed by performing a tensile test on the bundle of regenerated carbon fibers held at a predetermined interval (h) using the strength tester 1 and measuring the breaking strength.
ステップ５の再生炭素繊維の強度σ（ＭＰａ）の決定工程は、式２を用いて行われる。
以上のステップ１からステップ５の工程を行うことにより、再生炭素繊維の強度を、簡易且つ正確に知ることができる。本発明の再生炭素繊維の強度測定方法は、同一の種類の試料について、２０回以上の繰り返し試験をおこなうことで、十分な信頼性を得ることができる。 By performing the steps 1 to 5 described above, the strength of the regenerated carbon fiber can be easily and accurately known. In the method for measuring the strength of the regenerated carbon fiber of the present invention, sufficient reliability can be obtained by performing the test 20 times or more on the same type of sample.
１ 強度試験機
２ 保持具
３ ロードセル
１０ 再生炭素繊維の束
1 Strength Tester 2 Holder 3 Load Cell 10 Bundle of Recycled Carbon Fiber
Claims (1)
再生炭素繊維の束の繊維長を測定する工程と、
再生炭素繊維の束の重量を測定する工程と、
前記再生炭素繊維の束の断面積を、以下の式１を用いて決定する工程と、
前記再生炭素繊維の束の破断荷重を決定する工程と、
前記再生炭素繊維の強度を、以下の式２を用いて決定する工程と、
を備えており、
ここで式１が、
であり、Ｓが再生炭素繊維の束の断面積（ｍ２）であり、Ｗが測定した再生炭素繊維の束の重量（g）であり、ρが再生炭素繊維の密度（ｇ／ｃｍ３）であり、ｌが再生炭素繊維の束の繊維長（ｍｍ）であり、
且つ、式２が、
再生炭素繊維の強度測定方法。 A method for measuring the strength of recycled carbon fiber,
Measuring the fiber length of a bundle of recycled carbon fibers;
Measuring the weight of the bundle of regenerated carbon fibers;
Determining the cross-sectional area of the bundle of regenerated carbon fibers using Equation 1 below:
Determining a breaking load of the bundle of regenerated carbon fibers;
Determining the strength of the regenerated carbon fiber using Equation 2 below:
With
Where Equation 1 is
S is the cross-sectional area (m 2 ) of the bundle of regenerated carbon fibers, W is the weight (g) of the bundle of regenerated carbon fibers measured, and ρ is the density (g / cm 3 ) of the regenerated carbon fibers. Where l is the fiber length (mm) of the bundle of regenerated carbon fibers,
And Equation 2 is
A method for measuring the strength of recycled carbon fiber.
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| CN116296766A (en) * | 2023-05-22 | 2023-06-23 | 连云港鹰游工程技术研究院有限公司 | Carbon fiber bundle transverse strength detection device and application method thereof |
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| CN116296766A (en) * | 2023-05-22 | 2023-06-23 | 连云港鹰游工程技术研究院有限公司 | Carbon fiber bundle transverse strength detection device and application method thereof |
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